CN111154430A - Ultraviolet curing OCA pressure-sensitive adhesive film and preparation method thereof - Google Patents
Ultraviolet curing OCA pressure-sensitive adhesive film and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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Abstract
The invention discloses an ultraviolet curing OCA pressure-sensitive adhesive film, which comprises a film layer and an OCA pressure-sensitive adhesive layer arranged on the film layer, wherein the OCA pressure-sensitive adhesive layer comprises the following raw materials in percentage by mass: 7-11% of tackifying resin; 3-7% of a photoinitiator; 3-4.5% of a first reactive diluent; 3-4.5% of a second reactive diluent; the balance being urethane acrylate prepolymer. The invention also discloses a preparation method of the ultraviolet curing OCA pressure-sensitive adhesive film. Through tests, the ultraviolet curing type OCA pressure sensitive adhesive film has the advantages of initial adhesion of No. 9 balls, 180-degree peel strength of 2.1KN/m, constant adhesion of 23h, light transmittance of 99.1%, good constant adhesion performance and high light transmittance. The highest thermal decomposition temperature of the ultraviolet curing type OCA pressure-sensitive adhesive film can reach 255 ℃, no bubbles are generated after photo-aging and damp-heat aging, and the ultraviolet curing type OCA pressure-sensitive adhesive film has the characteristic of excellent aging resistance.
Description
Technical Field
The invention belongs to the technical field of pressure-sensitive adhesive films, and particularly relates to an ultraviolet curing OCA pressure-sensitive adhesive film and a preparation method thereof.
Background
The OCA pressure-sensitive adhesive film, i.e., the optically clear adhesive film, is a pressure-sensitive adhesive having excellent optical properties and adhesive properties, and is mainly used for bonding optical parts, and therefore, it is required to have not only excellent optical properties but also pressure-sensitive properties, adhesive properties and excellent aging resistance possessed by the pressure-sensitive adhesive.
The light transmittance of the UV-cured optical transparent pressure-sensitive adhesive film in the prior art is generally lower than 97%, the defects of low permanent adhesion, low light transmittance and poor aging resistance exist, and the requirements of high-performance electronic products on the adhesive film cannot be met.
Disclosure of Invention
The invention aims to provide an ultraviolet curing OCA pressure-sensitive adhesive film and a preparation method thereof, and aims to solve the technical problem that the OCA pressure-sensitive adhesive film in the prior art is low in permanent adhesion.
In order to achieve the above object, an embodiment of the present invention provides an ultraviolet curing type OCA pressure-sensitive adhesive film, which includes a film layer and an OCA pressure-sensitive adhesive layer disposed on the film layer, where the OCA pressure-sensitive adhesive layer includes the following raw materials by mass:
7-11% of tackifying resin;
3-7% of a photoinitiator;
3-4.5% of a first reactive diluent;
3-4.5% of a second reactive diluent;
the balance being urethane acrylate prepolymer.
Preferably, the OCA pressure sensitive adhesive layer further comprises the following raw materials in percentage by mass: 0.1-0.3% of sensitizer, 0.3-0.6% of stabilizer, 0.2-0.5% of antioxidant, 0.05-0.3% of flatting agent and 0.05-0.2% of anti-aging agent.
Preferably, the polyurethane acrylate prepolymer comprises the following raw materials in percentage by mass:
0.2-0.4% of polymerization inhibitor, 15-25% of third reactive diluent and the balance of monomer, wherein the monomer comprises polypropylene glycol, toluene diisocyanate and hydroxyethyl acrylate, and the mass ratio of the toluene diisocyanate to the polypropylene glycol to the hydroxyethyl acrylate is (2.2-2.3): 1: 2.
preferably, the light transmittance of the polyurethane acrylate prepolymer is 97-99%, the molecular weight is 10000-12000, the molecular weight distribution width index is 2.4-2.6, and the viscosity is 14000-16000 mPa.s.
Preferably, the first reactive diluent is a reactive diluent HDDA, the second reactive diluent is ethoxylated bisphenol A dimethacrylate, and the mass ratio of the two is 1: 1.
preferably, the tackifying resin is a terpene resin; the photoinitiator is a photoinitiator BP.
