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Preparation method of acrylate oligomer and polyurethane copolymerization emulsion pressure-sensitive adhesive for liquid crystal protection film

A technology of acrylates and oligomers, which is applied in the field of emulsion pressure-sensitive adhesive preparation, can solve the problems of not meeting the production requirements of clean technology, large residual amount of acrylic acid monomer, and poor mechanical properties of pressure-sensitive adhesives, etc., and achieves improvement Effects of monomer conversion, excellent mechanical properties and weather resistance, initial tack and viscosity optimization

Inactive Publication Date: 2012-06-27
CHANGZHOU BAOLI ADHESIVE
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  • Summary
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Japanese Patent JP2005136298-A relates to a pressure-sensitive adhesive prepared by adding a cross-linking agent containing isocyanate and epoxy groups and melamine to a polyacrylate emulsion synthesized by copolymerization of butyl acrylate, acrylonitrile and acrylic acid, but the Pressure-sensitive adhesive has poor mechanical properties, peel strength less than 200N / m, and poor stability, prone to residual glue; Chinese patent CN.1869139A introduces a preparation method of UV-curable waterborne polyurethane Diol, polyhydroxy carboxylic acid and aromatic diisocyanate are reacted to obtain a polyurethane prepolymer, and then hydroxyethyl methacrylate or hydroxypropyl methacrylate containing a polymerization inhibitor is added dropwise to the prepolymer to obtain a polyurethane-acrylic acid Ester oligomer, and finally through salt formation and emulsification in water to obtain water-based polyurethane acrylate adhesive
The problem of this method is that it is difficult to completely polymerize after the acrylic acid monomer is added, and the residual amount of acrylic acid monomer in the emulsion is large, which does not meet the production requirements of the clean process; Chinese patent CN.1355267A adopts IPN technology and seed emulsion polymerization to synthesize a PU / Polyurethane-modified acrylic adhesive with "core-shell" structure interpenetrated by PA polymer network. The method is to first synthesize a water-based polyurethane emulsion, then use the emulsion as a seed, add an emulsifier, and add an initiator in the form of dropwise addition. Emulsion polymerization with acrylic monomers and crosslinkers
An emulsifier needs to be added during the synthesis, and there is still the problem of low conversion rate of the monomer in the emulsion copolymerization

Method used

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  • Preparation method of acrylate oligomer and polyurethane copolymerization emulsion pressure-sensitive adhesive for liquid crystal protection film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: 4.0g N210 (polyoxypropylene diol-1000, difunctionality), 17.0g 330N (polyoxypropylene triol-3000, trifunctionality), 3g acrylate oligomer (Rf = H , Ri: n = 4, Rg = H, Rj: n = 2; the number average molecular weight is about 6500), and 1.55g of dihydroxypropionic acid (DMPA) were added to a three-necked flask, mixed and stirred, and placed in a 90°C water bath. After the solid particles are completely dissolved, vacuum dehydrate at a vacuum degree of -0.095Mpa for 1.0h. Cool down to 80°C, add 1.9g 1-methyl-2-pyrrolidone (NMP), 5.79g IPDI and 0.1% dibutyltin dilaurate, and the reaction time is 1~2h, until the value of NCO / OH in the system basically reaches the theoretical value When the prepolymer was obtained, the theoretical R value was 1.22, and 0.35g of trimethylolpropane (TMP) was added to react for 0.5~1h; the temperature was lowered to 50~60°C, and a proper amount of acetone was used to reduce the viscosity, and then 1.17g of triethylamine was added to ca...

