CN108276924A - A kind of high xanthochromia of resistance to UV cured film and preparation method thereof - Google Patents
A kind of high xanthochromia of resistance to UV cured film and preparation method thereof Download PDFInfo
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- CN108276924A CN108276924A CN201810037105.2A CN201810037105A CN108276924A CN 108276924 A CN108276924 A CN 108276924A CN 201810037105 A CN201810037105 A CN 201810037105A CN 108276924 A CN108276924 A CN 108276924A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/07—Aldehydes; Ketones
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
- C09J2301/162—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer the carrier being a laminate constituted by plastic layers only
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
- C09J2301/208—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being constituted by at least two or more adjacent or superposed adhesive layers, e.g. multilayer adhesive
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Laminated Bodies (AREA)
Abstract
The present invention relates to protection technical field of membrane; more particularly to a kind of high xanthochromia of resistance to UV cured film and preparation method thereof; the height thoroughly the xanthochromia of resistance to UV cured film include from top to bottom sequentially connected cuticular layer, use layer and peeling layer; the cuticular layer includes sequentially connected cuticula substrate layer and cuticula glue-line from top to bottom; it is described to include sequentially connected UV hardened layers, main substrate layer and PU glue-lines from top to bottom using layer; the lower surface of the cuticula glue-line is connect with the upper surface of the UV hardened layers, and the lower surface of the PU glue-lines is connect with the upper surface of the peeling layer.The xanthochromia of resistance to UV cured film can effectively absorb ultraviolet light, have preferable resistance to UV, color inhibition effect, in outdoor use for a long time without by influence of ultraviolet light, excellent transparency, excellent combination property the height of the present invention by the way that UV hardened layers and PU glue-lines is arranged thoroughly.
Description
Technical field
The present invention relates to protection technical field of membrane, and in particular to a kind of high xanthochromia of resistance to UV cured film and preparation method thereof.
Background technology
Domestic market has various cured films, the impact of performance having nothing in common with each other, and such as anti-blue light, hardness are high, saturating
Lightness height etc., but current cured film resistance to ultraviolet irradiation, color inhibition performance on it is still bad, as people are to electronic equipment
Frequency of use increase, in outdoor application, the UVResistant effect of protective film is undesirable, influences people's normal use protective film, and
The protective film of electronic equipment is susceptible to Yellowing afterwards by long-term use, influences the normal use of protective film, is easy to influence people
Eyesight.
Invention content
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of high resistance to UV is yellow
Become cured film, the xanthochromia of resistance to UV cured film can effectively absorb ultraviolet light to the height thoroughly, have preferable resistance to UV, color inhibition effect, in room
Outer long-time use is without by influence of ultraviolet light, haveing excellent performance.
The purpose of the present invention is to provide a kind of preparation method of the high xanthochromia of resistance to UV cured film, the preparation method, operations
Easy to control, stable quality, production efficiency is high, and production cost is low, is suitble to large-scale industrial production.
The purpose of the invention is achieved by the following technical solution：A kind of high xanthochromia of resistance to UV cured film, including from top to bottom
Sequentially connected cuticular layer, using layer and peeling layer, the cuticular layer include from top to bottom sequentially connected cuticula substrate layer and
Cuticula glue-line, it is described to include sequentially connected UV hardened layers, main substrate layer and PU glue-lines from top to bottom, the cuticula glue using layer
The lower surface of layer is connect with the upper surface of the UV hardened layers, and the lower surface of the PU glue-lines connects with the upper surface of the peeling layer
It connects.
The xanthochromia of resistance to UV cured film can effectively absorb ultraviolet light to the height of the present invention by using UV hardened layers and PU glue-lines thoroughly,
With preferable resistance to UV, color inhibition effect, in outdoor use for a long time without by influence of ultraviolet light, haveing excellent performance.
Preferably, the cuticula substrate layer is thickness in 50-100 μm of PET film, PE films, OPP films, BOPET films, BOPP
Any one in film；The cuticula glue-line be thickness 5-20 μm, peeling force 1-10gf/25mm organosilicon glue-line；Institute
State peeling layer be thickness 30-100 μm, off-type force 4-10gf/25mm silicone oil release film.
The present invention by using the base material film of mentioned kind as cuticula substrate layer, and strictly control cuticula substrate layer thickness
Degree has preferable dimensional stability and toughness, and light transmittance is high, can stablize with cuticula adhesive-layer and bond, be not easy delamination.By adopting
It uses organosilicon glue-line as cuticula glue-line, and strictly controls the thickness and peeling force of organosilicon glue-line, have and preferably bond surely
It is qualitative, can be with cuticula substrate layer and using the bonding stabilization of layer, interlayer is not easily disconnected from.By using silicone oil release film as stripping
Layer, and the thickness and off-type force of peeling layer are strictly controlled, there are preferable glass effects, the high xanthochromia of resistance to UV thoroughly obtained can be made hard
Changing film has preferable adsorption capacity, can be bonded with electronic product screen completely, appearance is good.