The embodiment of the invention also provides a preparation method of the ultraviolet curing OCA pressure-sensitive adhesive film, which comprises the following steps:
1) weighing the toluene diisocyanate in proportion, adding the toluene diisocyanate into a reaction kettle, and stirring and mixing uniformly; weighing the polypropylene glycol according to the proportion, and adding the polypropylene glycol into a reaction kettle for more than 3 times within 1 hour; introducing nitrogen, heating to 58-62 ℃, and reacting for 40-80 minutes; heating to 63-67 ℃, continuing to react for 40-80 minutes, and stopping the reaction;
2) weighing the hydroxyethyl acrylate and the polymerization inhibitor according to the proportion, and adding the hydroxyethyl acrylate and the polymerization inhibitor into a reaction kettle; heating to 75-85 ℃, adding the third reactive diluent in a ratio, and continuing to react for 2.5-3.5 hours; until the content of the isocyanic acid radical in the reaction system is detected to be less than 0.3%, after the reaction is finished, cooling to room temperature, and discharging to obtain the polyurethane acrylate prepolymer;
3) weighing pressure-sensitive adhesive raw materials according to a ratio, wherein the pressure-sensitive adhesive raw materials comprise: uniformly mixing the tackifying resin, the photoinitiator, the first reactive diluent, the second reactive diluent and the urethane acrylate prepolymer to prepare the ultraviolet curing OCA pressure sensitive adhesive;
4) and coating the ultraviolet curing type OCA pressure sensitive adhesive on the film layer to form the OCA pressure sensitive adhesive layer with the thickness of 80-120 micrometers, and irradiating the OCA pressure sensitive adhesive layer for 25-35 seconds by using an ultraviolet curing machine to obtain the ultraviolet curing type OCA pressure sensitive adhesive film.
Preferably, the preparation method of the ultraviolet curing type OCA pressure sensitive adhesive film further comprises the following steps:
5) and dehydrating the polypropylene glycol for 2-4 hours at the temperature of 100-120 ℃ and the vacuum degree of more than 0.09 Mpa.
Preferably, the preparation method of the ultraviolet curing type OCA pressure sensitive adhesive film further comprises the following steps:
6) and carrying out vacuum-pumping treatment on the first reactive diluent for 3-5 hours at the temperature of 75-85 ℃.
Preferably, in step 3), the pressure-sensitive adhesive raw material further comprises: sensitizer, stabilizer, antioxidant, leveling agent and anti-aging agent.
The one or more technical schemes in the ultraviolet curing type OCA pressure-sensitive adhesive film and the preparation method thereof provided by the embodiment of the invention have at least one of the following technical effects:
1. through tests, the ultraviolet curing type OCA pressure sensitive adhesive film has the advantages of initial adhesion of No. 9 balls, 180-degree peel strength of 2.1KN/m, constant adhesion of 23h, light transmittance of 99.1%, good constant adhesion performance and high light transmittance;
2. the highest thermal decomposition temperature of the ultraviolet curing type OCA pressure-sensitive adhesive film can reach 255 ℃, no bubbles are generated after photo-aging and damp-heat aging, and the ultraviolet curing type OCA pressure-sensitive adhesive film has the characteristic of excellent aging resistance;
3. the ultraviolet curing OCA pressure sensitive adhesive prepared by the preparation method of the ultraviolet curing OCA pressure sensitive adhesive film has the characteristics of being colorless and transparent and moderate in viscosity.
4. The optimized monomer ratio is as follows: the mass ratio of the toluene diisocyanate to the polypropylene glycol to the hydroxyethyl acrylate is 2.2-2.3: 1: 2, the prepared polyurethane acrylate prepolymer is colorless and transparent, the-NCO content is lower than 0.02 percent, and the storage period is long.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
Fig. 1 is a schematic structural diagram of an ultraviolet-curable OCA pressure-sensitive adhesive film provided in an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary and intended to be illustrative of the embodiments of the present invention, and should not be construed as limiting the invention.
