CN111171747B - High-temperature-resistant low-residue pu adhesive protective film and preparation method thereof - Google Patents
High-temperature-resistant low-residue pu adhesive protective film and preparation method thereof Download PDFInfo
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention provides a high-temperature-resistant low-residue pu adhesive protective film and a preparation method thereof, wherein the protective film comprises a fingerprint-resistant layer 1, a toughened glass layer 2, a hardened layer 3, a PET substrate layer 4, a glue layer 5 and a peelable liner 6; the glue layer is in a shape of a Chinese character 'hui' when viewed in a direction perpendicular to the glue layer, wherein the glue layer comprises a first area positioned at the periphery and a second area positioned at the center, the first area is coated with first glue, and the second area is coated with second glue on the glue layer 5; the preparation method comprises the steps of firstly preparing a composite film with a fingerprint-resistant layer 1, a toughened glass layer 2, a hardening layer 3 and a PET substrate layer 4, then coating first glue and second glue on the composite film to form a glue layer 5, and then covering a peelable liner 6 on the surface of the glue layer 5 to obtain the protective film; the protective film has good mechanical flexibility, can bear high temperature change and mechanical bending, and has excellent performances of environmental protection, long service life, wear resistance and the like.
Description
Technical Field
The invention relates to a high-temperature-resistant low-residue pu adhesive protective film and a preparation method thereof.
Background
With the popularization of digital products such as mobile phones and the like in the world, screens are used more and more, and screen protection is an inevitable requirement. The surface protection film is widely applied to the fields of mobile phones, tablet computers, liquid crystal televisions and the like, and the basic function of the surface protection film is to prevent a screen from being worn and crushed. Because the protective film is provided with the toughened glass layer, the protective film has poor bending resistance and temperature resistance service life, and pu glue has more residues, and the following method is provided for solving the problems.
Disclosure of Invention
The invention provides a high-temperature-resistant low-residue pu adhesive protective film and a preparation method thereof, wherein the protective film comprises a fingerprint-resistant layer 1, a toughened glass layer 2, a hardened layer 3, a PET substrate layer 4, a glue layer 5 and a peelable liner 6; the glue layer is in a shape of a Chinese character 'hui' when viewed in a direction perpendicular to the glue layer, wherein the glue layer comprises a first area positioned at the periphery and a second area positioned at the center, the first area is coated with first glue, and the second area is coated with second glue on the glue layer 5; the preparation method comprises the steps of firstly preparing a composite film with a fingerprint-resistant layer 1, a toughened glass layer 2, a hardening layer 3 and a PET substrate layer 4, then coating first glue and second glue on the composite film to form a glue layer 5, and then covering a peelable liner 6 on the surface of the glue layer 5 to obtain the protective film; the protective film has good mechanical flexibility, can bear high temperature change and mechanical bending, has low pu glue residue, and has excellent performances of environmental protection, long service life, wear resistance and the like.
The specific scheme is as follows:
a preparation method of a high-temperature-resistant low-residue pu adhesive protective film comprises a fingerprint-resistant layer 1, a toughened glass layer 2, a hardened layer 3, a PET substrate layer 4, an adhesive layer 5 and a peelable liner 6; wherein the glue layer appears in a "wrap" shape when viewed in a direction perpendicular to the layers, comprising a first region at the periphery and a second region at the center, the method comprising:
1) preparing a coating of a hardening layer;
2) uniformly coating a coating of a hardening coating on one surface of the PET substrate layer;
3) pasting a toughened glass layer, baking at 60 ℃ for 30-60 minutes, and curing the coating by using ultraviolet light to obtain a hardened layer clamped by the PET substrate layer and the toughened glass layer;
4) preparing a coating of the fingerprint-resistant layer;
5) coating the coating of the fingerprint-resistant layer on the surface of the toughened glass layer, and curing the coating by using ultraviolet light to form the fingerprint-resistant layer;
6) placing the laminated film obtained in the step 5 into an oven, baking at 70-80 ℃, naturally cooling to room temperature for 30-60 minutes, and taking out;
7) coating first glue on a first area of the PET base material layer side of the laminated film, coating second glue on a second area, and covering a peelable liner to obtain the protective film; wherein the first glue comprises the following components: 40-50 parts of polyurethane acrylate, 15-20 parts of epoxy resin and 8-10 parts of rosin resin; 5-8 parts of glycerol, 3-5 parts of sodium silicate, 0.2-0.4 part of polyacrylamide, 3-5 parts of silane coupling agent, 0.2-0.8 part of photoinitiator and 80-100 parts of organic solvent; the second glue comprises the following components: 20-30 parts of urethane acrylate, 25-30 parts of epoxy resin, 4-8 parts of rosin resin, 5-8 parts of glycerol, 3-5 parts of sodium silicate, 1-2 parts of polyacrylamide, 3-5 parts of silane coupling agent, 0.2-0.8 part of photoinitiator and 80-100 parts of organic solvent.