Preferably, the thickness of the UV hardened layers is 3-5 μm；The main substrate layer is thickness in 50-250 μm, light transmittance
In any one of 92%-98%, mist degree in the PET film of 0.02%-1%, PE films, OPP films, BOPET films, BOPP film；Institute
The thickness for stating PU glue-lines is 20-50 μm, peeling force 120-180gf.
The present invention has preferably resistance to ultraviolet and color inhibition effect, in outdoor by strictly controlling the thickness of UV cured films
It is used for a long time without by influence of ultraviolet light；By using the base material film of mentioned kind as main substrate layer, and strictly control main base
Thickness, light transmittance, the mist degree of material layer have preferable dimensional stability and toughness, and light transmittance is high, can be with UV hardened layers, PU glue
Layer, which is stablized, to be bonded, and delamination is not easy；By strictly controlling the thickness and peeling force of PU glue-lines, has and preferably bond stability, energy
With main substrate layer and the bonding stabilization of peeling layer, interlayer is made to be not easily disconnected from.
Preferably, the UV hardened layers are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
40-70 parts of acrylic resin
30-40 parts of photoinitiator
1-5 parts of UV absorbents.
The present invention as preparing the UV glue of UV hardened layers, and strictly controls each raw material by using the raw material of mentioned kind
Dosage, can make UV hardened layers obtained that there is preferable resistance to UV, color inhibition effect, effectively absorb ultraviolet light, when outdoor long
Between use without by influence of ultraviolet light.
Preferably, the photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxy cyclohexylphenyls
At least one of base phenyl ketone, 2- hydroxy-2-methyl -1- phenyl -1- acetone and 2- isopropyl thioxanthones；The UV inhales
Receipts agent is ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone, 2- (2 '-hydroxyls -5 '-methylbenzene
Base) benzotriazole, 2- (bis- tertiary amyl phenyl of 2- hydroxyls -3,5-) benzene a pair of horses going side by side triazole, septichen phenyl ester and 2,4- dihydroxies
At least one of base benzophenone.
The present invention is easy, efficiency of initiation height miscible with acrylic resin by using the photoinitiator of mentioned kind, and heat is steady
Qualitative good, no Yellowing, stable storing can enable the high xanthochromia of resistance to UV cured film thoroughly obtained effectively absorb ultraviolet radiant energy
And free radical or cation are formed, there is preferable space charge force and uv absorption capacity；More preferably, the light draws
Hair agent is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexyl phenyl ketones and 2- hydroxyl -2- first
Base -1- phenyl -1- acetone is 2.5-3.5 with weight ratio:1.4-2.2:The mixture of 1 composition.
And by using the UV absorbents of mentioned kind, good with the compatibility of acrylic resin, volatility is low, has preferable
Thermal stability, the xanthochromia of resistance to UV cured film thoroughly obtained high can be enable effectively to absorb ultraviolet light, and be not likely to produce Yellowing；More
To be preferred, the UV absorbents are ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone and 2-
(2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole is 2.4-3.2 with weight ratio:1.5-2.5:The mixture of 1 composition.
Preferably, the PU glue-lines have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The present invention as preparing the PU glue of PU glue-lines, and strictly controls each raw material by using the raw material of mentioned kind
Dosage, wherein benzophenone compound and isocyanates ultra-violet resistance are good, yellowing resistance is good, and PU glue-lines obtained can be made to have
Preferable resistance to UV, color inhibition effect, effectively absorb ultraviolet light, in outdoor use for a long time without by influence of ultraviolet light.
Preferably, the benzophenone compound be 4,4'-Dihydroxybenzophenone, 2,4-DihydroxyBenzophenone,
2- hydroxyl -4- dodecyls benzophenone, 4- amino -4 '-chlorobenzophenone, 4- nitros -4 '-chlorobenzophenone, 2- amino -
At least one in the chloro- 2 '-fluorine benzophenone of 5-, 2,3,4- trihydroxybenzophenones and 2-hydroxy-4-n-octoxybenzophenone
Kind；The solvent is at least one of ether, tetrahydrofuran, n-butanol, ethyl alcohol, acetone and cyclohexanone.