Example 1
The ultraviolet curing type OCA pressure sensitive adhesive film provided by the embodiment comprises a film layer 100 and an OCA pressure sensitive adhesive layer 200 arranged on the film layer 100, wherein the film layer 100 is made of PET. The OCA pressure sensitive adhesive layer 200 comprises the following raw materials in percentage by mass: 7% of tackifying resin, 3% of photoinitiator, 3% of first reactive diluent, 3% of second reactive diluent, 0.3% of sensitizer, 0.6% of stabilizer, 0.5% of antioxidant, 0.3% of leveling agent, 0.2% of anti-aging agent and 82.1% of urethane acrylate prepolymer.
The polyurethane acrylate prepolymer comprises the following raw materials in percentage by mass: 0.2% of polymerization inhibitor, 15% of third reactive diluent and 84.8% of monomer, wherein the monomer comprises polypropylene glycol, toluene diisocyanate and hydroxyethyl acrylate, and the mass ratio of the toluene diisocyanate to the polypropylene glycol to the hydroxyethyl acrylate is 2.2: 1: 2.
the light transmittance of the polyurethane acrylate prepolymer is 97%, the molecular weight is 10000, the molecular weight distribution width index is 2.4, and the viscosity is 14000 mPa.s.
The first reactive diluent is a reactive diluent HDDA, which is produced by Changxing chemical industry Co., Ltd. The second reactive diluent is ethoxylated bisphenol A dimethacrylate. This example used ethoxylated bisphenol A dimethacrylate (EM3260) from Changxing chemical industries, Inc. The mass ratio of the two is 1: 1.
the tackifying resin is a terpene resin, and the terpene resin HP901 produced by marchanchang electronic materials ltd is adopted in this embodiment. The photoinitiator is a photoinitiator BP. This example uses the photoinitiator BP manufactured by Saedoma, USA.
The embodiment also provides a preparation method of the ultraviolet curing type OCA pressure-sensitive adhesive film, which comprises the following steps:
1) the polypropylene glycol was dehydrated for 4 hours at a temperature of 100 ℃ and a vacuum of 0.1 MPa.
2) The first reactive diluent is subjected to a vacuum evacuation treatment at a temperature of 75 ℃ for 5 hours.
3) 358.7692g of toluene diisocyanate is weighed and added into a reaction kettle, and the mixture is stirred and mixed uniformly; 163.0769g of the polypropylene glycol is weighed, and the polypropylene glycol is added into a reaction kettle for 4 times within 1 hour; introducing nitrogen, heating to 58 ℃, and reacting for 80 minutes; heating to 63 ℃, continuing to react for 80 minutes, and stopping the reaction;
4) weighing 326.1538kg of hydroxyethyl acrylate and 2kg of polymerization inhibitor, and adding into a reaction kettle; heating to 75 ℃, adding the 150kg third reactive diluent in a proportion amount, and continuing to react for 3.5 hours; until the content of the isocyanic acid radical in the reaction system is detected to be less than 0.3%, after the reaction is finished, cooling to room temperature, and discharging to obtain the polyurethane acrylate prepolymer;
5) weighing pressure-sensitive adhesive raw materials according to a ratio, wherein the pressure-sensitive adhesive raw materials comprise: uniformly mixing 70kg of tackifying resin, 30kg of photoinitiator, 30kg of first reactive diluent, 30kg of second reactive diluent, 821kg of urethane acrylate prepolymer, 3kg of sensitizer, 6kg of stabilizer, 5kg of antioxidant, 3kg of leveling agent and 2kg of anti-aging agent to prepare the ultraviolet curing OCA pressure sensitive adhesive;
6) and coating the ultraviolet curing type OCA pressure sensitive adhesive on the film layer 100 to form the OCA pressure sensitive adhesive layer 200 with the thickness of 80 microns, and irradiating the OCA pressure sensitive adhesive layer 200 for 25 seconds by using an ultraviolet curing machine to obtain the ultraviolet curing type OCA pressure sensitive adhesive film.
Example 2
The present embodiment is different from embodiment 1 in that: the OCA pressure sensitive adhesive layer 200 comprises the following raw materials in percentage by mass: 10% of tackifying resin, 4% of photoinitiator, 3.5% of first reactive diluent, 3.5% of second reactive diluent, 0.2% of sensitizer, 0.4% of stabilizer, 0.3% of antioxidant, 0.15% of leveling agent, 0.15% of anti-aging agent and 77.8% of polyurethane acrylate prepolymer.
