A method for improving the stability of silicone pressure-sensitive adhesives for protective films

A silicon pressure-sensitive adhesive and protective film technology, applied in the direction of adhesives, etc., can solve problems such as viscosity and other performance changes gradually, cannot meet the use requirements, and use performance is unstable, so as to achieve good use performance, convenience and practicality Performance, stable temperature resistance and storage performance

Active Publication Date: 2018-07-17
ANHUI MINGXUN NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, due to the limitations of technological level and equipment, it is actually difficult for domestic silicone pressure-sensitive adhesives to meet the requirements of these three aspects at the same time, especially for the inactivation treatment of amine catalysts, only by adding acetic acid and other substances for neutralization
During the coating and drying process of this silicone pressure-sensitive adhesive, the amine salt neutralized by acid substances will be re-decomposed into amines. Slowly decompose the polycondensed silicone adhesive part into silicone rubber and silicone resin, and the difference in migration rate of silicone rubber or silicone resin will slowly change the adhesive layer structure of the adhesive product, thereby resulting in poor performance of the silicone adhesive product. Instability, mainly manifested in poor temperature resistance, easy residual glue, viscosity and other performance will change slowly over time and even fail to meet the requirements of use

Method used

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  • A method for improving the stability of silicone pressure-sensitive adhesives for protective films
  • A method for improving the stability of silicone pressure-sensitive adhesives for protective films
  • A method for improving the stability of silicone pressure-sensitive adhesives for protective films

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Step 1) polycondensation reaction

[0033]Put 100Kg of toluene and 200Kg of xylene into the reactor, add 500g of diethylamine, stir evenly, then add 225Kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of about 8000mPa.s and 275Kg of nM / nQ MQ resin with Mn of 0.75 about 5000g / mol, Mw about 18000g / mol and hydroxyl content of about 3% was stirred for 30min under nitrogen protection, then heated to about 135°C and kept under reflux for a stable reaction of about 210min. During the reaction The generated water is continuously discharged through the Dean-Stark trap or U-shaped pipe trap;

[0034] Step 2) Dehydration and Residual Hydroxyl Removal

[0035] The temperature in the reactor is reduced to about 45°C, and 10Kg of trimethylacetoxysilane (Me 3 SiOAc), stirring and reacting for more than 90min, then heating up to about 70°C, and starting to deactivate the polycondensation catalyst;

[0036] Step 3) Catalyst deactivation treatment

[0037] Keep the adh...

Embodiment 2

[0049] Step 1) polycondensation reaction

[0050] Put 100Kg of toluene and 200Kg of xylene into the reactor, add 500g of triethylamine, stir evenly, then add 200Kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of about 7000mPa.s and 300Kg of nM / nQ MQ resin with Mn of 0.80 about 5000g / mol, Mw about 18000g / mol and hydroxyl content of about 3% was stirred for 30min under nitrogen protection, then heated to about 135°C and kept under reflux for a stable reaction of about 210min. During the reaction The generated water is continuously discharged through the Dean-Stark trap or U-shaped pipe trap;

[0051] Step 2) remove water and remove hydroxyl

[0052] Keep the temperature in the reactor at 40°C to 45°C, and add 10.5Kg of trivinylacetoxysilane (Vi 3 SiOAc), stirring for more than 90min, then heating up to about 70°C, and starting to deactivate the polycondensation catalyst;

[0053] Step 3) Catalyst deactivation treatment

[0054] Keep the adhesive reaction syst...

Embodiment 3

[0065] Embodiment 3 (improves the stability of finished product silicone pressure-sensitive adhesive)

[0066] Step 1) remove water and remove hydroxyl

[0067] Place 1000Kg of a domestically produced silicone pressure-sensitive adhesive in a reactor, and add 12.0Kg of triethylacetoxysilane (Et 3 SiOAc), then be warming up to about 40 ℃ and continue to stir more than 90min;

[0068] Step 2) Catalyst deactivation treatment

[0069] Keep the adhesive reaction system at about 70°C under a nitrogen reaction atmosphere, add 5% HCl ether solution containing 1.5Kg HCl to the reaction kettle under stirring, and continue stirring for 90 minutes;

[0070] Step 3) Removal of Small Molecules

[0071] After step 2) is completed, raise the temperature of the reactor to 110°C or above, and then remove the small molecular substances in the adhesive reaction system from the reaction material under a vacuum condition of not less than -0.09MPa. less than 90min;

[0072] Step 4) Neutralize t...

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Abstract

The invention relates to a method for improving stability of an organosilicone pressure-sensitive adhesive for a protective film. The method comprises steps as follows: step 1), removal of water and hydroxyl: a water and hydroxyl removal agent containing organic acyloxy silane compounds is added to a reaction system to reduce water left in the adhesive and hydroxyl left on an adhesive structure; step 2), thorough inactivation of a catalyst: a) when primary amine or secondary amine is used as a condensation polymerization catalyst, an adhesive reaction system is kept at the temperature of about 70 DEG C at the nitrogen reaction atmosphere, primary amine or secondary amine and aldehydes, ketones or low-level carboxylic acid react to generate Schiff base, generated unstable Schiff base reacts with diethyl malonate, and Schiff base becomes beta-amino acid without catalytic activity; b), when secondary amine or tertiary amine is used as a condensation polymerization catalyst, acidic compounds which can react with secondary amine or tertiary amine to generate a stable compound are added to the reaction system; step 3), residual small molecular substances are removed in the vacuum state; step 4), neutralization of residual acidic compounds: sodium alcoholate is added to neutralize residual acidic compounds in the adhesive.

Description

technical field [0001] The invention relates to the technical field of adhesives, in particular to a method for improving the stability of silicone pressure-sensitive adhesives for protective films. Background technique [0002] Silicone pressure-sensitive adhesives are generally a high-performance pressure-sensitive material formed by polycondensation of hydroxyl-terminated polyorganosiloxane linear polymers under the action of a catalyst and MQ silicone resin with hydroxyl groups. Because of the structure, silicone pressure-sensitive adhesives have excellent high / low temperature resistance, excellent dielectric properties and aging resistance, and have low surface free energy and can stick to the surface of difficult-to-stick objects. Therefore, it is widely used. The preparation process of silicone pressure-sensitive adhesives is quite complicated. The silicone pressure-sensitive adhesives in the prior art are often caused by reasons such as insufficient raw material sou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J183/04C08G77/10
CPCC08G77/10C09J183/04
Inventor 潘成诚
Owner ANHUI MINGXUN NEW MATERIAL TECH
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