Further, wherein the coating of the hardened layer is composed of the following components; 10-30 parts of polyurethane acrylate, 2-5 parts of propyl trimethoxy silane, 15-20 parts of nano zirconia particles, 10-15 parts of hydroxyl-containing acrylate, 1-3 parts of silane coupling agent, 0.2-0.8 part of photoinitiator, 0.5-2 parts of leveling agent, 478-10 parts of blue light absorber Oldham and 80-120 parts of organic solvent.
Further, the coating of the fingerprint-resistant layer comprises the following components: 15-30 parts of urethane acrylate, 6-8 parts of polytrimethylene terephthalate, 5-8 parts of ethyl orthosilicate, 15-20 parts of epoxy resin, 8-10 parts of methyl methacrylate, 0.1-2 parts of isocyanate, 5-8 parts of lithium trifluoromethanesulfonate, 6-8 parts of nano titanium dioxide, 5-10 parts of nano silicon dioxide, 0.5-4 parts of silane coupling agent, 0.5-3 parts of photoinitiator, 0.5-2 parts of flatting agent and 80-120 parts of organic solvent.
Further, wherein the ultraviolet light illuminance is 600-2。
Further, the high-temperature-resistant low-residue pu adhesive protective film is characterized by being prepared by the preparation method.
The invention has the following beneficial effects:
1) the toughened glass layer and the substrate layer are connected through the hardening layer, so that the mechanical strength of the composite layer and the interlayer bonding force are enhanced;
2) the hardened layer is used as the middle layer of the toughened glass layer and the base material layer, so that the stress difference caused by uneven stress on the upper surface and the lower surface of the toughened glass layer can be relieved when the protective film is bent, reverse transverse stress in opposite directions can be formed on the two surfaces, in contact with the toughened glass layer, of the hardened layer when the toughened glass is bent, the stress difference of the toughened glass can be neutralized, and the bending resistance of the protective film is improved;
3) and the blue light absorbent is added into the hardening layer, so that the performance of filtering blue light can be improved.
4) The coating of the fingerprint resistant layer comprises: 15-30 parts of urethane acrylate, 6-8 parts of polytrimethylene terephthalate, 5-8 parts of ethyl orthosilicate, 15-20 parts of epoxy resin, 8-10 parts of methyl methacrylate, 0.1-2 parts of isocyanate, 5-8 parts of lithium trifluoromethanesulfonate, 6-8 parts of nano titanium dioxide, 5-10 parts of nano silicon dioxide and 0.5-4 parts of silane coupling agent, so that the mechanical strength of the fingerprint-resistant layer is improved, and the fingerprint-resistant layer is positioned on the surface of the toughened glass layer, wherein two surfaces, contacting the fingerprint-resistant layer and the toughened glass layer, can form reverse transverse stress in opposite directions, can neutralize the stress difference of the toughened glass, and improve the bending resistance of the protective film;
5) the glue layer of two kinds of differences, inlayer glue has higher mechanical strength after the sclerosis, and outer glue can keep higher viscosity and toughness, prevents that the edge from upwarping to the inlayer glue reduces PU's use amount through adding epoxy, has improved the high temperature resistance performance of protection film, and reduces PU's residual.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
In the examples, the fingerprint resistant layer is 80 microns, the toughened glass layer is 100 microns, the cured layer is 80 microns, the PET substrate layer is 50 microns, and the glue layer is 40 microns.
