Method for preparing sulfur-containing high-refractive-index resin

A technology of resin and dithiol, applied in adhesive types, polyurea/polyurethane adhesives, coatings, etc., can solve heat resistance, weather resistance, wear resistance, solvent resistance, poor moisture absorption resistance, refraction Problems such as low index and low hardness achieve the effect of high refractive index

Inactive Publication Date: 2013-03-27
深圳市迪凯鑫科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 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 r

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In the first step, add 2 mol of epichlorohydrin into a 1000 mL three-necked flask, stir and heat to 60°C, then add 0.2 mol of 4,4'-dimercaptodiphenyl sulfide, and then add about 200 mL of 20% NaOH solution, Stir the reaction for 0.5 h, cool to room temperature, add 2 times the volume of diethyl ether and 2 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 the sulfur-containing ring Oxygen; Weigh 0.1mol of the above-synthesized sulfur-containing epoxy into a 500mL three-necked flask, stir and heat to 110°C, then add 0.5% catalyst N,N-diethylbenzylamine and 0.5% polymerization inhibitor agent p-hydroxyanisole; then add 0.2mol of acrylic acid, and continue to react for 4h to obtain sulfur-containing epoxy acrylate In the second step, add 1.0mol of toluene diisocyanate (TDI) in a three-necked flask of 1000mL, heat to 55°C, dibu...

Embodiment 2

[0028]In the first step, add 3mol of epichlorohydrin into a 1000mL three-necked flask, stir and heat to 50°C, then add 0.6mol of 1,8-octanedithiol, then add about 320mL of 20% NaOH solution, and stir for 1h , cooled to room temperature, added 3 times the volume of diethyl ether and 5 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; Add 0.3mol of the sulfur-containing epoxy synthesized above into a 500mL three-necked flask, stir and heat to 120°C, then add 0.1% catalyst tetrabutylammonium bromide and 0.8% polymerization inhibitor p-hydroxyanisole; Then add 0.6mol of methacrylic acid and continue to react for 2.5h to obtain sulfur-containing epoxy acrylate ; In the second step, add 1.2mol of hexamethylene diisocyanate (HDI) in a 1000mL three-necked flask, heat to 65°C, and dibutyltin dilaurate i...

Embodiment 3

[0030] In the first step, add 2mol of epichlorohydrin into a 1000mL three-necked flask, stir and heat to 100°C, then add 0.3mol of 2,4-dimercaptopyrimidine, then add about 200mL of 20% NaOH solution, and stir for 0.5h , cooled to room temperature, added 5 times the volume of diethyl ether and 3 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; Add 0.2mol of the sulfur-containing epoxy synthesized above into a 500mL three-necked flask, stir and heat to 90°C, then add 0.8% catalyst tris(acetylacetonate) lanthanum(Ⅲ) and 0.2% inhibitor p-hydroxy Anisole; then add 0.4mol of acrylic acid, continue to react for 6h, obtain sulfur-containing epoxy acrylate ; In the second step, add 1.0 mol of isophorone diisocyanate (IPDI) to a 1000 mL three-neck flask, heat to 75°C, add 1.0% of dibutyltin dilaurate to...

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PUM

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Abstract

The invention discloses a method for preparing sulfur-containing high-refractive-index resin, comprising the steps of (A) preparing a sulfur-containing epoxy acrylate chain segment; (B) preparing a urethane acrylate chain segment; and (C) preparing the sulfur-containing high-refractive-index resin. According to the invention, a dithiol compound is reacted with epoxy chloropropane firstly to prepare sulfur-containing epoxy; the sulfur-containing epoxy is reacted with acrylic acid to form sulfur-containing epoxy acrylate; and then a urethane acrylate prepolymer with a NCO functional group at one end is grafted at the side chain of the sulfur-containing epoxy acrylate. The resin prepared by adopting the method disclosed by the invention has higher refractive index, is provided with an ultraviolet-polymerizable acrylate double bond and can be applied to products such as light curing adhesives, coatings and the like.

Description

technical field [0001] The invention belongs to the technical field of organic polymer synthesis, and in particular relates to a method for preparing a sulfur-containing high-refractive resin. The resin has acrylate double bonds that can be polymerized by ultraviolet light, and is used in the fields of photocurable adhesives, coatings, and the like. [0002] Background technique [0003] Optical materials are generally divided into two categories: inorganic optical materials and organic polymer optical materials. With the deepening of polymer research and the advancement of related technologies, polymer optical materials have flourished in the past few decades, greatly broadening the application level of optical materials, and are gradually replacing inorganic optical materials. Polymer optical materials have the advantages of light weight, impact resistance, easy processing and molding, and excellent optical properties. They have broad application prospects in optical disc...

Claims

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Application Information

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IPC IPC(8): C08G18/83C08G18/67C08G18/66C08G18/32C09D175/14C09J175/14
Inventor 刘红波林峰肖望东张武英
Owner 深圳市迪凯鑫科技有限公司
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