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Silicone pressure-sensitive adhesive and preparation method thereof

A silicone pressure-sensitive adhesive and solvent technology, used in adhesives and other directions, can solve the problems of increased cross-linking, failure, and brittleness of adhesives, and achieve the effects of simple synthesis process, easy ratio, and excellent heat resistance.

Active Publication Date: 2019-06-25
芜湖三维航空材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the heat resistance of silicone pressure-sensitive adhesives synthesized from methyl silicone resins is not good. This type of pressure-sensitive adhesives may fail when used for a long time at high temperatures exceeding 300°C. The thermal decomposition of organic groups such as radicals increases the crosslinking degree of the adhesive sharply.
Using phenyl silicone resin instead of methyl silicone resin has slightly better heat resistance, but it will appear debonding and brittle after long-term use under ultra-high temperature conditions higher than 300 °C

Method used

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  • Silicone pressure-sensitive adhesive and preparation method thereof
  • Silicone pressure-sensitive adhesive and preparation method thereof
  • Silicone pressure-sensitive adhesive and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] (1) Synthesis of fluorine-containing phenyl silicone resin

[0061] 5L three-neck flask, equipped with thermometer, reflux condenser and constant pressure dropping funnel, heated by oil bath. Add 800g of toluene and 650g of pentafluorostyrene in sequence, stir and dissolve, and add 2.6g of chloroplatinic acid catalyst under nitrogen protection. Turn on the heating, and after the temperature rises to 80°C, add 510 g of methyldichlorohydrogensilane dropwise, and the addition is completed in 30 minutes, and the dropping time is controlled at about 1 hour. After the dropwise addition, the insulation reaction was continued for 2 hours. After the reaction, the solvent and unreacted methyldichlorosilane were distilled off, and the 132°C fraction (3.75kPa) was collected by distillation under reduced pressure to obtain 950g of pentafluorophenethyldimethylchlorosilane. The purity of the product as measured by gas chromatography was 96.6 %, yield 90.9%.

[0062] In a 250mL Erle...

Embodiment 2

[0075] (1) The steps for synthesizing fluorine-containing phenyl silicone resin are the same as in Example 1.

[0076] (2) Polycondensation reaction

[0077] 2L three-neck flask, equipped with thermometer, water separator and reflux condenser, constant pressure addition funnel, heated by oil bath. Add 170g of 107 gum and 165g of xylene in sequence, stir and raise the temperature to 90°C, and add 1.5g of dibutyltin dilaurate (DBTL). Nitrogen was blown, and a solution of 1 g of dimethyldimethoxysilane dissolved in 20 g of xylene was added dropwise, and the addition was completed in 30 minutes, and the reaction was kept for 3 hours. Then, a solution of 325 g of fluorine-containing phenyl silicone resin dissolved in 200 g of xylene was added, the temperature was raised to 138° C., and the reaction was carried out by reflux and water separation for 24 h.

[0078] (3) Post-processing

[0079] Add 15 g of hexamethyldisilazane and 6.5 g of isopropanol to the polycondensation produc...

Embodiment 3

[0088] (1) Polycondensation reaction

[0089] 2L three-neck flask, equipped with thermometer, water separator and reflux condenser, constant pressure addition funnel, heated by oil bath. Add 169g of 107 gum and 180g of xylene in turn, stir and raise the temperature to 80°C, and add 1.5g of dibutyltin dilaurate (DBTL). Nitrogen was blown, and a solution of 1 g of dimethyldimethoxysilane dissolved in 20 g of xylene was added dropwise, and the addition was completed in 30 minutes, and the reaction was kept for 3 hours. Then, a solution of 320 g of fluorine-containing phenyl silicone resin dissolved in 200 g of xylene was added, the temperature was raised to 140° C., refluxed and water separated for 48 h.

[0090] (2) Post-processing

[0091] Add 15 g of hexamethyldisilazane and 6.5 g of isopropanol to the polycondensation product, and keep it warm for 5 hours. After the reaction is finished, the reaction is stopped, cooled, and discharged to obtain a high-temperature resistant...

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Abstract

The invention discloses a preparation method of an organic silicon pressure sensitive adhesive. Fluorine-containing phenyl silicone resin and silicone rubber (107 glue) are taken as the raw materials;and the organic silicon pressure sensitive adhesive is prepared through condensation polymerization. A certain amount of fluorine containing phenyl is added into the structure of the product, the obtained pressure sensitive adhesive has an excellent high temperature resistant performance and bonding performance; moreover, the preparation technology is simple, the equipment requirements are low, and the preparation method is suitable of industrial production.

Description

technical field [0001] The invention relates to a high-temperature-resistant silicone pressure-sensitive adhesive and a preparation method thereof, belonging to the field of silicone material and adhesive preparation. Background technique [0002] The active ingredient of silicone pressure-sensitive adhesive is the product of polycondensation reaction between silicone resin and silicone rubber (also known as 107 glue). It is diluted to a certain solid content by adding organic solvent, and then added crosslinking agent and other additives to obtain the product. Among them, the main function of silicone rubber is to give the pressure-sensitive adhesive the necessary cohesion. 107 rubber, which is commonly used in the synthesis of silicone pressure-sensitive adhesives, has a number-average molecular weight of 100,000 to 500,000. It is generally colorless and transparent at room temperature. It is an extremely viscous liquid or semi-solid; the molecular structure of silicone re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J183/10C08G77/06C08G77/24C08G77/32C08G77/44
CPCC08G77/06C08G77/24C08G77/32C08G77/44C08G77/80C09J183/10
Inventor 李战雄孙弋纵亚坤
Owner 芜湖三维航空材料有限公司
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