The present invention uses the benzophenone compound of mentioned kind, can be mixed instead with polyurethane resin and other raw materials
It answers, absorption UV resistance is strong, and PU glue-lines obtained can be made to have preferable resistance to UV, color inhibition effect, effectively absorb ultraviolet light,
In outdoor use for a long time without by influence of ultraviolet light；More preferably, the benzophenone compound is 4,4 '-dihydroxy
Benzophenone, 2- hydroxyls -4- dodecyls benzophenone and 4- amino -4 '-chlorobenzophenone are 1.6-2.4 with weight ratio:
1.0-1.5:The mixture of 1 composition.
Another object of the present invention is achieved through the following technical solutions：A kind of system of the saturating xanthochromia of the resistance to UV cured film of above-mentioned height
Preparation Method includes the following steps：
(1) cuticular layer is prepared：A cuticula base material is taken, organic silica gel glue is coated on the surface of cuticula base material, after cured
Obtain cuticular layer；
(2) composite layer is prepared：A main base material is taken, in the coated on one side UV glue of main base material, passes through first time thermosetting successively
Change, after first time photocuring, forms UV hardened layers on a surface of main base material, be then covered with step on the surface of UV hardened layers
(1) cuticular layer made from, obtains composite layer；
(3) the high xanthochromia of resistance to UV cured film thoroughly is prepared：The another side of main base material is coated with PU in the composite layer made from step (2)
Glue forms PU glue-lines on another surface of main base material, is then covered on the surface of PU glue-lines release after second of heat cure
Film obtains the high xanthochromia of resistance to UV cured film thoroughly.
The preparation method convenient operation and control of the present invention, stable quality, production efficiency is high, and production cost is low, by using
Above-mentioned steps can enable the high xanthochromia of resistance to UV cured film thoroughly obtained effectively absorb ultraviolet light, have preferable resistance to UV, color inhibition effect
Fruit, in outdoor use for a long time without by influence of ultraviolet light, excellent combination property is suitble to large-scale industrial production.
Preferably, in the step (2), coating UV glue uses comma scraper coating method, the first time heat cure
Temperature be 60-150 DEG C, time of first time heat cure is 1-3min；The first time photocuring uses UV photocuring modes,
The UV lamp energy of UV photocurings is 460-710mJ/cm2, the time of UV photocurings is 1-5min.
The present invention carries out the coating of UV glue by using comma scraper coating method, and UV glue can be spread evenly across to shield
On film base material, and the temperature and time of first time heat cure, the UV lamp energy of first time photocuring and hardening time are strictly controlled,
UV glue can adequately be cured, and the UV hardened layers of stable state, energy are formed without influence on UV glue raw material and performance
Ultraviolet light is effectively absorbed, has preferable resistance to UV, color inhibition effect, comprehensive performance good.
Preferably, in the step (3), the temperature of second of heat cure is 60-150 DEG C, second of heat cure
Time is 1-3min.The present invention can carry out PU glue sufficient by strictly controlling the temperature and time of second of heat cure
Solidification, and is formed by the PU glue-lines of stable state, can effectively absorb ultraviolet light without influence for PU glue material performance, have preferable
Resistance to UV, color inhibition effect, comprehensive performance is good.
The beneficial effects of the present invention are：The high xanthochromia of resistance to UV cured film thoroughly of the invention is by using UV hardened layers and PU glue
Layer, can effectively absorb ultraviolet light, have preferable resistance to UV, color inhibition effect, in outdoor use for a long time without by ultraviolet shadow
It rings, has excellent performance.
The preparation method of the present invention, convenient operation and control, stable quality, production efficiency is high, and production cost is low, is suitble to big rule
Mould industrialized production.
Description of the drawings
Fig. 1 is the partial sectional view of the present invention.
Reference numeral is：1-cuticular layer, 11-cuticula substrate layers, 12-cuticula glue-lines, 2-use layer 2,21-UV hard
Change layer, 22-main substrate layers, 23-PU glue-lines, 3-peeling layers.
Specific implementation mode
For the ease of the understanding of those skilled in the art, the present invention is made with reference to embodiment and attached drawing 1 further
Illustrate, the content that embodiment refers to not is limitation of the invention.
Embodiment 1
See Fig. 1, a kind of high xanthochromia of resistance to UV cured film, including from top to bottom sequentially connected cuticular layer 1, use 2 and of layer
Peeling layer 3, the cuticular layer 1 includes sequentially connected cuticula substrate layer 11 and cuticula glue-line 12 from top to bottom, described to use layer 2
Including sequentially connected UV hardened layers 21, main substrate layer 22 and PU glue-lines 23 from top to bottom, the lower surface of the cuticula glue-line 12
It is connect with the upper surface of the UV hardened layers 21, the lower surface of the PU glue-lines 23 is connect with the upper surface of the peeling layer 3.
