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Preparation method and application of silicon resin

A technology of resin and silicate, which is applied in the direction of adhesives, etc., can solve problems such as the decline of aging resistance, the development of silicone pressure-sensitive adhesive technology and the influence of research on the performance of pressure-sensitive adhesives, and the impact on the catalyst activity of pressure-sensitive adhesives. Content, the effect of improving aging resistance

Active Publication Date: 2022-04-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN1058739895A provides a method for end-capping MQ resins, using chlorosilanes in polar solvents to carry out end-capping reactions on MQ resins that have been obtained, which can effectively improve the end-capping efficiency of MQ resins, but does not mention that this method has The effect of reducing the silanol content
[0005] Patent CN102061142A provides a method for preparing MQ resin pressure-sensitive adhesives, MQ silicone resin is prepared by tetraethyl orthosilicate and trimethylchlorosilane, and then used as a raw material for silicone pressure-sensitive adhesives, but MQ is not mentioned Effects of Resin Hydroxyl Content on Properties of Pressure Sensitive Adhesives
[0006] Patent CN201310430580 provides a way to use silazane to treat the hydroxyl content of MQ resin, and apply it to LED packaging materials. Since silazane will have amine residues after hydrolysis, it may affect the catalyst activity of pressure-sensitive adhesives. Lead to decline in product aging resistance
[0007] Existing patents and documents have done more research on the synthesis method of MQ resin, but none of them have carried out the process development of MQ resin for silicone pressure-sensitive adhesives and studied its influence on the performance of pressure-sensitive adhesives

Method used

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  • Preparation method and application of silicon resin

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Experimental program
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Effect test

Embodiment 1

[0047] Add 304.6g of methyl orthosilicate, 210g of hexamethyldisiloxane and 160g of xylene into reactor A, and gradually add the mixed solution of 28.8g of deionized water and 1.8g of concentrated hydrochloric acid into the system after stirring , Control the reaction temperature at 35°C during the dropwise addition. After the dropwise addition was completed, the temperature was raised to 80°C for reflux reaction for 3 hours, and then the temperature was gradually raised to 100°C to distill out methanol and water. After the product was washed with deionized water to neutrality, the residual water and methanol in the system were removed by vacuum distillation to obtain Xylene solution of MQ resin.

[0048] Add 300g of methyltrimethoxysilane, 500g of tetramethyldisiloxane, and 1.2g of trifluoromethanesulfonic acid into reactor B, stir evenly, add 105g of deionized water dropwise, and heat up to 70°C to reflux after the dropwise addition After reacting for 4h, the hydrogen-conta...

Embodiment 2

[0051] In reactor A, add 350.6g tetraethyl orthosilicate oligomer (Si40), 230g hexamethyldisiloxane and 100g xylene, start stirring and mix 32.3g deionized water and 3.2g concentrated hydrochloric acid Gradually add it dropwise to the system, and control the reaction temperature at 40°C during the process. After the dropwise addition was completed, the temperature was raised to 80°C for reflux reaction for 3 hours, and then the temperature was gradually raised to 100°C to distill out ethanol and water, and after the product was washed with deionized water to neutrality, the residual water and ethanol in the system were removed by distillation under reduced pressure to obtain Resin solution in xylene.

[0052] Add 300 g of methyltriethoxysilane, 600 g of 1,1,3,3,5,5-hexamethyl 1,5-dihydro-trisiloxane, and 2.4 g of trifluoromethanesulfonic acid into reactor B , stirred evenly, added dropwise 135g of deionized water, after the dropwise addition was completed, the temperature was...

Embodiment 3

[0055]Add 416.6g of ethyl orthosilicate, 210g of hexamethyldisiloxane and 130g of xylene into reactor A, and gradually add a mixed solution of 30g of deionized water and 2.5g of concentrated hydrochloric acid dropwise into the system after stirring is started. During the process, the reaction temperature was controlled at 30°C. After the dropwise addition was completed, the temperature was raised to 80°C for reflux reaction for 3 hours, and then the temperature was gradually raised to 100°C to distill out ethanol and water. After the product was washed with deionized water until neutral, the remaining water and ethanol in the system were removed by distillation under reduced pressure to obtain Resin solution in xylene.

[0056] Add 300g of methyltrimethoxysilane, 550g of tetramethyldisiloxane, and 1.8g of trifluoromethanesulfonic acid into reactor B, stir evenly, add 120g of deionized water dropwise, heat up to 75°C and reflux after the dropwise addition After reacting for 5h...

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Abstract

The invention provides the preparation method of the MQ resin for the pressure-sensitive adhesive, and the prepared MQ resin can effectively improve the aging resistance of the pressure-sensitive adhesive. The preparation process comprises the following steps: a) preparing an MQ resin solution by taking silicate ester and an end-capping reagent as raw materials under an acidic condition; b) preparing a hydrogen-containing end-capping reagent by taking alkoxy silane and hydrogen-containing silane as raw materials; and c) treating the obtained MQ resin solution by using a self-made hydrogen-containing end-capping reagent under the action of a catalyst, and removing redundant solvents and small molecules under reduced pressure to obtain the MQ resin. The hydroxyl content of the prepared MQ resin is lower than 0.3 wt%, the alkoxy content is lower than 0.5 wt%, and the aging resistance of the organic silicon pressure-sensitive adhesive can be remarkably improved.

Description

technical field [0001] The invention relates to a preparation method of silicone resin, in particular to a preparation method of MQ resin. Background technique [0002] MQ resin is a special type of silicone resin, which is composed of monovalent trimethylsilyl (M) units and tetravalent (Q) units. MQ resin is usually obtained by the co-hydrolysis of silicate containing Q units and hexamethyldisiloxane containing M units. During the hydrolysis process, siloxy groups are hydrolyzed to generate silanol groups. Due to incomplete condensation, some silanol groups remain, and silicon The higher the hydroxyl content, the worse the aging resistance. How to reduce the hydroxyl content of MQ resin has always been a hot research direction in the industry. [0003] Patent US3772247 provides a batch method to prepare MQ resin synthesis method, the patent uses xylene as solvent and trimethylchlorosilane reflux reaction method can reduce the silanol content of MQ resin to below 1wt%. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/06C09J183/05
Inventor 马伟曹骏纪学顺李西龙马岩龙孙家宽
Owner WANHUA CHEM GRP CO LTD