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Silicone resin containing alkenyl and preparation method thereof

A technology of silicone resin and alkenyl silicon, which is applied in the field of organic silica gel materials, can solve the problems of luminous flux reduction, molecular structure deformation, and poor heat resistance of light-emitting devices, and achieve M/Q ratio and easy structure control, narrow molecular weight distribution, and improved The effect of mechanical strength

Active Publication Date: 2013-05-08
汕头海洋第一聚酯薄膜有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, some people have used MQ silicone resin to package light-emitting elements. However, with the rapid development of LED and other light-emitting devices in lighting applications in recent years, the requirement for high brightness has led to increased heat generation or shorter wavelengths of light.
However, the previous MQ silicone resin material for packaging cannot meet the high heat requirements of current light-emitting elements, and its heat resistance is relatively poor, which makes the molecular structure of the packaging colloid easily deformed, resulting in cracks and yellowing inside the colloid, which directly lead to light emission. The luminous flux of the device decreases rapidly with the cumulative working time, which leads to a series of problems such as low light extraction efficiency and short service life

Method used

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  • Silicone resin containing alkenyl and preparation method thereof
  • Silicone resin containing alkenyl and preparation method thereof
  • Silicone resin containing alkenyl and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 40 grams of distilled water, 120 grams of absolute ethanol, and 25 grams of 37% concentrated hydrochloric acid into a four-neck flask with stirring, reflux condenser, thermometer and dropping funnel, and stir to mix. Then add 130 grams of hexamethyldisiloxane (capping agent) and 39.6 grams of methylvinyldimethoxysilane, raise the temperature to 60 ° C, hydrolyze for 1 hour, and add 208.33 grams of ethyl orthosilicate dropwise under reflux (tetrafunctional organosilicon monomer), continue to stir for 1 hour of hydrolysis reaction. After the hydrolysis reaction was completed, 400 g of isododecane was added as an extractant. After the extraction reaction was performed for 3 hours, the mixture was allowed to stand for stratification, the water phase was removed, and the organic phase was washed with distilled water until neutral. The neutral organic phase was distilled under reduced pressure to remove the low boilers to obtain a colorless and transparent vinyl-containin...

Embodiment 2

[0038] Add 50 grams of distilled water, 120 grams of absolute ethanol, and 20 grams of 37% concentrated hydrochloric acid into a four-neck flask with stirring, reflux condenser, thermometer and dropping funnel, and stir to mix. Then add 150 grams of dodecamethylpentasiloxane and 12.1 grams of methylvinyldimethoxysilane, raise the temperature to 70 ° C, hydrolyze for 1.5 hours, add 208.33 grams of methyl orthosilicate dropwise under reflux, and continue stirring Hydrolysis reaction 2.5h. After the hydrolysis reaction was completed, 100 g of isohexadecane was added as an extraction agent. After the extraction reaction was completed for 0.5 h, the mixture was allowed to stand for stratification, the water layer was removed, and the organic phase was washed with distilled water until neutral. The neutral organic phase was distilled off under reduced pressure to remove low boilers to obtain vinyl-containing solid silicone resin.

[0039]

Embodiment 3

[0041] Add 50 grams of distilled water, 120 grams of absolute ethanol, and 20 grams of 37% concentrated hydrochloric acid into a four-neck flask with stirring, reflux condenser, thermometer and dropping funnel, and stir to mix. Then add 55 grams of tetramethyldivinyldisiloxane and 12.1 grams of octenyl trimethoxysilane, raise the temperature to 60 ° C, and hydrolyze for 2.5 hours, add 208.33 grams of ethyl orthosilicate dropwise under reflux, and continue stirring Hydrolysis reaction 1.5h. After the hydrolysis reaction was completed, 300 g of hexamethyldisiloxane was added as an extraction agent. After the extraction reaction was completed for 0.5 h, the mixture was allowed to stand for stratification, the water layer was removed, and the organic phase was washed with distilled water until neutral. The neutral organic phase was distilled off under reduced pressure to remove low boilers to obtain octenyl-containing silicone resin.

[0042]

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Abstract

The invention relates to a field of silica gel materials, and discloses silicone resin and a preparation method thereof. The silicone resin is the silicone resin containing an alkenyl active group and having a three-dimensional mesh-like structure. The method comprises co-hydrolyzing an end-capping reagent and the silane agent containing the alkenyl functional group in the presence of an acid catalyst, adding tetrafunctional organic silicon monomer in drops, performing a hydrolysis-condensation reaction, extracting, cleaning, and distilling to obtain the silicone resin solution containing the alkenyl. The silicone resin provided by the invention not only improves adhesion, reinforcement and other aspects of performance with metal materials and inorganic materials, but also has good compatibility and dispersibility. The method for preparing the silicone resin provided by the invention uses a nontoxic and harmless extractant to substitute toluene used in prior art, and thus does not cause harm to human and pollute the environment; and the silicone resin is not easy to gel, and wide in application.

Description

technical field [0001] The invention relates to a silicone resin material, in particular to an organic silica gel material used for packaging light-emitting elements. Background technique [0002] Light-emitting devices such as light-emitting diodes (LEDs) are emerging environmentally friendly light sources, and countries all over the world are actively promoting their use. In addition to the function of protecting the light-emitting element from the outside, this type of material for light-emitting element encapsulation is also required to have high transparency in order to prevent the brightness of the light-emitting element from decreasing. At present, materials such as epoxy resin and polymethyl methacrylate with good transparency are often used in production as materials for packaging light-emitting elements. There is also an organic silica gel material (CN 101414655) with a high refractive index, and the luminous flux can be increased by 5-8%. However, the above pack...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08L83/07C09K3/10
Inventor 曹坚林
Owner 汕头海洋第一聚酯薄膜有限公司
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