Example 1
1) Dispersing 10 parts by weight of polyurethane acrylate, 2 parts by weight of propyl trimethoxy silane, 15 parts by weight of nano zirconium oxide particles, 10 parts by weight of acrylate containing hydroxyl, 1 part by weight of silane coupling agent, 0.2 part by weight of photoinitiator, 0.5 part by weight of flatting agent and 478 parts by weight of Eupatorium TM of blue light absorber in 80 parts by weight of acetone, and uniformly stirring;
2) uniformly coating a coating of a hardening coating on one surface of the PET substrate layer;
3) attaching a toughened glass layer, baking at 60 ℃ for 30 minutes, and curing the coating by using ultraviolet light of 600mJ/cm2 to obtain a hardened layer clamped by the PET substrate layer and the toughened glass layer;
4) dispersing 15 parts by weight of polyurethane acrylate, 6 parts by weight of polytrimethylene terephthalate, 5 parts by weight of ethyl orthosilicate, 15 parts by weight of epoxy resin, 8 parts by weight of methyl methacrylate, 0.1 part by weight of isocyanate, 5 parts by weight of lithium trifluoromethanesulfonate, 6 parts by weight of nano titanium dioxide, 5 parts by weight of nano silicon dioxide, 0.5 part by weight of a silane coupling agent, 0.5 part by weight of a photoinitiator and 0.5 part by weight of a leveling agent in 80 parts by weight of acetone, and uniformly stirring;
5) coating the paint of the fingerprint-resistant layer on the surface of the toughened glass layer, and curing the coating by using ultraviolet light of 600mJ/cm2 to form the fingerprint-resistant layer;
6) placing the laminated film obtained in the step 5 into an oven, baking at 70 ℃, naturally cooling to room temperature for 30 minutes, and taking out;
7) coating first glue on a first area of the PET base material layer side of the laminated film, coating second glue on a second area, and covering a peelable liner to obtain the protective film; wherein the first glue comprises the following components: 40 parts of urethane acrylate, 15 parts of epoxy resin and 8 parts of rosin resin; 5 parts by weight of glycerol, 3 parts by weight of sodium silicate, 0.2 part by weight of polyacrylamide, 3 parts by weight of a silane coupling agent, 0.2 part by weight of a photoinitiator, and 80 parts by weight of acetone; the second glue comprises the following components: 20 parts of urethane acrylate, 25-parts of epoxy resin, 4 parts of rosin resin, 5 parts of glycerol, 3 parts of sodium silicate, 1 part of polyacrylamide, 3 parts of silane coupling agent, 0.2 part of photoinitiator and 80 parts of acetone.
Example 2
1) Dispersing 30 parts by weight of polyurethane acrylate, 5 parts by weight of methyltrimethoxysilane, 20 parts by weight of nano zirconia particles, 15 parts by weight of acrylate containing hydroxyl, 3 parts by weight of silane coupling agent, 0.8 part by weight of photoinitiator, 2 parts by weight of flatting agent and 4710 parts by weight of blue light absorber Oldham (TM) in 120 parts by weight of acetone, and uniformly stirring;
2) uniformly coating a coating of a hardening coating on one surface of the PET substrate layer;
3) pasting a toughened glass layer, baking at 60 ℃ for 60 minutes, and curing the coating by using ultraviolet light of 800mJ/cm2 to obtain a hardened layer clamped by the PET substrate layer and the toughened glass layer;
4) dispersing 30 parts by weight of polyurethane acrylate, 8 parts by weight of polytrimethylene terephthalate, 8 parts by weight of ethyl orthosilicate, 20 parts by weight of epoxy resin, 10 parts by weight of methyl methacrylate, 2 parts by weight of isocyanate, 8 parts by weight of lithium trifluoromethanesulfonate, 8 parts by weight of nano titanium dioxide, 10 parts by weight of nano silicon dioxide, 4 parts by weight of a silane coupling agent, 3 parts by weight of a photoinitiator and 2 parts by weight of a leveling agent in 120 parts by weight of acetone, and uniformly stirring;
5) coating the paint of the fingerprint-resistant layer on the surface of the toughened glass layer, and curing the coating by using ultraviolet light of 800mJ/cm2 to form the fingerprint-resistant layer;
6) placing the laminated film obtained in the step 5 into an oven, baking at 80 ℃, naturally cooling to room temperature for 30 minutes, and taking out;
7) coating first glue on a first area of the PET base material layer side of the laminated film, coating second glue on a second area, and covering a peelable liner to obtain the protective film; wherein the first glue comprises the following components: 50 parts of urethane acrylate, 20 parts of epoxy resin and 10 parts of rosin resin; 8 parts by weight of glycerol, 5 parts by weight of sodium silicate, 0.4 part by weight of polyacrylamide, 5 parts by weight of a silane coupling agent, 0.8 part by weight of a photoinitiator, and 100 parts by weight of acetone; the second glue comprises the following components: 30 parts of urethane acrylate, 30 parts of epoxy resin, 8 parts of rosin resin, 8 parts of glycerol, 5 parts of sodium silicate, 2 parts of polyacrylamide, 5 parts of silane coupling agent, 0.8 part of photoinitiator and 100 parts of acetone.