The rest of this embodiment is the same as embodiment 1, and the features not explained in this embodiment are explained by embodiment 1, which is not described again here.
Example 3
The present embodiment is different from embodiment 1 in that: the ultraviolet curing type OCA pressure sensitive adhesive film provided by the embodiment comprises a film layer 100 and an OCA pressure sensitive adhesive layer 200 arranged on the film layer 100, wherein the film layer 100 is made of PET. The OCA pressure sensitive adhesive layer 200 comprises the following raw materials in percentage by mass: 9% of tackifying resin, 5% of photoinitiator, 3.75% of first reactive diluent, 3.75% of second reactive diluent and 78.5% of urethane acrylate prepolymer.
The polyurethane acrylate prepolymer comprises the following raw materials in percentage by mass: 0.3% of polymerization inhibitor, 20% of third reactive diluent and 79.7% of monomer, wherein the monomer comprises polypropylene glycol, toluene diisocyanate and hydroxyethyl acrylate, and the mass ratio of the toluene diisocyanate to the polypropylene glycol to the hydroxyethyl acrylate is 2.25: 1: 2.
the urethane acrylate prepolymer had a light transmittance of 98%, a molecular weight of 11000, a molecular weight distribution breadth index of 2.5, and a viscosity of 15000 mpa.s.
The mass ratio of the first reactive diluent to the second reactive diluent is 1: 1.
the embodiment also provides a preparation method of the ultraviolet curing type OCA pressure-sensitive adhesive film, which comprises the following steps:
1) the polypropylene glycol was dehydrated for 3 hours at a temperature of 110 ℃ and a vacuum of 0.1 MPa.
2) The first reactive diluent is subjected to vacuum treatment under reduced pressure for 4 hours at a temperature of 80 ℃.
3) Weighing 341.5714kg of the toluene diisocyanate, adding the toluene diisocyanate into a reaction kettle, and stirring and mixing uniformly; 151.9085kg of polypropylene glycol is weighed, and the polypropylene glycol is added into a reaction kettle for 5 times within 1 hour; introducing nitrogen, heating to 60 ℃, and reacting for 60 minutes; heating to 65 ℃, continuing to react for 60 minutes, and stopping the reaction;
4) 303.817kg of hydroxyethyl acrylate and 3kg of polymerization inhibitor are weighed and added into a reaction kettle; heating to 80 ℃, adding 200kg of the third reactive diluent, and continuing to react for 3 hours; until the content of the isocyanic acid radical in the reaction system is detected to be less than 0.3%, after the reaction is finished, cooling to room temperature, and discharging to obtain the polyurethane acrylate prepolymer;
5) weighing pressure-sensitive adhesive raw materials according to a ratio, wherein the pressure-sensitive adhesive raw materials comprise: uniformly mixing 90kg of tackifying resin, 50kg of photoinitiator, 37.5kg of first reactive diluent, 37.5kg of second reactive diluent and 785kg of polyurethane acrylate prepolymer to prepare the ultraviolet curing OCA pressure sensitive adhesive;
6) and coating the ultraviolet curing type OCA pressure sensitive adhesive on the film layer 100 to form the OCA pressure sensitive adhesive layer 200 with the thickness of 100 micrometers, and irradiating the OCA pressure sensitive adhesive layer 200 for 30 seconds by using an ultraviolet curing machine to obtain the ultraviolet curing type OCA pressure sensitive adhesive film.
The rest of this embodiment is the same as embodiment 1, and the features not explained in this embodiment are explained by embodiment 1, which is not described again here.
Example 4
The present embodiment is different from embodiment 1 in that: the ultraviolet-curable OCA pressure-sensitive adhesive film provided by the embodiment comprises a film layer 100 and an OCA pressure-sensitive adhesive layer 200 arranged on the film layer 100. Wherein, the material of the film layer 100 is BOPET. The OCA pressure sensitive adhesive layer 200 comprises the following raw materials in percentage by mass: 11% of tackifying resin, 7% of photoinitiator, 4.5% of first reactive diluent, 4.5% of second reactive diluent, 0.1% of sensitizer, 0.3% of stabilizer, 0.2% of antioxidant, 0.05% of leveling agent, 0.05% of anti-aging agent and 72.3% of urethane acrylate prepolymer.
