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Phenyl MDT silicon resin and preparation method thereof

A silicone resin and phenyl technology, applied in the field of polymer chemistry, to achieve the effect of simple operation steps, saving procedures, and low equipment and operation requirements

Active Publication Date: 2013-08-07
CHENGDU GUIBAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the MDT resin raw material in the prior art has strong corrosion to the equipment during the reaction, the present invention provides a phenyl MDT silicone resin and a preparation method thereof. The raw material of the MDT silicone resin is monofunctional organosilane as the M chain Section, choose difunctional organosilane containing phenyl as D chain link and trifunctional organosilane as T chain link, which not only effectively improves the refractive index of the product, but also has mild reaction conditions and no corrosive substances are produced

Method used

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  • Phenyl MDT silicon resin and preparation method thereof

Examples

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Effect test

Embodiment 1

[0024] Add the source of T chain link into the three-necked bottle: 100 parts of phenyltrimethoxysilane; the source of D chain link: 25 parts of diphenyldimethoxysilane, 50 parts of dimethyldiethoxysilane; the source of M chain link: 10 parts of vinyldimethylethoxysilane, 20 parts of hexamethyldisiloxane; 55 parts of hydrochloric acid with a mass fraction of 1% was added dropwise at room temperature, and the drop was completed in 30 minutes. After completion, the temperature was raised to 50°C for 1 hour, and then the temperature was raised Reaction at 70°C for 5h. The reaction solution was left to stand for stratification, the organic layer was washed to neutrality, dried with 5 parts of calcium chloride, and the filtrate was collected by filtration. The filtrate was equilibrated with tetramethylammonium hydroxide at 110°C for 5 hours and heated to 180°C. The catalyst was decomposed and removed, and the low-molecular substances were removed under the negative pressure conditi...

Embodiment 2

[0026] Add T chain link: 121 parts of phenyltriethoxysilane into the three-necked bottle; D chain link: 28 parts of diphenyldiethoxysilane, 40 parts of dimethyldimethoxysilane; M chain link: vinyl 10 parts of dimethylmethoxysilane, 20 parts of hexamethyldisiloxane; 50 parts of 0.5% sulfuric acid aqueous solution was added dropwise at room temperature, and the dripping was completed in 30 minutes. After completion, the temperature was raised to 50°C for 1 hour, and then the temperature was raised to 70°C Reaction 5h. The reaction solution was left to stand for stratification, the organic layer was washed to neutrality, dried with 5 parts of calcium chloride and filtered to collect the filtrate, the filtrate was reacted at 120°C for 5h with 0.03% of the weight of the filtrate, and the temperature was raised to 180°C for decomposition The catalyst was removed, and low-molecular substances were removed under negative pressure conditions of -0.096MPa to obtain a colorless and trans...

Embodiment 3

[0027] Add T chain link: 100 parts of phenyltrimethoxysilane into the three-necked bottle; D chain link: 50 parts of diphenyldimethoxysilane; M link: 16 parts of vinyldimethylmethoxysilane, hexamethoxy 20 parts of base disiloxane; 8 parts of macroporous strongly acidic cation exchange resin, 50 parts of deionized water; the temperature was raised to 80° C., and the reaction was carried out at this temperature for 8 hours. The reaction solution was filtered, the filtrate was allowed to stand and separated, the water layer was removed, the organic layer was dried with 5 parts of calcium chloride and filtered, and the filtrate was reacted with 0.5 parts of 1% KOH at 140°C for 6 hours, and CO 2 Filter the reaction solution until the reaction solution is neutral, and remove low-molecular substances from the filtrate under negative pressure conditions of 180°C / -0.096MPa to obtain a colorless and transparent oily product. Product refractive index n D =1.5421, the vinyl content is 2....

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Abstract

The invention discloses phenyl MDT silicon resin and a preparation method thereof. The phenyl MDT silicon resin adopts single-group organic silane as a M link, adopts two-group organic silane as a D link and adopts three-group organic silane as a T link, wherein at least one of the D link or the T link is the phenyl silane, and the phenyl silane is collectively hydrolyzed under an acidic catalyst and concentrated under an alkaline catalyst. Raw materials for the phenyl MDT silicon resin are available, no strong corrosive substance is generated in the reaction process, and the requirement on equipment and operation is low. The preparation method comprises the following steps of adding the acidic catalyst in the mixed liquor of the M-link silane, the D-link silane and the T-link silane. The M link, the D link and the T link are unnecessary to drop into a reactor respectively, so that the operation step is simple, the procedure is saved, the production efficiency can be improved, and the industrialized mass production can be realized. The refractive index nD of the prepared phenyl MDT silicon resin is more than 1.53.

Description

technical field [0001] The invention belongs to the technical field of polymer chemistry, and relates to a phenyl MDT silicone resin and a preparation method thereof. Background technique [0002] In recent years, LED has developed rapidly as a semiconductor light-emitting device. LED lighting has been favored by more and more people for its long life, low energy consumption, and high efficiency. Therefore, LED lighting is bound to become a new mainstream lighting form. Among the components of the LED, its packaging structure and its packaging glue play a crucial role in the quality of the product. Silicone rubber and silicone resin are ideal packaging materials for LED packaging. In order to improve the light extraction rate of the LED chip and effectively protect the chip, it is required that the refractive index and the strength of the LED packaging adhesive be increased as much as possible. [0003] At present, there are few reports on the use of phenyl MDT silicone res...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/18C08G77/06C09K3/10
Inventor 暴玉强叶波熊婷李步春王有治
Owner CHENGDU GUIBAO SCI & TECH
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