CN111849008B - High-ductility optical hardening film and preparation method thereof - Google Patents
High-ductility optical hardening film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-ductility optical hardening film and a preparation method thereof. The protective film has high ductility, can be generally applied to screen protection of various mobile phones, can realize various forming modes, and can meet the requirement of product luminous flux by selecting the base material in consideration of fingerprint unlocking; the protective film has excellent touch feeling and wear resistance, can prevent scratching and fingerprint residue under the condition of long-time use, and provides stable, effective and comprehensive protection for a screen.
Description
Technical Field
The invention relates to the technical field of protective films, in particular to a high-ductility optical hardening film and a preparation method thereof.
Background
In recent years, mobile phone products gradually enter a full-screen era, various screen display modes are provided by manufacturers, and in order to increase the screen occupation ratio, different modes such as a 2.5D/3D mode, a waterfall screen mode and a full-screen mode are adopted. Various molding requirements also determine that the ductility of the hardened coating cannot be too low, and hardened coatings with too low ductility are prone to cracking during molding or poor shape retention after molding, i.e., they tend to spring back after hoop testing. Therefore, there is a need for an optical cured film that has both hardening performance and high ductility.
At present, the high-ductility optical hardening film has the following two schemes: the first scheme is to use a common PET base film mode to carry out hardening coating treatment on the base film, but the physical property and ductility of the hardening coating of the protective film cannot be well balanced, cracks can occur after the protective film is used for a certain number of times, and the bonding warping condition can also occur after ring measurement; the second method is a post-curing method, which is equivalent to an improvement in the molding method, and a coating solution is prepared by using a thermosetting-UV dual-curing component, and thermosetting is performed first or thermosetting is performed and then a part of UV curing is performed to make a reactive component in a system in a half-reaction state, and then UV curing is performed after lamination to make the reactive component sufficiently react. However, this approach requires the consumer or manufacturer to coordinate the use of back-end UV curing and control during shipping becomes problematic. The above two solutions provide a certain protection of the protective film to some extent, but the corresponding defects are generated and need to be improved.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defect of balance of high ductility and other physical properties which is not possessed by the conventional protective films of the same type, and provides a high-ductility optical hardening film and a preparation method thereof. The high-ductility optical hardening film has the advantages of bonding performance, fingerprint prevention effect and wear resistance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a high-ductility optical hardening film comprises a high-ductility hardening layer, a bottom coating and a base material layer which are sequentially laminated from top to bottom;
the high-ductility hardened layer comprises 30-45% of hexa-functionality unsaturated functional group polymer, 45-63% of solvent, 2-8% of initiator and 1-5% of additive in percentage by mass; the mass percentage of each component of the high-ductility hardened layer accounts for the total components of the high-ductility hardened layer;
the primer layer comprises 20-55% of trifunctional or tetrafunctional unsaturated functional group polymer, 40-75% of solvent and 2-8% of initiator by mass percentage; the mass percentage of each component of the base coat accounts for the total components of the base coat;
the polymer with unsaturated functional groups comprises any one or more of polyurethane oligomer, polyurethane acrylate oligomer, polyester acrylate oligomer and epoxy acrylate oligomer.
In the technical scheme, the high-ductility hardened layer is a coating formed by heating and baking hardening coating liquid to volatilize a solvent and then curing after UV irradiation, and further has the functions of hardness, wear resistance and other physical properties after curing.
In the technical scheme, the base coat is formed by curing a thermosetting or UV curing coating liquid, and has the main function of preventing the hardening coating liquid from penetrating into the base material so as to influence the characteristics of the base material; another function is to promote adhesion of the high ductility hardened layer to the substrate.
Preferably, the hexafunctional unsaturated functional polymer is a hexafunctional urethane acrylate oligomer having 6 reactive double bonds.
Preferably, the solvent comprises any one or more of isopropanol, acetone, methyl isobutyl ketone, butanone, propylene glycol methyl ether, propylene glycol monobutyl ether, methyl acetate, ethyl acetate and butyl acetate.
More preferably, the solvent is methyl isobutyl ketone.