The cuticula substrate layer 11 is BOPP film of the thickness at 50 μm；The cuticula glue-line 12 is thickness in 5 μm, peeling force
In the organosilicon glue-line of 1gf/25mm；The peeling layer 3 be thickness 30 μm, off-type force 4gf/25mm silicone oil release film.
The thickness of the UV hardened layers 21 is 3 μm；The main substrate layer 22 is for thickness in 50 μm, light transmittance in 98%, mist
Any one of degree in 0.02% BOPP film；The thickness of the PU glue-lines 23 is 20 μm, peeling force 180gf.
The UV hardened layers 21 are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
40 parts of acrylic resin
30 parts of photoinitiator
1 part of UV absorbents.
The photoinitiator is 2- hydroxy-2-methyl -1- phenyl -1- acetone；The UV absorbents be 2- (hydroxyl -3 2-,
Bis- tertiary amyl phenyl of 5-) benzene a pair of horses going side by side triazole.
The PU glue-lines 23 have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The benzophenone compound is 2,3,4- trihydroxybenzophenones；The solvent is n-butanol.
A kind of preparation method of the saturating xanthochromia of the resistance to UV cured film of above-mentioned height, includes the following steps：
(1) cuticular layer 1 is prepared：A cuticula base material is taken, organic silica gel glue is coated on the surface of cuticula base material, after cured
Obtain cuticular layer 1；
(2) composite layer is prepared：A main base material is taken, in the coated on one side UV glue of main base material, passes through first time thermosetting successively
Change, after first time photocuring, forms UV hardened layers 21 on a surface of main base material, be then covered with step on the surface of UV hardened layers 21
Suddenly cuticular layer 1 made from (1), obtains composite layer；
(3) the high xanthochromia of resistance to UV cured film thoroughly is prepared：The another side of main base material is coated with PU in the composite layer made from step (2)
Glue forms PU glue-lines 23 on another surface of main base material, is then covered on the surface of PU glue-lines 23 after second of heat cure
Release film obtains the high xanthochromia of resistance to UV cured film thoroughly.
In the step (2), coating UV glue is using comma scraper coating method, the temperature of the first time heat cure
60 DEG C, the time of first time heat cure is 3min；The first time photocuring uses UV photocuring modes, the UV lamp of UV photocurings
Energy is 460mJ/cm2, the time of UV photocurings is 5min.
In the step (3), the temperature of second of heat cure is 60 DEG C, and the time of second of heat cure is 3min.
Embodiment 2
The present embodiment and above-described embodiment 1 difference lies in：
The cuticula substrate layer 11 is BOPET film of the thickness at 60 μm；The cuticula glue-line 12 is thickness in 8 μm, stripping
Organosilicon glue-line of the power in 3gf/25mm；The peeling layer 3 be thickness 48 μm, silicone oil of the off-type force in 6gf/25mm it is release
Film.
The thickness of the UV hardened layers 21 is 3.5 μm；The main substrate layer 22 be thickness 100 μm, light transmittance 96%,
BOPET film of the mist degree 0.04%；The thickness of the PU glue-lines 23 is 28 μm, peeling force 160gf.
The UV hardened layers 21 are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
48 parts of acrylic resin
32 parts of photoinitiator
2 parts of UV absorbents.
The photoinitiator is 1- hydroxycyclohexyl phenyl ketones；The UV absorbents are 2- (2 '-hydroxyls -5 '-methylbenzene
Base) benzotriazole.
The PU glue-lines 23 have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The benzophenone compound is 2- hydroxyls -4- dodecyls benzophenone and/or 4- amino -4 '-chlorine two
Benzophenone；The solvent is acetone.
In the step (2), coating UV glue is using comma scraper coating method, the temperature of the first time heat cure
83 DEG C, the time of first time heat cure is 2.5min；The first time photocuring uses UV photocuring modes, the UV of UV photocurings
Lamp energy is 530mJ/cm2, the time of UV photocurings is 4min.
In the step (3), the temperature of second of heat cure is 83 DEG C, and the time of second of heat cure is
2.5min。
Embodiment 3
The present embodiment and above-described embodiment 1 difference lies in：
The cuticula substrate layer 11 is PET film of the thickness at 75 μm；The cuticula glue-line 12 is thickness in 12 μm, peeling force
In the organosilicon glue-line of 5gf/25mm；The peeling layer 3 be thickness 65 μm, off-type force 7gf/25mm silicone oil release film.
