Sulphur-containing optical epoxy resin and preparation method thereof

A technology of epoxy resin and sulfur optics, which is applied in the field of optical epoxy resin containing sulfur and high refractive index and its synthesis. High efficiency and transparent appearance

Inactive Publication Date: 2012-05-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Guan Jianguo et al. (Guan Jianguo, Huang Jun, Yuan Runzhang. Current status and research progress of optically transparent materials II: Organic-inorganic nanocomposite optically transparent materials [J]. Journal of Wuhan University of Technology, 1998, 20(9): 11-13) It is pointed out that there are several problems in the preparation of monolithic optically transparent composite materials by the traditional sol-gel method, which is a nanocomposite technology: (1) low molecular by-products such as water and alcohol produced in the process of volatilization, hydrolysis and polycondensation The product and a large amount of solvent will have serious volume shrinkage (greater than 50%), and then bring large internal stress and significant cracks, so it is difficult to make a block optically transparent ...

Method used

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  • Sulphur-containing optical epoxy resin and preparation method thereof
  • Sulphur-containing optical epoxy resin and preparation method thereof
  • Sulphur-containing optical epoxy resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add ECH (0.2 mol) and DMTD (0.1 mol) into a nitrogen-protected flask equipped with a stirring device, a thermometer and a reflux condenser (the flask needs a water bath), and stir and dissolve in an ice-water bath. And add 10% (mass concentration) sodium hydroxide solution containing 0.001 mol of alkali. After the DMTD was completely dissolved, the temperature was raised to 50°C, and the reaction was carried out for 2 hours. Recover the unreacted ECH by distillation at 120°C; finally cool down to 50°C; add 0.2mol methyl isobutyl ketone, keep the reaction temperature at 50°C, and gradually dropwise add sodium hydroxide solution with a mass concentration of 10%. The amount of sodium hydroxide added is 0.2mol, and the addition is completed within 1h; then keep warm for 0.5h. Stop stirring and discharge. Put the material in a separatory funnel, add deionized water, shake, separate and remove the water layer. Then add deionized water, repeat the liquid separation several ...

Embodiment 2

[0032] Add ECH (2 mol) and DMTD (0.1 mol) into a nitrogen-protected flask equipped with a stirring device, a thermometer and a reflux condenser (the flask needs a water bath), and stir and dissolve in an ice-water bath. And add 10% sodium hydroxide solution containing 0.001 mol of alkali. After the DMTD was completely dissolved, the temperature was raised to 50°C, and the reaction was carried out for 2 hours. Recover the unreacted ECH distillation under the condition of 120 ℃; finally cool down to 50 ℃; add 0.2mol methyl isobutyl ketone, keep the reaction temperature at 50 ℃, gradually dropwise add the sodium hydroxide solution whose mass concentration is 10%, The amount of sodium hydroxide added is 0.2mol, and the addition is completed within 1h; then keep warm for 0.5h. Stop stirring and discharge. Put the material in a separatory funnel, add deionized water, shake, separate and remove the water layer. Then add deionized water, repeat the liquid separation several times u...

Embodiment 3

[0034] Add ECH (1mol) and DMTD (0.1mol) into a nitrogen-protected flask equipped with a stirring device, a thermometer, and a reflux condenser (the flask needs a water bath), and stir and dissolve in an ice-water bath. And add 10% 1 sodium hydroxide solution containing 0.001 mol of alkali. After the DMTD was completely dissolved, the temperature was raised to 50°C, and the reaction was carried out for 2 hours. Recover the unreacted ECH distillation under the condition of 100°C; finally cool down to 50°C; add 0.2mol methyl isobutyl ketone, keep the reaction temperature at 50°C, and gradually add a mass concentration of 10% sodium hydroxide solution, The amount of sodium hydroxide added is 0.2mol, and the addition is completed within 1h; then keep warm for 0.5h. Stop stirring and discharge. Put the material in a separatory funnel, add deionized water, shake, separate and remove the water layer. Then add deionized water, repeat the liquid separation several times until the org...

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Abstract

The invention discloses sulphur-containing optical epoxy resin and a preparation method thereof. The method comprises the following steps of: taking 2,5-disulfydryl-1,3,4-DMTD and epoxy chloropropane as reaction raw materials; taking one or more of an alkaline solution, quaternary ammonium salt and triphenylphosphine as catalysts; taking aqueous solution or solid of one or more of sodium hydroxide, lithium hydroxide and potassium hydroxide as reaction raw materials in the second step; taking one or more of methylbenzene, dimethylbenzene, benzene, ethylbenzene, diethylbenzene, carbon tetrachloride, methyl isobutyl ketone and methyl ethyl ketone as solvents; and finally, drying in vacuum at room temperature or under the ultra-low temperature condition to obtain dimercaptothiodiazole glycidyl ether epoxy resin. The prepared epoxy resin has the advantages of being high in epoxy value, low in viscosity, higher in refractive index, better in transparent property and the like. The epoxy resin can be applied to the fields, such as optical packaging, optical adhesive, optical part and the like.

Description

technical field [0001] The invention relates to an epoxy resin, in particular to an optical epoxy resin with high refractive index containing sulfur atoms, in particular to a sulfur-containing optical epoxy resin with high refractive index and a synthesis method thereof. Background technique [0002] With the advancement of science, optical materials are increasingly used in technology and life. Epoxy resin is widely used in the field of optical resins due to its characteristics of easy curing, adjustable curing conditions, and good transparency, such as optical devices, optical packaging, and optical adhesives. However, epoxy has a low refractive index. The refractive index of ordinary epoxy resin is about 1.57, which is far from meeting the increasingly high requirements of optical materials. [0003] Inorganic materials generally have a relatively high refractive index. For example, titanium dioxide is widely used as a white pigment because of its particularly high ref...

Claims

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Application Information

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IPC IPC(8): C08G59/02C07D417/14
Inventor 罗超云赵建青刘述梅肖仁亮左建东
Owner SOUTH CHINA UNIV OF TECH
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