The polyurethane acrylate prepolymer comprises the following raw materials in percentage by mass: 0.4% of polymerization inhibitor, 25% of third reactive diluent and 74.6% of monomer, wherein the monomer comprises polypropylene glycol, toluene diisocyanate and hydroxyethyl acrylate, and the mass ratio of the toluene diisocyanate to the polypropylene glycol to the hydroxyethyl acrylate is 2.3: 1: 2.
the urethane acrylate prepolymer has the light transmittance of 99%, the molecular weight of 12000, the molecular weight distribution breadth index of 2.6 and the viscosity of 16000 mPa.s.
The mass ratio of the first reactive diluent to the second reactive diluent is 1: 1.
the embodiment also provides a preparation method of the ultraviolet curing type OCA pressure-sensitive adhesive film, which comprises the following steps:
1) the polypropylene glycol was dehydrated for 2 hours at a temperature of 120 ℃ and a vacuum of 0.1 MPa.
2) The first reactive diluent was subjected to vacuum evacuation at 85 ℃ for 3 hours.
3) Weighing 323.7358kg of the toluene diisocyanate, adding the toluene diisocyanate into a reaction kettle, and stirring and mixing uniformly; 140.7547kg of polypropylene glycol is weighed, and the polypropylene glycol is added into a reaction kettle for more than 3 times within 1 hour; introducing nitrogen, heating to 62 ℃, and reacting for 40 minutes; heating to 67 ℃, continuing to react for 40 minutes, and stopping the reaction;
4) 281.5094kg of hydroxyethyl acrylate and 4kg of polymerization inhibitor are weighed and added into a reaction kettle; heating to 85 ℃, adding 250kg of the third reactive diluent, and continuing to react for 2.5 hours; until the content of the isocyanic acid radical in the reaction system is detected to be less than 0.3%, after the reaction is finished, cooling to room temperature, and discharging to obtain the polyurethane acrylate prepolymer;
5) weighing pressure-sensitive adhesive raw materials according to a ratio, wherein the pressure-sensitive adhesive raw materials comprise: uniformly mixing 110kg of tackifying resin, 70kg of photoinitiator, 45kg of first reactive diluent, 45kg of second reactive diluent, 723kg of urethane acrylate prepolymer, 1kg of sensitizer, 3kg of stabilizer, 2kg of antioxidant, 0.5kg of leveling agent and 0.5kg of anti-aging agent to prepare the ultraviolet curing type OCA pressure sensitive adhesive;
6) and coating the ultraviolet curing type OCA pressure sensitive adhesive on the film layer 100 to form the OCA pressure sensitive adhesive layer 200 with the thickness of 120 microns, and irradiating the OCA pressure sensitive adhesive layer 200 for 35 seconds by using an ultraviolet curing machine to obtain the ultraviolet curing type OCA pressure sensitive adhesive film.
The rest of this embodiment is the same as embodiment 1, and the features not explained in this embodiment are explained by embodiment 1, which is not described again here.
Example 5
The ultraviolet-curable OCA pressure-sensitive adhesive films prepared in examples 1-4 were tested for initial adhesion, 180-degree peel strength, permanent adhesion, light transmittance and haze, and the test results were as follows:
the initial adhesion is tested according to the regulation of the national standard GB/T4852; the 180-degree peel strength is tested according to the specification of the national standard GB 2792; the permanent adhesion is tested according to the regulation of national standard GB/T4851; the light transmittance and the haze are tested according to the specification of the national standard GB/T2410. According to the test data, the ultraviolet curing OCA pressure sensitive adhesive film has the advantages of good adhesive property and high light transmittance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The utility model provides an ultraviolet curing type OCA pressure sensitive adhesive film, includes the rete and locates OCA pressure sensitive adhesive layer on the rete, its characterized in that, OCA pressure sensitive adhesive layer includes the following raw materials by mass percent:
7-11% of tackifying resin;
3-7% of a photoinitiator;
3-4.5% of a first reactive diluent;
3-4.5% of a second reactive diluent;
the balance being urethane acrylate prepolymer.