The thickness of the UV hardened layers 21 is 4 μm；The main substrate layer 22 is for thickness in 150 μm, light transmittance in 95%, mist
Spend the PET film 0.06%；The thickness of the PU glue-lines 23 is 35 μm, peeling force 150gf.
The UV hardened layers 21 are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
55 parts of acrylic resin
35 parts of photoinitiator
3 parts of UV absorbents.
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone；The UV absorbents are 2-
Hydroxyl -4- methoxy benzophenones and/or 2-hydroxy-4-n-octoxybenzophenone.
The PU glue-lines 23 have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The benzophenone compound is 4,4'-Dihydroxybenzophenone and/or 2,4-DihydroxyBenzophenone；It is described
Solvent is ether and/or tetrahydrofuran.
In the step (2), coating UV glue is using comma scraper coating method, the temperature of the first time heat cure
100 DEG C, the time of first time heat cure is 2min；The first time photocuring uses UV photocuring modes, the UV of UV photocurings
Lamp energy is 590mJ/cm2, the time of UV photocurings is 3min.
In the step (3), the temperature of second of heat cure is 100 DEG C, and the time of second of heat cure is 2min.
Embodiment 4
The present embodiment and above-described embodiment 1 difference lies in：
The cuticula substrate layer 11 is PE film of the thickness at 90 μm；The cuticula glue-line 12 is thickness in 16 μm, peeling force
In the organosilicon glue-line of 8gf/25mm；The peeling layer 3 be thickness 82 μm, off-type force 8gf/25mm silicone oil release film.
The thickness of the UV hardened layers 21 is 4.5 μm；The main substrate layer 22 be thickness 200 μm, light transmittance 94%,
PE film of the mist degree 0.08%；The thickness of the PU glue-lines 23 is 42 μm, peeling force 130gf.
The UV hardened layers 21 are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
62 parts of acrylic resin
38 parts of photoinitiator
4 parts of UV absorbents.
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone；The UV absorbents are neighbour
Phenyl hydroxybenzoate.
The PU glue-lines 23 have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The benzophenone compound is 4- nitros -4 '-chlorobenzophenone and/or the chloro- 2 '-fluorine hexichol of 2- amino -5-
Ketone；The solvent is cyclohexanone.
In the step (2), coating UV glue is using comma scraper coating method, the temperature of the first time heat cure
120 DEG C, the time of first time heat cure is 1.5min；The first time photocuring uses UV photocuring modes, UV photocurings
UV lamp energy is 650mJ/cm2, the time of UV photocurings is 2min.
In the step (3), the temperature of second of heat cure is 120 DEG C, and the time of second of heat cure is
1.5min。
Embodiment 5
The present embodiment and above-described embodiment 1 difference lies in：
The cuticula substrate layer 11 is OPP film of the thickness at 100 μm；The cuticula glue-line 12 is thickness in 20 μm, stripping
Organosilicon glue-line of the power in 10gf/25mm；The peeling layer 3 be thickness 100 μm, off-type force 10gf/25mm silicone oil from
Type film.
The thickness of the UV hardened layers 21 is 5 μm；The main substrate layer 22 is for thickness in 250 μm, light transmittance in 92%, mist
Spend the OPP films 1%；The thickness of the PU glue-lines 23 is 50 μm, peeling force 120gf.
The UV hardened layers 21 are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
70 parts of acrylic resin
40 parts of photoinitiator
5 parts of UV absorbents.
The photoinitiator is 2- isopropyl thioxanthones；The UV absorbents are 2,4-DihydroxyBenzophenone.
The PU glue-lines 23 have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The benzophenone compound is 2-hydroxy-4-n-octoxybenzophenone；The solvent is ethyl alcohol.
In the step (2), coating UV glue is using comma scraper coating method, the temperature of the first time heat cure
150 DEG C, the time of first time heat cure is 1min；The first time photocuring uses UV photocuring modes, the UV of UV photocurings
Lamp energy is 710mJ/cm2, the time of UV photocurings is 1min.
In the step (3), the temperature of second of heat cure is 150 DEG C, and the time of second of heat cure is 1min.
Embodiment 6
The present embodiment and above-described embodiment 1 difference lies in：
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexylphenyls
Ketone and 2- hydroxy-2-methyl -1- phenyl -1- acetone are with weight ratio for 2.5:2.2:The mixture of 1 composition.
The UV absorbents are ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone and 2-
(2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole is with weight ratio for 2.4:1.5:The mixture of 1 composition.
The benzophenone compound is 4,4 '-dihydroxy benaophenonels, 2- hydroxyl -4- dodecyl benzophenone
With 4- amino -4 '-chlorobenzophenone with weight ratio for 1.6:1.0:The mixture of 1 composition.