Embodiment 2

[0016] 4.0g N210 (polyoxypropylene diol-1000, difunctionality), 5.0g 330N (polyoxypropylene triol-3000, trifunctionality), with 15g acrylate oligomer (Rf = H, Ri: n = 4, Rg = H, Rj: n = 2; the number average molecular weight is about 45000), and 1.55g of dihydroxypropionic acid (DMPA) were added to a three-necked flask, mixed and stirred, put in a 90°C water bath, and the solid particles After completely dissolving, vacuumize and dehydrate for 1.0h at a vacuum degree of -0.095Mpa. Cool down to 80°C, add 1.9g of 1-methyl-2-pyrrolidone (NMP), 5.79g of IPDI and 0.1% of dibutyltin dilaurate, the reaction time is 3~4h, until the value of NCO / OH in the system basically reaches the theoretical value When the prepolymer was obtained, the theoretical R value was 1.22, and 0.35g of trimethylolpropane (TMP) was added to react for 0.5~1h; the temperature was lowered to 50~60°C, and a proper amount of acetone was used to reduce the viscosity, and then 1.17g of triethylamine was added to ca...

Embodiment 3

[0018] Mix 7.0g N210 (polyoxypropylene diol-1000, difunctionality), 11.43g 330N (polyoxypropylene triol-3000, trifunctionality), 3g acrylate oligomer (Rf = H, Ri: n = 4, Rg = H, Rj: n = 2; the number average molecular weight is about 6500), and 1.55g of dihydroxypropionic acid (DMPA) were added to a three-necked flask and mixed and stirred, the reaction time was 1~2h, and placed at 90°C In a water bath, after the solid particles are completely dissolved, vacuum dehydrate at a vacuum degree of -0.095Mpa for 1.0h. Cool down to 80°C, add 1.9g 1-methyl-2-pyrrolidone (NMP), 6.0g IDI and 0.1% dibutyltin dilaurate, and react for 1~3h until the value of NCO / OH in the system basically reaches the theoretical value. Prepolymer, the theoretical R value is 1.22, add 1.0g acrylate oligomer (Rf = H, Ri: n = 0, Rg = CH3, Rj: n = 2; number average molecular weight is about 4000) to react 1~ 2h; lower the temperature to 50~60°C, first reduce the viscosity with an appropriate amount of acetone...

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Abstract

The invention relates to a preparation of an acrylate oligomer and polyurethane copolymerization emulsion pressure-sensitive adhesive for a liquid crystal protection film. The preparation comprises the following steps: 1, carrying out a grafting copolymerization reaction: reacting hydroxy monomers, a hydrophilic chain extender and isocyanate monomers, and adding acrylate oligomers to graft-copolymerize; 2, carrying out a crosslinking reaction through adding a polyhydroxy crosslinking agent to the graft-copolymerized prepolymer obtained in step 1; and 3, neutralizing to form a salt, emulsifying in water, and carrying out chain extension to form a transparent or semitransparent blue acrylate oligomer and aqueous polyurethane copolymerization emulsion pressure-sensitive adhesive. The synthesized acrylate oligomer and polyurethane copolymerization emulsion pressure-sensitive adhesive which has the advantages of excellent mechanical property and weatherability, good film forming ability, emulsion stability, and optimized compatibility of initial adhesion and cohesion can be applied to a liquid crystal protection film material, and no adhesive is residual on the liquid crystal surface when the protection film is stripped.

Description

technical field [0001] The invention relates to the technical field of preparation of water-based adhesives, in particular to a preparation method of an emulsion pressure-sensitive adhesive co-polymerized with acrylate oligomers and polyurethane for liquid crystal protective films. Background technique [0002] Liquid crystal protective film was first used to protect mobile phone screens, and then developed to protect LCD screens such as notebook screens. It is a protective film that can be used to protect mobile phone screens, LCD screens and other display equipment objects. The LCD protective film can not only make the LCD screen look new, bright and eye-catching, and have the effect of refurbishing the old machine, but also can protect the screen from water, dust, and fingerprints. [0003] The quality of the pressure-sensitive adhesive coated on the protective film plays a key role in the quality of the protective film. It must have moderate adhesion, good cohesion and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/62C09J175/06C09J175/08
Inventor 胡叔平胡文虎
Owner CHANGZHOU BAOLI ADHESIVE
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