Example 3
1) Dispersing 20 parts by weight of urethane acrylate, 3 parts by weight of methyltrimethoxysilane, 16 parts by weight of nano zirconia particles, 12 parts by weight of acrylate containing hydroxyl, 2 parts by weight of silane coupling agent, 0.4 part by weight of photoinitiator, 1 part by weight of flatting agent and 479 parts by weight of blue light absorber Oldham (TM) in 100 parts by weight of acetone, and uniformly stirring;
2) uniformly coating a coating of a hardening coating on one surface of the PET substrate layer;
3) pasting a toughened glass layer, baking for 40 minutes at 60 ℃, and curing the coating by using ultraviolet light of 700mJ/cm2 to obtain a hardened layer clamped by the PET substrate layer and the toughened glass layer;
4) dispersing 20 parts by weight of urethane acrylate, 7 parts by weight of polytrimethylene terephthalate, 6 parts by weight of ethyl orthosilicate, 17 parts by weight of epoxy resin, 9 parts by weight of methyl methacrylate, 1 part by weight of isocyanate, 6 parts by weight of lithium trifluoromethanesulfonate, 7 parts by weight of nano titanium dioxide, 6 parts by weight of nano silicon dioxide, 2 parts by weight of a silane coupling agent, 2 parts by weight of a photoinitiator and 1 part by weight of a leveling agent in 100 parts by weight of acetone, and uniformly stirring;
5) coating the paint of the fingerprint-resistant layer on the surface of the toughened glass layer, and curing the coating by using ultraviolet light of 700mJ/cm2 to form the fingerprint-resistant layer;
6) placing the laminated film obtained in the step 5 into an oven, baking at 75 ℃, naturally cooling to room temperature for 40 minutes, and taking out;
7) coating first glue on a first area of the PET base material layer side of the laminated film, coating second glue on a second area, and covering a peelable liner to obtain the protective film; wherein the first glue comprises the following components: 45 parts of polyurethane acrylate, 18 parts of epoxy resin and 9 parts of rosin resin; 7 parts by weight of glycerol, 4 parts by weight of sodium silicate, 0.3 part by weight of polyacrylamide, 4 parts by weight of a silane coupling agent, 0.6 part by weight of a photoinitiator, and 90 parts by weight of acetone; the second glue comprises the following components: 25 parts of urethane acrylate, 28 parts of epoxy resin, 6 parts of rosin resin, 6 parts of glycerol, 4 parts of sodium silicate, 2 parts of polyacrylamide, 4 parts of silane coupling agent, 0.6 part of photoinitiator and 90 parts of acetone.
Example 4
1) Dispersing 25 parts by weight of urethane acrylate, 4 parts by weight of methyltrimethoxysilane, 20 parts by weight of nano zirconium oxide particles, 15 parts by weight of acrylate containing hydroxyl, 2 parts by weight of silane coupling agent, 0.6 part by weight of photoinitiator, 1 part by weight of flatting agent and 4710 parts by weight of blue light absorber Oldham (TM) in 110 parts by weight of acetone, and uniformly stirring;
2) uniformly coating a coating of a hardening coating on one surface of the PET substrate layer;
3) pasting a toughened glass layer, baking for 50 minutes at 60 ℃, and curing the coating by using ultraviolet light of 700mJ/cm2 to obtain a hardened layer clamped by the PET substrate layer and the toughened glass layer;
4) dispersing 20 parts by weight of polyurethane acrylate, 7 parts by weight of polytrimethylene terephthalate, 7 parts by weight of ethyl orthosilicate, 18 parts by weight of epoxy resin, 9 parts by weight of methyl methacrylate, 1 part by weight of isocyanate, 7 parts by weight of lithium trifluoromethanesulfonate, 7 parts by weight of nano titanium dioxide, 8 parts by weight of nano silicon dioxide, 3 parts by weight of a silane coupling agent, 3 parts by weight of a photoinitiator and 2 parts by weight of a leveling agent in 110 parts by weight of acetone, and uniformly stirring;
5) coating the paint of the fingerprint-resistant layer on the surface of the toughened glass layer, and curing the coating by using ultraviolet light of 700mJ/cm2 to form the fingerprint-resistant layer;
6) placing the laminated film obtained in the step 5 into an oven, baking at 75 ℃, naturally cooling to room temperature for 50 minutes, and taking out;
7) coating first glue on a first area of the PET base material layer side of the laminated film, coating second glue on a second area, and covering a peelable liner to obtain the protective film; wherein the first glue comprises the following components: 50 parts of urethane acrylate, 20 parts of epoxy resin and 9 parts of rosin resin; 7 parts by weight of glycerol, 4 parts by weight of sodium silicate, 0.4 part by weight of polyacrylamide, 4 parts by weight of a silane coupling agent, 0.6 part by weight of a photoinitiator, and 100 parts by weight of acetone; the second glue comprises the following components: 25 parts of urethane acrylate, 30 parts of epoxy resin, 7 parts of rosin resin, 7 parts of glycerol, 5 parts of sodium silicate, 2 parts of polyacrylamide, 4 parts of silane coupling agent, 0.6 part of photoinitiator and 100 parts of acetone.