Embodiment 7
The present embodiment and above-described embodiment 2 difference lies in：
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexylphenyls
Ketone and 2- hydroxy-2-methyl -1- phenyl -1- acetone are with weight ratio for 2.8:2:The mixture of 1 composition.
The UV absorbents are ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone and 2-
(2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole is with weight ratio for 2.6:1.8:The mixture of 1 composition.
The benzophenone compound is 4,4 '-dihydroxy benaophenonels, 2- hydroxyl -4- dodecyl benzophenone
With 4- amino -4 '-chlorobenzophenone with weight ratio for 1.8:1.1:The mixture of 1 composition.
Embodiment 8
The present embodiment and above-described embodiment 3 difference lies in：
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexylphenyls
Ketone and 2- hydroxy-2-methyl -1- phenyl -1- acetone are with weight ratio for 3:1.8:The mixture of 1 composition.
The UV absorbents are ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone and 2-
(2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole is with weight ratio for 2.8:2:The mixture of 1 composition.
The benzophenone compound is 4,4 '-dihydroxy benaophenonels, 2- hydroxyl -4- dodecyl benzophenone
With 4- amino -4 '-chlorobenzophenone with weight ratio for 2:1.2:The mixture of 1 composition.
Embodiment 9
The present embodiment and above-described embodiment 4 difference lies in：
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexylphenyls
Ketone and 2- hydroxy-2-methyl -1- phenyl -1- acetone are with weight ratio for 3.2:1.6:The mixture of 1 composition.
The UV absorbents are ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone and 2-
(2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole is with weight ratio for 3:2.2:The mixture of 1 composition.
The benzophenone compound is 4,4 '-dihydroxy benaophenonels, 2- hydroxyl -4- dodecyl benzophenone
With 4- amino -4 '-chlorobenzophenone with weight ratio for 2.2:1.3:The mixture of 1 composition.
Embodiment 10
The present embodiment and above-described embodiment 5 difference lies in：
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexylphenyls
Ketone and 2- hydroxy-2-methyl -1- phenyl -1- acetone are with weight ratio for 3.5:1.4:The mixture of 1 composition.
The UV absorbents are ESCALOL 567,2-hydroxy-4-n-octoxybenzophenone and 2-
(2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole is with weight ratio for 3.2:2.5:The mixture of 1 composition.
The benzophenone compound is 4,4 '-dihydroxy benaophenonels, 2- hydroxyl -4- dodecyl benzophenone
With 4- amino -4 '-chlorobenzophenone with weight ratio for 2.4:1.5:The mixture of 1 composition.
Comparative example 1
A kind of high protective film, including from top to bottom sequentially connected cuticular layer 1, use layer 2 and peeling layer 3, the shield
Film layer 1 includes sequentially connected cuticula substrate layer 11 and cuticula glue-line 12 from top to bottom, it is described using layer 2 include from top to bottom according to
The main substrate layer 22 and PU glue-lines 23 of secondary connection, the lower surface of the cuticula glue-line 12 and the upper surface of the main substrate layer 22 connect
It connects, the lower surface of the PU glue-lines 23 is connect with the upper surface of the peeling layer 3.
The cuticula substrate layer 11 is PET film of the thickness at 75 μm；The cuticula glue-line 12 is thickness in 12 μm, peeling force
In the organosilicon glue-line of 5gf/25mm；The peeling layer 3 be thickness 65 μm, off-type force 7gf/25mm silicone oil release film.
The main substrate layer 22 is thickness in 150 μm, PET film of the light transmittance in 95%, mist degree 0.06%；The PU glue
The thickness of layer 23 is 35 μm, peeling force 150gf.
The PU glue-lines 23 have PU glue is cured to be made, and the PU glue includes the raw material of following parts by weight：
The benzophenone compound is 4,4'-Dihydroxybenzophenone and/or 2,4-DihydroxyBenzophenone；It is described
Solvent is ether and/or tetrahydrofuran.
A kind of preparation method of the saturating protective film of above-mentioned height, includes the following steps：
(1) cuticular layer 1 is prepared：A cuticula base material is taken, organic silica gel glue is coated on the surface of cuticula base material, after cured
Obtain cuticular layer 1；
(2) composite layer is prepared：A main base material is taken, in the coated on one side PU glue of main base material, successively after heat cure,
One surface of main base material forms PU glue-lines 23, is then covered with release film on the surface of PU glue-lines 23, is covered in the another side of main base material
Cuticular layer 1 made from upper step (1) obtains high saturating protective film.