Preferably, the initiator includes any one or two of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 1-hydroxycyclohexylphenylketone, ethyl 2,4, 6-trimethylbenzoylphosphonate, 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-propanone, 2-isopropylthioxanthone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone, and phenylbis (2, 4, 6-trimethylbenzoyl) phosphine oxide.
More preferably, the initiator is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide or 1-hydroxycyclohexylphenylketone.
Preferably, the additive comprises any one or two of a surface leveling auxiliary agent, a silicon dioxide particle dispersion liquid, an initiator aid and a reaction catalyst, and plays a role in adjusting the performance of the hardened coating.
More preferably, the additive is a leveling agent.
Most preferably, the leveling agent is a siloxane-modified perfluoropolyether polymer.
Preferably, the trifunctional or tetrafunctional unsaturated functional group polymer is a trifunctional or tetrafunctional urethane acrylate oligomer having a number of reactive double bonds of 3 or 4.
Preferably, the thickness of the high ductility hardened layer is 1 to 10 μm.
More preferably, the thickness of the high ductility hardened layer is 2 to 8 μm.
Preferably, the primer layer is in a UV cured form.
Preferably, the thickness of the primer layer is 0.1 to 10 μm.
More preferably, the thickness of the primer layer is 0.1 to 5 μm.
Preferably, the substrate layer is a transparent substrate film layer, and the material of the substrate layer is any one of PET, TAC, SRF, PI, TPU, and COP.
More preferably, the material of the substrate layer is TPU due to its unique properties.
Most preferably, the substrate layer is made by Ningbohui Star New Material science and technology, inc., under the name H8HY1T-NR-080.
Preferably, the thickness of the substrate layer is 75 to 125 μm.
Preferably, the thickness of the substrate layer is 50 to 125 μm.
A method for preparing a high-ductility optical hardening film comprises the following steps:
a first coating step: coating a primer coating liquid on one surface of the upper layer of the substrate layer, heating the substrate layer in an oven, volatilizing a solvent, and carrying out UV curing to obtain a primer coating;
a second coating step: and under the condition that the first coating step is completed, coating a high-ductility hardening coating solution on the upper layer of the bottom coating, heating the coating by using an oven, volatilizing the solvent, and carrying out UV curing to obtain the high-ductility hardening layer.
Preferably, in the first coating step, the bottom coating is coated by a micro-gravure coating mode, the rotating speed of a coating roller is 3-17 m/min, the feeding speed of the base material is 5-25 m/min, the oven temperature is 60-150 ℃, the curing time is 2-5 min, the UV curing energy is 100-300 mJ/cm 2 。
More preferably, in the first coating step, the rotation speed of the coating roll5-13 m/min, the feeding speed of the base material is 8-16 m/min, the temperature of the oven is 60-80 ℃, the curing time is 2-4 min, and the UV curing energy is 200-300 mJ/cm 2 。
Preferably, in the second coating step, the high-ductility hardened layer is coated by a micro-gravure coating method, the rotating speed of a coating roller is 3-17 m/min, the feeding speed of the base material coated with the base coating is 5-25 m/min, the temperature of an oven is 60-150 ℃, the curing time is 2-4 min, the UV curing energy is 100-600 mJ/cm 2 。
More preferably, in the second coating step, the rotation speed of the coating roller is 5-13 m/min, the feeding speed of the base material coated with the base coating is 8-16 m/min, the temperature of the oven is 60-80 ℃, the curing time is 2min, and the UV curing energy is 150-300 mJ/cm 2 。
The basic principle of the invention is as follows:
the invention provides a high-ductility optical hardening film, which mainly comprises a base material layer, an intermediate primer layer and a topmost high-ductility hardening layer. Wherein the substrate layer is the transparent substrate who has special optical structure that Ningbo costing star new material science and technology limited produced, and middle under coat is for possessing the bonding, preventing solvent infiltration and playing the thermosetting or the UV curing coating of transition modulus effect, and high ductility sclerosis layer is the UV curing coating that possesses functions such as high wear-resisting, high hydrolysis and high ductility.