Experiment and data
Abrasion resistance test the protective films of the examples were tested under a load of 1.5kg using an abrasion resistance tester, and the number of repeated rubbing cycles when significant breakage occurred was recorded.
The protective film of the example was attached to a 5-inch glass screen, and a free fall was performed with 150g to the center of the glass screen to which the surface protective film was attached, and the height (cm) at which glass breakage occurred was recorded.
Residual stain test the protective film of the example was adhered to a glass plate, left at 160 ℃ for 1 hour, then left at 23 ℃ for 30 minutes and returned to room temperature, and then the surface protective sheet was peeled off at 23 ℃ to visually confirm the presence or absence of staining due to the residue of the adhesive on the glass.
A: no contamination due to adhesive residue on the glass was observed after the surface protective sheet was peeled off.
B: a small amount of contamination due to a small amount of adhesive remaining on the glass was confirmed in the partial area after the surface protective sheet was peeled off.
C: contamination by adhesive residue on the glass was confirmed in most of the area after peeling of the surface protective sheet.
D: it was confirmed that the adhesive on the glass was seriously remained after the surface protective sheet was peeled off to cause serious contamination.
TABLE 1
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.
Claims (1)
1. A preparation method of a high-temperature-resistant low-residue polyurethane resin protective film comprises a fingerprint-resistant layer 1, a toughened glass layer 2, a hardened layer 3, a PET (polyethylene terephthalate) substrate layer 4, a glue layer 5 and a peelable liner 6; wherein the glue layer appears in a "wrap" shape when viewed in a direction perpendicular to the layers, comprising a first region at the periphery and a second region at the center, the method comprising:
1) dispersing 20 parts by weight of urethane acrylate, 3 parts by weight of methyltrimethoxysilane, 16 parts by weight of nano zirconia particles, 12 parts by weight of acrylate containing hydroxyl, 2 parts by weight of silane coupling agent, 0.4 part by weight of photoinitiator, 1 part by weight of flatting agent and 479 parts by weight of blue light absorber Oldham (TM) in 100 parts by weight of acetone, and uniformly stirring;
2) uniformly coating a coating of a hardening coating on one surface of the PET substrate layer;
3) coating a toughened glass layer, baking at 60 deg.C for 40 min, and baking at 700mJ/cm2Curing the coating by using the ultraviolet light to obtain a hardened layer clamped by the PET substrate layer and the toughened glass layer;
4) dispersing 20 parts by weight of urethane acrylate, 7 parts by weight of polytrimethylene terephthalate, 6 parts by weight of ethyl orthosilicate, 17 parts by weight of epoxy resin, 9 parts by weight of methyl methacrylate, 1 part by weight of isocyanate, 6 parts by weight of lithium trifluoromethanesulfonate, 7 parts by weight of nano titanium dioxide, 6 parts by weight of nano silicon dioxide, 2 parts by weight of a silane coupling agent, 2 parts by weight of a photoinitiator and 1 part by weight of a leveling agent in 100 parts by weight of acetone, and uniformly stirring;
5) coating the paint of the fingerprint-resistant layer on the surface of the toughened glass layer at 700mJ/cm2The ultraviolet light cures the coating to form a fingerprint resistant layer;
6) placing the laminated film obtained in the step 5 into an oven, baking at 75 ℃, naturally cooling to room temperature for 40 minutes, and taking out;
7) coating first glue on a first area of the PET base material layer side of the laminated film, coating second glue on a second area, and covering a peelable liner to obtain the protective film; wherein the first glue comprises the following components: 45 parts of polyurethane acrylate, 18 parts of epoxy resin and 9 parts of rosin resin; 7 parts by weight of glycerol, 4 parts by weight of sodium silicate, 0.3 part by weight of polyacrylamide, 4 parts by weight of a silane coupling agent, 0.6 part by weight of a photoinitiator, and 90 parts by weight of acetone; the second glue comprises the following components: 25 parts of urethane acrylate, 28 parts of epoxy resin, 6 parts of rosin resin, 6 parts of glycerol, 4 parts of sodium silicate, 2 parts of polyacrylamide, 4 parts of silane coupling agent, 0.6 part of photoinitiator and 90 parts of acetone.
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