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Synthesis method of special catalyst for addition-type high refractive index LED encapsulation resin

A technology of LED packaging and high refractive index, which is applied in the direction of electrical components, circuits, semiconductor devices, etc., can solve the problems of reducing the initial heat release peak, too fast rise in viscosity, shortening the operating time window, etc., to achieve the reduction of vinyl content, Good compatibility, reduced handling and contamination loss

Inactive Publication Date: 2017-06-13
YANTAI DARBOND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to reduce the initial exothermic peak, the result of reducing the amount of polymerization inhibitor is that the viscosity rises too fast when mixing at room temperature, so that the operable time window is shortened

Method used

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  • Synthesis method of special catalyst for addition-type high refractive index LED encapsulation resin
  • Synthesis method of special catalyst for addition-type high refractive index LED encapsulation resin
  • Synthesis method of special catalyst for addition-type high refractive index LED encapsulation resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The synthesis of embodiment 1 vinyl phenyl silicone resin

[0032] 1.1 Synthesis of vinylphenyl silicone resin V-11

[0033] Add 978.75g (5.25mol) divinyltetramethyldisiloxane, 2082g (10.5mol) phenyltrimethoxy Silane, 458g (1wt%) sulfuric acid aqueous solution, equipped with mechanical stirring, thermometer, dean-stark tube and condenser tube, receiving bottle, after the mixture was stirred at room temperature for 1.5 hours, the temperature of the liquid was raised to 40 ° C, at this time the oil The heating temperature of the bath was raised to 70° C., and after stirring and reacting for 3 hours, the temperature of the oil bath was raised to 100° C. to distill out the generated by-products. The distillation continued for about 2 hours, at which time the temperature of the reaction mixture rose to 90°C. Stirring and heating were discontinued and the reaction mixture was allowed to stand overnight. Add 2.6g of potassium hydroxide, 700mL of toluene and 13mL of water to...

Embodiment 2

[0040] The synthesis of embodiment 2 Pt-divinyltetramethyldisiloxane solution

[0041] 2.1 Add 1g of chloroplatinic acid hexahydrate (molecular formula H 2 PtCl 6 6H 2 (0, effective Pt content ≥ 37%), 30mL absolute ethanol, 10g divinyltetramethyldisiloxane, and 3g sodium bicarbonate powder, equipped with a magnetic stirring oil bath heating device and a condenser, to the reaction system Under the protection of nitrogen gas, the temperature was raised to 70° C. for 1 hour, and the mixture changed from brownish red to light yellow at first, and the obtained mixture was named B-1.

[0042] 2.2 Add 1g of chloroplatinic acid hexahydrate (molecular formula H 2 PtCl 6 6H 2 (0, effective Pt content ≥ 37%), 60mL absolute ethanol, 40g divinyltetramethyldisiloxane, and 5g sodium bicarbonate powder, equipped with a magnetic stirring oil bath heating device and a condenser, to the reaction system Under nitrogen protection, the temperature was raised to 65°C for 0.5 hour reaction, the...

Embodiment 3

[0044] The synthesis of embodiment 3 catalyst

[0045] 3.1 Synthesis and post-treatment of a highly active low-vinyl high-phenyl catalyst with an active ingredient content of 5000ppm:

[0046] The reaction mixture B-1 prepared in Example 2 and the low-viscosity, low-vinyl content, high-phenyl ligand resin V-11 prepared in 74g of Example 1 were jointly added in a 500mL single-mouthed eggplant-shaped bottle, and were mixed with a rotary evaporator. At 60°C, under the condition of air pressure <1mbar, vacuumize to remove low boilers. The obtained turbid liquid was filtered once to obtain a pale yellow transparent Pt-resin complex with an active ingredient content of 5000 ppm, which was named as C-1.

[0047] 3.2 Synthesis and post-treatment of a highly active low-vinyl high-phenyl catalyst with an active ingredient content of 1000ppm:

[0048] The reaction mixture B-2 prepared in Example 2 and the low-viscosity, low-vinyl content, and high-phenyl ligand resin V-23 prepared in 3...

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Abstract

The invention relates to a special addition type high-activity catalyst for high-refractive index LED packaging resin. The special addition type high-activity catalyst is prepared through the following steps of: firstly synthesizing low-viscosity low-vinyl content high-phenyl ligand resin, wherein the low-viscosity low-vinyl content high-phenyl ligand resin contains no volatile organic solvent or low molecule; then synthesizing a Pt-divinyl tetramethyl disiloxane solution. According to the special addition type high-activity catalyst, the low-viscosity low-vinyl content high-phenyl ligand resin is adopted for dilution, the low-viscosity low-vinyl content high-phenyl ligand resin has good compatibility with the high-refractive index LED packaging resin without causing system turbidity, contains no low molecule component and can not release a harmful gas; and the vinyl content of a system can be obviously reduced by mixing the catalyst generated in situ and low-viscosity resin and removing organ volatile components by directly carrying out high-vacuum rotational evaporation, so that the activity of the catalyst is enhanced.

Description

technical field [0001] The invention relates to the preparation of a special high-activity catalyst for an addition-type high-refractive index LED packaging resin, belonging to the field of synthetic chemistry. Background technique [0002] Known LED encapsulation resins are usually addition-type two-component products, using Si-H and Si-CH=CH 2 Addition reaction between them and cross-linking solidification. The commonly used catalyst is a vinyl coordination type, and its basic structure is as follows: [0003] [0004] Dissolve the Pt(0) complex of this structure in divinyltetramethyldisiloxane, tetravinyltetramethylcyclotetrasiloxane or toluene to make a diluted catalyst, which can be used for catalytic addition into a reaction. [0005] Compared with chloroplatinic acid, the above-mentioned catalyst system has higher activity and does not contain chlorine, which meets the requirements of electronic packaging for halogen content, and can ensure that the product pass...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/08C08G77/20H01L33/56
Inventor 陈维张学超王建斌陈田安
Owner YANTAI DARBOND TECH
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