Hydrogen-based silicone resin containing trifunctional group chain element and preparation method thereof

A trifunctional, silicone resin technology, applied in electrical components, circuits, semiconductor devices, etc., can solve the problems such as wrinkles in addition-crosslinking reaction products, inability to achieve smooth and bright appearance, slow reaction speed, etc., to improve production efficiency and Luminous efficiency, smooth and bright appearance, fast response

Active Publication Date: 2012-08-15
BEIJING KMT TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product containing a difunctional chain link structure has low reactivity in the addition crosslinking reaction, resulting in a slow reaction rate, and the obtained addition crosslinking reaction product has wrinkles and lines, which cannot meet the requirements of smooth and bright appearance.

Method used

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  • Hydrogen-based silicone resin containing trifunctional group chain element and preparation method thereof
  • Hydrogen-based silicone resin containing trifunctional group chain element and preparation method thereof
  • Hydrogen-based silicone resin containing trifunctional group chain element and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Add 136g of methyltrimethoxysilane, 67g of tetramethyldihydrodisiloxane, 70g of xylene and 0.35g of concentrated sulfuric acid into a 500ml three-necked flask, and add 35g of deionized water dropwise at 55°C under constant stirring. Run for about 50 minutes, then reflux for 1.5 hours. Change it to a distillation device, raise the temperature to 105°C, and distill out by-products. After cooling down to 45°C, 0.8g of pyridine was added and stirred for about 30 minutes to make the solution neutral. After filtering with filter paper, at 130° C., the solvent xylene and low-molecular substances were distilled off under reduced pressure using a vacuum pump to obtain 123 g of a colorless and transparent hydrogen-based silicone resin containing trifunctional chain members. The viscosity measured by the NDJ-79 rotational viscometer is 15 mPa.s, and the active H mass fraction is 0.7% as measured by the nuclear magnetic resonance method.

Embodiment 2

[0058] Add 267g of methyltriethoxysilane, 67g of tetramethyldihydrodisiloxane, 360g of toluene and 3.3g of concentrated hydrochloric acid into a 1000ml three-necked flask, and add 100g of deionized water dropwise at 85°C under constant stirring, Run for about 50 minutes, then reflux for 3.5 hours. Change to a distillation device, raise the temperature to 100°C, and distill out by-products. After cooling down to 42°C, 3.5g of sodium bicarbonate was added and stirred for about 30 minutes to make the solution neutral. After filtering with filter paper, at 120° C., the solvent toluene and low-molecular substances were distilled off using a vacuum water pump under reduced pressure to obtain 150 g of a colorless and transparent hydrogen-based silicone resin containing trifunctional chain members. Using the same method as in Example 1, its viscosity was measured to be 21 mPa.s, and the mass fraction of active H was 0.58%.

Embodiment 3

[0060] Add 102g of methyltrimethoxysilane, 67g of tetramethyldihydrodisiloxane, 10g of absolute ethanol, 140g of toluene, and 0.33g of trifluoromethanesulfonic acid into a 500ml three-necked flask. Add 40 g of deionized water for about 35 minutes, then reflux for 2 hours. Change it to a distillation device, raise the temperature to 105°C, and distill out by-products. After cooling down to 48°C, 1.5g of sodium bicarbonate was added and stirred for about 30 minutes to make the solution neutral. After filtering with filter paper, at 130° C., the solvent toluene, ethanol and low-molecular substances were distilled off using a vacuum water pump to obtain 109 g of a colorless and transparent hydrogen-based silicone resin containing trifunctional chain members. Using the same method as in Example 1, its viscosity was measured to be 12 mPa.s, and the mass fraction of active H was 0.79%.

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Abstract

The invention relates to hydrogen-based silicone resin containing a trifunctional group chain element and a preparation method thereof. The hydrogen-based silicone resin containing the trifunctional group chain element has the following structural general formula: (R12HSiO1/2) a (R2SiO3/2) b, wherein a is not less than 3 and is of an integer, b is not less than 1 and is of an integer, the relation between a and b meets the condition that b/a is not less than 0.33 and not more than 4, R1 is of alkyl with 1-3 carbon atoms, and R2 is of phenyl or alkyl with 1-3 carbon atoms. The preparation method sequentially comprises the following steps of: 1) mixing trifunctional alkoxy silane, tetra-alkyl-dihydro-disiloxane, an organic solvent and an acid catalyst; 2) adding water to perform hydrolysis on the trifunctional alkoxy silane; and 3) evaporating out byproducts so as to get the hydrogen-based silicone resin disclosed by the invention. The hydrogen-based silicone resin disclosed by the invention can be used for cross-linking and curing reaction of LED (light-emitting diode) packaging materials and other addition type polysiloxane, and has the characteristics of high curing speed and smooth appearance of the obtained product.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a hydrogen-based silicone resin containing trifunctional chain segments and a preparation method thereof. Background technique [0002] Light Emitting Diode, referred to as LED (Light Emitting Diode), is a type of electroluminescent solid-state device, and its structure is mainly composed of PN junction chips, electrodes and optical systems. LED has excellent characteristics such as small size, safe low voltage, long life, high electro-optical conversion efficiency, fast response speed, energy saving, environmental protection, etc., and it is called "green lighting source". Today's LED applications are extremely extensive, status display, sign lighting, LCD backlight, traffic signs, graphic display full-color screens, and indoor lighting that requires point or surface light sources are all LED application markets. [0003] The structure and process of LED packaging a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/06C08L83/05H01L33/56
Inventor 李振忠李平
Owner BEIJING KMT TECH
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