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Synthesis method for polymer acrylate resin with photosensitive self-catalytic activity

An acrylate, autocatalytic technology, applied in non-polymer adhesive additives, non-polymer organic compound adhesives, adhesive additives, etc., can solve the problem of poor toughness of cured products, poor flexibility of adhesive layer, Problems such as poor surface dryness

Active Publication Date: 2019-02-22
YANTAI DARBOND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, acrylate light-curable adhesives also have their own unavoidable shortcomings, such as poor surface dryness caused by oxygen inhibition on the surface of the adhesive layer after curing, poor flexibility of the adhesive layer, and many other problems.
In order to solve the above shortcomings, rubber toughening resins are widely used in acrylate light-curable adhesives, but the current common rubber tougheners only improve the toughness of the cured adhesive layer, and need to add small molecule photoinitiators to the light-curing system. Accelerator accelerator, even so, can not balance the problem of poor toughness and poor surface drying of acrylate light-curable adhesive cured products

Method used

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  • Synthesis method for polymer acrylate resin with photosensitive self-catalytic activity
  • Synthesis method for polymer acrylate resin with photosensitive self-catalytic activity
  • Synthesis method for polymer acrylate resin with photosensitive self-catalytic activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 430g of hydroxyl-terminated polybutadiene liquid rubber, add 30g of tert-butyldiphenylchlorosilane and 0.5g of diethyltetramethylimidazole under nitrogen protection, and react at 30°C for 4 hours to obtain silicon ether-protected rubber at both ends. the pretreatment;

[0026] Add the above reactant to 22 g of HBr with a concentration of 40%, and react at 70°C for 3 hours to obtain a halogenated hydrocarbon protected by silicon ether at both ends;

[0027] Add 55 g of N-methyl-N-hydroxyethyl-p-toluidine (CAS No. 2842-44-6) to the halogenated hydrocarbon protected with silicon ether at both ends prepared above, and react at 30°C under nitrogen protection for 3 hours;

[0028] Dissolve the product of the third step in tetrahydrofuran (THF) solvent, add catalyst tetraalkylammonium fluoride (TBAF) 0.26g, react at 25°C for 3-4h, and finally remove the solvent THF by rotary evaporation; after the above rotary evaporation The obtained product was vacuumized at 115°C for ...

Embodiment 2

[0030] Take 430g of hydroxyl-terminated polybutadiene liquid rubber, add 35g of tert-butyldiphenylchlorosilane and 1.5g of diethyltetramethylimidazole under nitrogen protection, and react at 40°C for 2 hours to obtain silicon ether-protected rubber at both ends. the pretreatment;

[0031] Add 20 g of the above reactant to 40% HBr, and react at 70°C for 3 hours to obtain a halogenated hydrocarbon protected by silicon ether at both ends;

[0032] Add 70 g of N-methyl-N-hydroxyethyl-p-toluidine (CAS No. 2842-44-6) to the halogenated hydrocarbon protected with silicon ether at both ends prepared above, and react at 30°C under nitrogen protection for 3 hours;

[0033] Dissolve the product of the third step in tetrahydrofuran (THF) solvent, add catalyst tetraalkylammonium fluoride (TBAF) 0.50g, react at 25°C for 3-4h, and finally remove the solvent THF by rotary evaporation; after the above rotary evaporation The obtained product was vacuumized at 110°C for 3 hours to remove moistu...

Embodiment 3

[0035] Take 430g of hydroxyl-terminated polybutadiene liquid rubber, add 30g of tert-butyldiphenylchlorosilane and 1.0g of diethyltetramethylimidazole under nitrogen protection, and react at 40°C for 4 hours to obtain silicon ether-protected rubber at both ends. the pretreatment;

[0036] Add 26 g of the above reactant to 40% HBr, and react at 70°C for 3 hours to obtain a halogenated hydrocarbon protected by silicon ether at both ends;

[0037] Add 48 g of N-methyl-N-hydroxyethyl-p-toluidine (CAS No. 2842-44-6) to the halogenated hydrocarbon protected with silicon ether at both ends prepared above, and react at 30°C under nitrogen protection for 3 hours;

[0038] Dissolve the product of the third step in tetrahydrofuran (THF) solvent, add catalyst tetraalkylammonium fluoride (TBAF) 0.38g, react at 25°C for 3-4h, and finally remove the solvent THF by rotary evaporation; after the above rotary evaporation The obtained product was vacuumized at 113°C for 2.5 hours to remove mois...

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Abstract

The invention relates to a synthesis method for polymer acrylate resin with photosensitive self-catalytic activity. The synthesis method comprises the synthesis steps: adding tert-butyldiphenylsilylchloride and 2-ethyl-4-methylimidazole serving as a catalyst into hydroyl-terminated polybutadiene liquid rubber under the protection of nitrogen, then, carrying out a reaction with HBr for 3-4 h, carrying out a reaction with an active unit containing a tertiary amine structure at 30 DEG C under the protection of nitrogen for 3-5 h, dissolving the product into a tetrahydrofuran solution, adding tetraalkyl ammonium fluoride serving as a catalyst, removing the solvent by rotary evaporation, adding isocyanate, finally, adding hydroxyl-containing acrylate, and carrying out a reaction at 70-80 DEG Cfor 1-3 h to obtain the polymer acrylate resin with photosensitive self-catalytic activity. The acrylate resin disclosed by the invention has the advantages of improving poor surface dry while improving the toughness after being cured by using an acrylate photosetting adhesive.

Description

technical field [0001] The invention relates to the synthesis of a high molecular weight acrylate resin with photosensitive self-catalysis activity, which belongs to the field of light-curing materials. Background technique [0002] Acrylic light-curing adhesives are suitable for bonding glass, plastic or metal. The cured product has good transparency and fast curing speed, which can realize many advantages such as automatic production line and high productivity, and is widely used in electronic and electrical industries. However, acrylate light-curable adhesives also have their own unavoidable shortcomings, such as poor surface dryness caused by oxygen inhibition on the surface of the adhesive layer after curing, poor flexibility of the adhesive layer, and many other problems. In order to solve the above shortcomings, rubber toughening resins are widely used in acrylate light-curable adhesives, but the current common rubber tougheners only improve the toughness of the cure...

Claims

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Application Information

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IPC IPC(8): C08G18/67C08G18/69C08G18/73C09J4/06C09J11/04C09J11/06C08C19/25C08C19/16C08C19/22
CPCC08C19/16C08C19/22C08C19/25C08G18/672C08G18/73C09J4/06C09J11/04C09J11/06C08G18/696
Inventor 陈加立王建斌陈田安
Owner YANTAI DARBOND TECH
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