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

A silicone pressure-sensitive adhesive, stability 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 inhibit the occurrence of reverse reactions and improve the use performance. Good, the effect of improving stability

Active Publication Date: 2018-06-08
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

[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 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;

[0033] Step 2) Remove water

[0034] The temperature in the reactor is lowered to room temperature, and the composition of 1.5Kg is added to the reactor under stirring. Water agent A", continue to stir for more than 30 minutes;

[0035] Step 3) Removal of Residual Hydroxyl

[0036]Under nitrogen protection and stirring state, the reaction tempe...

Embodiment 2

[0048] Step 1) polycondensation reaction

[0049] 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;

[0050] Step 2) Remove water

[0051] Keep the temperature in the reactor at room temperature, add 1.0Kg of water remover ALT-201 into the reactor under stirring, and continue stirring for more than 30 minutes;

[0052] Step 3) Removal of Residual Hydroxyl

[0053] Under nitrogen protection and stirring state, the reaction temperature was maintained at 50°C, 5000g of hexa...

Embodiment 3

[0064] Embodiment 3 (improves the stability of finished product silicone pressure-sensitive adhesive)

[0065] Step 1) Remove water

[0066] Put 1000Kg of domestic finished silicone pressure-sensitive adhesive in the reaction kettle, add 1.0Kg of water remover ALT-202 into the reaction kettle while stirring, and continue stirring for more than 30 minutes;

[0067] Step 2) remove residual hydroxyl

[0068] Under the protection of nitrogen and stirring, the reaction temperature was reduced to 50°C, and 5000g of tetramethyldivinyldisilazane was added to stir the reaction for 1 hour, then the temperature was raised to 90°C, and the flow rate of nitrogen was increased to drive off the reaction generated NH3 cannot detect the ammonia component until the outlet of the condenser; when the ammonia removal is completed, keep the adhesive reaction system at about 70°C, and start to deactivate the polycondensation catalyst;

[0069] Step 3) Catalyst deactivation treatment

[0070] Keep...

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Abstract

The invention discloses a method for improving the stability of organic silicon pressure-sensitive adhesive for protective film. The method comprises the following steps: (1) water removal: adding a dehydrating agent containing oxazolidine compounds into a reaction system to remove the residual water in the reaction system; (2) hydroxy group removal: adding a hydroxy removing agent containing silazane compounds into the reaction system; (3) radical inactivation of catalyst: (a) when primary amine or secondary amine is taken as the condensation polymerization catalyst, maintaining the adhesive reaction system to be at a temperature of 70 DEG C or so under a nitrogen gas atmosphere, reacting primary amine or secondary amine with aldehyde, ketone, and lower carboxylic acid to generate Schiff base, reacting the generated unstable Schiff base with diethyl malonate to convert the Schiff base into beta-amino acid without catalytic activity; (b) when secondary amine or tertiary amine is taken as the condensation polymerization catalyst, adding an acidic substance, which can react with secondary amine or tertiary amine to generate stable compounds, into the reaction system; (4) removing residual micromolecular substances in vacuum.

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 can easily lead to The temperature resistance of the product is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/34C09J183/04
CPCC08G77/34C08G77/38C09J183/04
Inventor 潘成诚
Owner ANHUI MINGXUN NEW MATERIAL TECH
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