The base material layer is a layer of base material which simultaneously has the advantages of drop resistance, good forming performance and stable luminous flux; the invention effectively exerts the advantages of the transparent base material through the specific high-ductility optical hardening coating and the preparation method thereof, prevents the penetration of coating liquid to the base material by utilizing the bottom coating and ensures the adhesive force, and the bottom coating is used as an intermediate transition layer, and indirectly used as the intermediate modulus transition layer because the modulus is between the bottom coating and the intermediate modulus transition layer, thereby improving the situation that the traditional structure is easy to tear, and the high-ductility optical coating on the outermost layer not only provides various physical properties required by the optical hardening film, but also ensures that the protective film has excellent forming effect.
The coating and laminating method for the protective film provided by the invention has the advantages of simple process requirement, safe operation and easy realization.
Compared with the prior art, the invention has the beneficial effects that:
(1) The protective film has high ductility, can be generally applied to screen protection of various mobile phones, can realize various forming modes, and can meet the requirement of product luminous flux by selecting the base material in consideration of fingerprint unlocking; the protective film has excellent touch hand feeling and wear resistance, can prevent scratching and fingerprint residue under the condition of long-time use, and provides stable, effective and comprehensive protection for a screen;
(2) The high-ductility optical hardening film provided by the invention overcomes the defects that the existing protective film cannot realize various forming modes or does not have universal luminous flux requirements;
(3) According to the high-ductility optical hardening film disclosed by the invention, a double-layer coating structure is adopted, and the additive with better reactivity is used in the second coating layer, so that the wear resistance and the surface water contact angle of a finished product are enhanced.
Drawings
FIG. 1 is a schematic structural diagram of a high-ductility optically hardened film according to example 1 of the present invention.
The corresponding part names for the various reference numbers in the figures are:
1-a high ductility hardened layer; 2-a base coat; 3-a substrate layer.
Detailed Description
For a better understanding of the present invention, reference is made to the following detailed description and accompanying drawings. It should be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
The trifunctional urethane acrylate oligomer described in examples 1 to 3 and comparative examples 1 to 4 was CN8009 NS manufactured by Shadoma (China) Co., ltd., the hexafunctional urethane acrylate oligomer was 6161 to 100 manufactured by Changxing Special materials Co., ltd., the sixteen functional urethane acrylate oligomer was CN2302 manufactured by Shadoma (China) Co., ltd., the leveling agent was UVR-610 manufactured by Shanghai Korea International trade Co., ltd., and the base material layer was manufactured by Ningbo Star New materials science & technology Co., ltd., the name H8HY1T-NR-080.
Example 1
A high-ductility optically hardened film, as shown in FIG. 1, comprises a high-ductility hardened layer 1, an undercoat layer 2, and a base material layer 3 stacked in this order from the top.
The high-ductility hardened layer 1 comprises 30% of hexa-functionality polyurethane acrylate oligomer (with good flexibility and hardness and serving as a main film forming substance), 63% of methyl isobutyl ketone, 4% of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 3% of leveling agent siloxane modified perfluoropolyether polymer (performance after film forming is adjusted).
The primer layer 2 comprises 25% of trifunctional polyurethane acrylate oligomer, 69% of methyl isobutyl ketone and 6% of 1-hydroxycyclohexyl phenyl ketone by mass percentage.
The substrate layer 3 is a transparent base film layer.
The transparent substrate layer 3 of the protection film that this embodiment provided has special construction and shaping mode, can not influence fingerprint unblock under the screen, and the modulus of itself is lower, easily realizes the shaping of various modes. The transparent base layer 3 has various functions and can be adjusted in performance according to the purpose.
The preparation method of the high-ductility optical hardening protective film comprises the following steps:
a first coating step: taking a transparent substrate layer 3, coating a primary coating liquid on the single side of the upper layer of the transparent substrate layer 3, heating by an oven, volatilizing a solvent, and carrying out UV curing to obtain a primary coating layer 2;
a second coating step: and (3) taking the transparent substrate film in the first coating step, coating the high-ductility hardening coating liquid on the upper layer of the bottom coating layer 2, heating in an oven, volatilizing the solvent, and carrying out UV curing to obtain the high-ductility hardening layer 1.
