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

A silicon pressure-sensitive adhesive and stability technology, applied in the direction of adhesives, etc., can solve problems such as viscosity and other use performance slowly changing, unable to meet use requirements, unstable use performance, etc., to inhibit the occurrence of reverse reaction and use performance. Good and stable temperature resistance and storage performance

Active Publication Date: 2018-07-31
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
Comparison scheme
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 200Kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of about 8000mPa.s and 300Kg of nM / nQ MQ resin with Mn of 0.75 about 5000g / mol, Mw about 18000g / mol and hydroxyl content of about 3%, continued to stir for 30min under the protection of nitrogen, then raised the temperature to about 135°C and kept the reflux for stable reaction for about 210min, during the reaction The generated water is continuously discharged through the Dean-Stark trap or U-shaped pipe trap;

[0034] Step 2) Remove water

[0035] Lower the temperature in the reactor to about 40°C, add 1.2Kg of dimethyl acetone into the reactor while stirring, and then add 150g of acetic acid after stirring for 10 minutes and continue stirring for more than 30 minutes;

[0036] Step 3) Removal of Residual Hydroxyl

[0037] Maintain the reaction temperatu...

Embodiment 2

[0051] Step 1) polycondensation reaction

[0052] 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;

[0053] Step 2) Remove water

[0054] Keep the temperature in the reactor at room temperature, add 1.0Kg of dewatering agent methyl ethyl acetone to the reactor under stirring, add 150g of acetic acid after stirring for 10 minutes and continue stirring for more than 30 minutes;

[0055] Step 3) Removal of Residual Hydroxyl

[0056] Under nitrogen protection and stirring, ...

Embodiment 3

[0069] Embodiment 3 (improves the stability of finished product silicone pressure-sensitive adhesive)

[0070] Step 1) Remove water

[0071] Put 1000Kg of domestic finished silicone pressure-sensitive adhesive in the reaction kettle, add 1.5Kg of water remover diethyl acetone into the reaction kettle under stirring, add 250g of acetic acid after stirring for 10 minutes and continue stirring for more than 30 minutes ;

[0072] Step 2) remove residual hydroxyl

[0073] Lower the reaction temperature to 50°C under nitrogen protection and stirring, add 6000g of isocyanatotripropylpropoxysilane and stir for 1 hour, keep the adhesive reaction system at about 70°C, and start the polycondensation catalyst Inactivation;

[0074] Step 3) Catalyst deactivation treatment

[0075] 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...

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Abstract

The invention relates to a method for improving the stability of an organic silicon pressure-sensitive adhesive for a protecting film. The method comprises the following steps of (1) water removal: a water removal agent containing a ketal type or acetal type compound is added; (2) hydroxyl removal: a silicon hydroxyl removal agent containing an isocyanate group alkyl alkoxy silane type compound is added; (3) catalyst thorough inactivation: (a) when primary amine or secondary amine is used as a polycondensation catalyst, the primary amine or secondary amine and aldehydes or ketone low-grade carboxylic acid take reaction to generate Schiff base; then, the generated unstable Schiff base and diethyl malonate take a reaction, so that the Schiff base becomes Beta-amino acid without catalytic activity; (b) when secondary amine or tertiary amine is used as a polycondensation catalyst, an acidic substance capable of forming a stable compound with the secondary amine or tertiary amine through reaction is added into a reaction system; (4) residual acidic substance neutralization: sodium alkoxide is added for neutralizing residual acidic substances in the adhesive; (5) vacuum removal of residual small-molecule substances.

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. 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 sources, poor research f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/34C08G77/32C08G77/44C09J183/04
CPCC08G77/32C08G77/34C08G77/44C09J183/04
Inventor 潘成诚
Owner ANHUI MINGXUN NEW MATERIAL TECH
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