In the step (2), the temperature of the heat cure is 100 DEG C, and the time of heat cure is 2min.
Comparative example 2
A kind of high protective film, including from top to bottom sequentially connected cuticular layer 1, use layer 2 and peeling layer 3, the shield
Film layer 1 includes sequentially connected cuticula substrate layer 11 and cuticula glue-line 12 from top to bottom, it is described using layer 2 include from top to bottom according to
The UV hardened layers 21 and main substrate layer 22 of secondary connection, the upper surface of the lower surface of the cuticula glue-line 12 and the UV hardened layers 21
Connection, the lower surface of the main substrate layer 22 is connect with the upper surface of the peeling layer 3.
The cuticula substrate layer 11 is PET film of the thickness at 75 μm；The cuticula glue-line 12 is thickness in 12 μm, peeling force
In the organosilicon glue-line of 5gf/25mm；The peeling layer 3 be thickness 65 μm, off-type force 7gf/25mm silicone oil release film.
The thickness of the UV hardened layers 21 is 4 μm；The main substrate layer 22 is for thickness in 150 μm, light transmittance in 95%, mist
Spend the PET film 0.06%.
The UV hardened layers 21 are made by UV glue is cured, and the UV glue includes the raw material of following parts by weight：
55 parts of acrylic resin
35 parts of photoinitiator
3 parts of UV absorbents.
The photoinitiator is 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone；The UV absorbents are 2-
Hydroxyl -4- methoxy benzophenones and/or 2-hydroxy-4-n-octoxybenzophenone.
A kind of preparation method of the saturating protective film of above-mentioned height, includes the following steps：
(1) cuticular layer 1 is prepared：A cuticula base material is taken, organic silica gel glue is coated on the surface of cuticula base material, after cured
Obtain cuticular layer 1；
(2) composite layer is prepared：A main base material is taken, it is solid by heat cure, light successively in the coated on one side UV glue of main base material
After change, UV hardened layers 21 are formed on a surface of main base material, are then covered with step (1) shield obtained on the surface of UV hardened layers 21
Film layer 1 is covered with release film in the another side of main base material, obtains high saturating protective film.
In the step (2), coating UV glue uses comma scraper coating method, and the temperature of the heat cure is 60 DEG C,
The time of heat cure is 2min；The photocuring uses UV photocuring modes, and the UV lamp energy of UV photocurings is 590mJ/cm2,
The time of UV photocurings is 3min.
Protective film made from embodiment 1-10 and comparative example 1-2 is subjected to the dependence tests such as color inhibition test, test result
As follows：
The color inhibition test is the installation 2-3 branch quartz burners in chamber, and the temperature in chamber is room temperature, purple
The wavelength of light of outside line fluorescent tube is 280-400nm, and test sample is prevented on the pallet of rotation, and the rotary rpm of pallet is constant,
Quartz burner is parallel with test sample surface, at a distance of 230-270mm, irradiates 3-9h, test sample is taken out after the completion of irradiation,
Standard sources obtains the color inhibition grade of test sample to being compared with gray scale under colored lights.
According to above-mentioned experiment and experimental data, the present invention is further limited by the way that UV hardened layers 21 and PU glue-lines 23 is arranged
The raw material of UV hardened layers 21 and its raw material and its type and dosage of type and dosage and PU glue-lines 23 are determined, can make to be made
Height the xanthochromia of resistance to UV cured film has preferable resistance to UV, color inhibition effect, excellent transparency thoroughly, and can effectively absorb ultraviolet light,
Outdoor use for a long time is without by influence of ultraviolet light, excellent combination property.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other manner,
Any obvious replacement is not departed under the premise of present inventive concept within protection scope of the present invention.
Claims (10)
1. a kind of high xanthochromia of resistance to UV cured film, it is characterised in that：Including sequentially connected cuticular layer from top to bottom, using layer and
Peeling layer, the cuticular layer include sequentially connected cuticula substrate layer and cuticula glue-line from top to bottom, it is described using layer include from
Sequentially connected UV hardened layers, main substrate layer and PU glue-lines under, the lower surface of the cuticula glue-line and the UV hardened layers
Upper surface connection, the lower surface of the PU glue-lines is connect with the upper surface of the peeling layer.
2. a kind of high xanthochromia of resistance to UV cured film according to claim 1, it is characterised in that：The cuticula substrate layer is thickness
Any one of degree in 50-100 μm of PET film, PE films, OPP films, BOPET films, BOPP film；The cuticula glue-line is thickness
5-20 μm, peeling force 1-10gf/25mm organosilicon glue-line；The peeling layer is that thickness exists in 30-100 μm, off-type force
The silicone oil release film of 4-10gf/25mm.
