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A method for extending the stability of silicone pressure-sensitive adhesives

A silicone pressure-sensitive adhesive, stability technology, applied in the direction of adhesives, etc., can solve problems such as viscosity and other performance changes slowly, cannot meet the use requirements, and use performance is unstable, so as to inhibit the occurrence of reverse reactions and achieve better results. Good, good performance

Active Publication Date: 2018-08-24
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 extending the stability of silicone pressure-sensitive adhesives
  • A method for extending the stability of silicone pressure-sensitive adhesives
  • A method for extending the stability of silicone pressure-sensitive adhesives

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Step 1) polycondensation reaction

[0034]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% 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;

[0035] Step 2) Remove water

[0036] The temperature in the reactor was lowered to room temperature, and 1.2 Kg of ethyl orthoacetate was added to the reactor under stirring, and after stirring for 10 minutes, 200 g of acetic acid was added and the stirring was continued for more than 30 minutes;

[0037] Step 3) Removal of Residual Hydroxyl

[0038] Maintain the reaction ...

Embodiment 2

[0052] Step 1) polycondensation reaction

[0053] 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;

[0054] Step 2) Remove water

[0055] Keep the temperature in the reaction kettle at room temperature, add 1.0Kg of water remover ethyl orthoformate to the reaction kettle under stirring, add 200g of formic acid after stirring for 10 minutes and continue stirring for more than 30 minutes;

[0056] Step 3) Removal of Residual Hydroxyl

[0057] Maintain the reaction tempera...

Embodiment 3

[0070] Embodiment 3 (improves the stability of finished product silicone pressure-sensitive adhesive)

[0071] Step 1) Remove water

[0072] Put 1000Kg of domestic finished silicone pressure-sensitive adhesive in the reaction kettle, add 1.5Kg of water remover methyl orthoacetate into the reaction kettle under stirring, add 250g of acetic acid after stirring for 10 minutes and continue stirring for more than 30 minutes ;

[0073] Step 2) remove residual hydroxyl

[0074] Lower the reaction temperature to 50°C under nitrogen protection and stirring, add 7000g of methyl trimethylsilylacetate and stir for 1 hour, keep the adhesive reaction system at about 70°C, and start to deactivate the polycondensation catalyst;

[0075] Step 3) Catalyst deactivation treatment

[0076] Keep the adhesive reaction system at about 70°C under a nitrogen reaction atmosphere, add 10% acetyl chloride toluene solution containing 2.5Kg acetyl chloride to the reaction kettle under stirring, and conti...

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Abstract

The invention provides a method for expanding stability of an organosilicone pressure-sensitive adhesive. The method comprises the following steps: (1) removing water; (2) removing hydroxyl, namely adding a silicon hydroxyl remover containing a trialkyl silicon carboxylate compound to a reaction system to reduce residual oxhydryl in an adhesive molecular structure; (3) thoroughly inactivating a catalyst, wherein the step is performed according to the following two conditions: when primary amine or secondary amine is utilized as a polycondensation catalyst, enabling the primary amine or the secondary amine to react with aldehydes or ketones and low-level carboxylic acid to generate a schiff base in a nitrogen reaction atmosphere, enabling the generated instable schiff base to react with diethyl malonate, and changing the schiff base into beta-amino acid free of catalytic activity; and when secondary amine or tertiary amine is utilized as the polycondensation catalyst, adding an acid substance which can react with the secondary amine or the tertiary amine to form a stable compound to the reaction system; (4) removing residual small molecular substances in vacuum; and (5) neutralizing the residual acid substance.

Description

technical field [0001] The invention relates to the technical field of adhesives, in particular to a method for extending 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): C09J183/04C08G77/38C08G77/32
CPCC08G77/32C08G77/38C09J183/04
Inventor 潘成诚
Owner ANHUI MINGXUN NEW MATERIAL TECH
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