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A kind of method for improving the stability of silicone pressure-sensitive adhesive

A silicone pressure-sensitive adhesive and stability technology, applied in the field of adhesives, can solve problems such as viscosity and other use performance slowly changing, unable to meet use requirements, unstable use performance, etc., to ensure stability and use. good performance, 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 kind of method for improving the stability of silicone pressure-sensitive adhesive
  • A kind of method for improving the stability of silicone pressure-sensitive adhesive
  • A kind of method for improving the stability of silicone pressure-sensitive adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1) polycondensation reaction

[0032]Put 100Kg of toluene and 200Kg of xylene into the reactor, add 500g of diethylamine, stir evenly, then add 300Kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of about 6500mPa.s and 200Kg 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;

[0033] Step 2) Dehydration and Residual Hydroxyl Removal

[0034] Lower the temperature in the reactor to about 45°C, and add 6Kg of NH to the reactor while stirring 2 (CH 2 ) 6 NHCH 2 -Si(CH 3 ) 2 -OCH 2 CH 3 , stirring and reacting for more than 90 minutes, then heating up to about 70°C, and starting to deactivate the polycondensation catalyst;

[0035] Step 3) Ca...

Embodiment 2

[0046] Step 1) polycondensation reaction

[0047] 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;

[0048] Step 2) remove water and remove hydroxyl

[0049] Keep the temperature in the reactor at 40°C to 45°C, add 6.5Kg of (CH 3 CH 2 ) 2 N-CH 2 -Si(CH 3 ) 2 -OCH 2 CH 3 , stirred for more than 90 minutes, then raised the temperature to about 70°C, and started to deactivate the polycondensation catalyst;

[0050] Step 3) Catalyst deactivation treatment

[0051] K...

Embodiment 3

[0060] Embodiment 3 (improves the stability of finished product silicone pressure-sensitive adhesive)

[0061] Step 1) remove water and remove hydroxyl

[0062] Put 1000Kg of a domestically produced silicone pressure-sensitive adhesive in the reactor, and add 10.0Kg of CH 3 (CH 2 ) 3 N-CH 2 -Si(CH 3 ) 2 -OCH 3 , then heat up to about 40°C and continue to stir for more than 90min;

[0063] Step 2) Catalyst deactivation treatment

[0064] Keep the adhesive reaction system at about 70°C under a nitrogen reaction atmosphere, add 5% HCl ether solution containing 5.0Kg of pure HCl to the reaction kettle under stirring, and continue stirring for 90 minutes;

[0065] Step 3) Neutralize the remaining acidic substances in the adhesive: After step 2) is completed, reduce the temperature of the reactor to below 50°C, and then gradually add the toluene dispersion containing 5% sodium isopropoxide until the adhesive is detected by sampling. The viscous system is neutral, continue t...

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Abstract

The invention discloses a method for improving stability of an organosilicone pressure-sensitive adhesive. The method comprises steps as follows: step 1), removal of water and hydroxyl: a water and hydroxyl removal agent containing alpha-functional group siloxane compounds is added to a reaction system; step 2), thorough inactivation of a catalyst: inactivation is performed in the following two ways: a) when primary amine or secondary amine is used as a condensation polymerization catalyst, the 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 acidic compounds are neutralized; step 4), residual small molecular substances are removed in the vacuum state.

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): C08G77/34C08G77/32
CPCC08G77/32C08G77/34
Inventor 潘成诚
Owner ANHUI MINGXUN NEW MATERIAL TECH
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