3. a kind of high xanthochromia of resistance to UV cured film according to claim 1, it is characterised in that：The thickness of the UV hardened layers
It is 3-5 μm；The main substrate layer be thickness 50-250 μm, light transmittance 92%-98%, mist degree 0.02%-1% PET
Any one in film, PE films, OPP films, BOPET films, BOPP film；The thickness of the PU glue-lines is 20-50 μm, and peeling force is
120-180gf。
4. a kind of high xanthochromia of resistance to UV cured film according to claim 1, it is characterised in that：The UV hardened layers are by UV glue
Water is cured to be made, and the UV glue includes the raw material of following parts by weight：
40-70 parts of acrylic resin
30-40 parts of photoinitiator
1-5 parts of UV absorbents.
5. a kind of high xanthochromia of resistance to UV cured film according to claim 4, it is characterised in that：The photoinitiator is 2- first
Base -1- (4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 1- hydroxycyclohexyl phenyl ketones, 2- hydroxy-2-methyl -1- phenyl -
At least one of 1- acetone and 2- isopropyl thioxanthones；The UV absorbents are ESCALOL 567,2-
(2- hydroxyls -3,5- two is special by hydroxyl -4- oxy-octyl benzophenones, 2- (2 '-hydroxyls -5 '-aminomethyl phenyl) benzotriazole, 2-
At least one of amyl phenyl) benzene a pair of horses going side by side triazole, septichen phenyl ester and 2,4-DihydroxyBenzophenone.
6. a kind of high xanthochromia of resistance to UV cured film according to claim 1, it is characterised in that：The PU glue-lines have PU glue
Cured to be made, the PU glue includes the raw material of following parts by weight：
7. a kind of high xanthochromia of resistance to UV cured film according to claim 6, it is characterised in that：The benzophenone chemical combination
Object is 4,4'-Dihydroxybenzophenone, 2,4-DihydroxyBenzophenone, 2- hydroxyl -4- dodecyls benzophenone, 4- ammonia
The chloro- 2 '-fluorine benzophenone of base -4 '-chlorobenzophenone, 4- nitros -4 '-chlorobenzophenone, 2- amino -5-, 2,3,4- trihydroxies
At least one of benzophenone and 2-hydroxy-4-n-octoxybenzophenone；The solvent is ether, tetrahydrofuran, positive fourth
At least one of alcohol, ethyl alcohol, acetone and cyclohexanone.
8. a kind of preparation method of the high xanthochromia of the resistance to UV cured film thoroughly of such as claim 1-7 any one of them, it is characterised in that：Packet
Include following steps：
(1) cuticular layer is prepared：A cuticula base material is taken, organic silica gel glue is coated on the surface of cuticula base material, is obtained after cured
Cuticular layer；
(2) composite layer is prepared：A main base material is taken, in the coated on one side UV glue of main base material, passes through first time heat cure, the successively
After photocuring, UV hardened layers are formed on a surface of main base material, being then covered with step (1) on the surface of UV hardened layers is made
Cuticular layer, obtain composite layer；
(3) the high xanthochromia of resistance to UV cured film thoroughly is prepared：The another side of main base material is coated with PU glue in the composite layer made from step (2)
Water forms PU glue-lines on another surface of main base material, is then covered on the surface of PU glue-lines release after second of heat cure
Film obtains the high xanthochromia of resistance to UV cured film thoroughly.
9. a kind of preparation method of the high xanthochromia of resistance to UV cured film according to claim 8, it is characterised in that：The step
(2) in, coating UV glue uses comma scraper coating method, and the temperature of the first time heat cure is 60-150 DEG C, for the first time
The time of heat cure is 1-3min；The first time photocuring uses UV photocuring modes, and the UV lamp energy of UV photocurings is
460-710mJ/cm2, the time of UV photocurings is 1-5min.
10. a kind of preparation method of the high xanthochromia of resistance to UV cured film according to claim 8, it is characterised in that：The step
Suddenly in (3), the temperature of second of heat cure is 60-150 DEG C, and the time of second of heat cure is 1-3min.
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| CN111704872A (en) * | 2020-06-29 | 2020-09-25 | 极天羽技术股份有限公司 | PU (polyurethane) adhesive protective film for display screen and preparation method thereof |
| CN115403874A (en) * | 2022-08-19 | 2022-11-29 | 国网黑龙江省电力有限公司电力科学研究院 | Nonlinear ethylene propylene rubber composite material with high electric strength resistance and high electric conductivity and preparation method thereof |
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Application publication date: 20180713 |