2. The ultraviolet-curable OCA pressure-sensitive adhesive film of claim 1, further comprising the following raw materials in percentage by mass: 0.1-0.3% of sensitizer, 0.3-0.6% of stabilizer, 0.2-0.5% of antioxidant, 0.05-0.3% of flatting agent and 0.05-0.2% of anti-aging agent.
3. The ultraviolet-curable OCA pressure-sensitive adhesive film according to claim 2, wherein the polyurethane acrylate prepolymer comprises the following raw materials in percentage by mass: 0.2-0.4% of polymerization inhibitor, 15-25% of third reactive diluent and the balance of monomer, wherein the monomer comprises polypropylene glycol, toluene diisocyanate and hydroxyethyl acrylate, and the mass ratio of the toluene diisocyanate to the polypropylene glycol to the hydroxyethyl acrylate is (2.2-2.3): 1: 2.
4. the ultraviolet-curable OCA pressure-sensitive adhesive film according to claim 3, wherein the urethane acrylate prepolymer has a light transmittance of 97-99%, a molecular weight of 10000-12000, a molecular weight distribution width index of 2.4-2.6, and a viscosity of 14000-16000 mPa.s.
5. The UV-curable OCA pressure-sensitive adhesive film according to claim 3 or 4, wherein the first reactive diluent is HDDA (high Density Diolff), the second reactive diluent is ethoxylated bisphenol A dimethacrylate, and the mass ratio of the two is 1: 1.
6. the ultraviolet-curable OCA pressure-sensitive adhesive film according to claim 3 or 4, wherein the tackifier resin is a terpene resin; the photoinitiator is a photoinitiator BP.
7. The preparation method of the ultraviolet curing type OCA pressure sensitive adhesive film according to any one of claims 3 to 6, which is characterized by comprising the following steps:
1) weighing the toluene diisocyanate in proportion, adding the toluene diisocyanate into a reaction kettle, and stirring and mixing uniformly; weighing the polypropylene glycol according to the proportion, and adding the polypropylene glycol into a reaction kettle for more than 3 times within 1 hour; introducing nitrogen, heating to 58-62 ℃, and reacting for 40-80 minutes; heating to 63-67 ℃, continuing to react for 40-80 minutes, and stopping the reaction;
2) weighing the hydroxyethyl acrylate and the polymerization inhibitor according to the proportion, and adding the hydroxyethyl acrylate and the polymerization inhibitor into a reaction kettle; heating to 75-85 ℃, adding the third reactive diluent in a ratio, and continuing to react for 2.5-3.5 hours; until the content of the isocyanic acid radical in the reaction system is detected to be less than 0.3%, after the reaction is finished, cooling to room temperature, and discharging to obtain the polyurethane acrylate prepolymer;
3) weighing pressure-sensitive adhesive raw materials according to a ratio, wherein the pressure-sensitive adhesive raw materials comprise: uniformly mixing the tackifying resin, the photoinitiator, the first reactive diluent, the second reactive diluent and the urethane acrylate prepolymer to prepare the ultraviolet curing OCA pressure sensitive adhesive;
4) and coating the ultraviolet curing type OCA pressure sensitive adhesive on the film layer to form the OCA pressure sensitive adhesive layer with the thickness of 80-120 micrometers, and irradiating the OCA pressure sensitive adhesive layer for 25-35 seconds by using an ultraviolet curing machine to obtain the ultraviolet curing type OCA pressure sensitive adhesive film.
8. The method for preparing the ultraviolet curing type OCA pressure sensitive adhesive film according to claim 7, further comprising the following steps:
5) and dehydrating the polypropylene glycol for 2-4 hours at the temperature of 100-120 ℃ and the vacuum degree of more than 0.09 Mpa.
9. The method for preparing the ultraviolet curing type OCA pressure-sensitive adhesive film according to claim 7 or 8, characterized by further comprising the steps of:
6) and carrying out vacuum-pumping treatment on the first reactive diluent for 3-5 hours at the temperature of 75-85 ℃.
10. The method for preparing the ultraviolet curing type OCA pressure-sensitive adhesive film according to claim 9, wherein in the step 3), the pressure-sensitive adhesive raw material further comprises: sensitizer, stabilizer, antioxidant, leveling agent and anti-aging agent.
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