In the first coating step, the thickness of the base material layer 3 is 100 μm; the bottom coating 2 is coated by adopting a micro-concave coating mode, the rotating speed of a coating roller is 5-6 m/min, the feeding speed of a base material is 10m/min, the temperature of an oven is 120 ℃, the curing time is 2min, and the UV curing energy is 200-250 mJ/cm 2 The thickness of the coating was 1.0. Mu.m.
In the second coating step, the high-elongation-rate hardened coating 1 is coated in a micro-concave coating mode, the rotating speed of a coating roller is 6-8 m/min, the feeding speed of the base material coated with the base coating 2 is 10m/min, the temperature of an oven is 80 ℃, the curing time is 2min, the UV curing energy is 200-250 mJ/cm 2 The coating thickness was 2.6. Mu.m.
The protective film provided in this embodiment has the undercoat layer 2 provided on the transparent base material layer 3, and the undercoat layer 2 can maintain good adhesion after completion of curing and can prevent penetration of the cured coating liquid into the base material.
The protection film provided by the embodiment is provided with the high ductility hardening layer 1 on the primer layer 2, and the high ductility hardening layer 1 can reach at least 105 degrees of water contact angle and at least 60 degrees of oil contact angle after being cured, so that the residual fingerprint is easier to erase, and the requirement that the steel wool is resistant to abrasion for at least 2500 times can be met.
Example 2
This example is substantially the same as example 1, except that:
the high-ductility hardened layer 1 comprises 38% of hexafunctional polyurethane acrylate oligomer, 55% of methyl isobutyl ketone, 5% of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 2% of leveling agent siloxane modified perfluoropolyether polymer in percentage by mass.
The primer layer 2 comprises 40% of trifunctional urethane acrylate oligomer, 53% of methyl isobutyl ketone and 7% of 1-hydroxycyclohexyl phenyl ketone by mass percentage.
A method for preparing a high ductility optical hardening protective film as described above is substantially the same as in example 1, except that:
in the first coating step, the rotating speed of the coating roller is 7 to E8m/min, the feeding speed of the base material is 10m/min, the temperature of the oven is 120 ℃, the curing time is 2min, the UV curing energy is 200-250 mJ/cm 2 The coating thickness was 2.0. Mu.m.
In the second coating step, the rotating speed of a coating roller is 6-8 m/min, the feeding speed of the base material coated with the bottom coating is 10m/min, the temperature of an oven is 80 ℃, the curing time is 2min, and the UV curing energy is 200-250 mJ/cm 2 The coating thickness was 3.1. Mu.m.
Example 3
This example is essentially the same as example 1, except that:
the high-ductility hardened layer 1 comprises 43% of hexafunctional polyurethane acrylate oligomer, 47% of methyl isobutyl ketone, 5% of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 5% of leveling agent siloxane modified perfluoropolyether polymer in percentage by mass.
The primer layer 2 comprises 55% of trifunctional urethane acrylate oligomer, 41% of methyl isobutyl ketone and 4% of 1-hydroxycyclohexyl phenyl ketone by mass percentage.
The method for preparing the high-ductility optical hardening protective film is basically the same as the embodiment 1, except that:
in the first coating step, the rotating speed of the coating roller is about 10m/min, the feeding speed of the base material is 12m/min, the temperature of the oven is 120 ℃, the curing time is 2min, and the UV curing energy is 200-250 mJ/cm 2 The thickness of the coating layer was about 3.5. Mu.m.
In the second coating step, the rotating speed of a coating roller is about 9m/min, the feeding speed of the base material coated with the bottom coating is 10m/min, the temperature of an oven is 80 ℃, the curing time is 2min, and the UV curing energy is 250-300 mJ/cm 2 The thickness of the coating layer was about 3.7. Mu.m.
Comparative example 1
This comparative example is substantially the same as example 1 except that the primer layer 2 is not present in the cured film of this comparative example.
The comparative example hardened film was produced in substantially the same manner as in example 1 except that: this comparative example eliminates the primer layer 2 in the first coating step and directly coats the high ductility hardening layer 1 on the transparent base material layer 3.
Comparative example 2
This comparative example is substantially the same as example 1 except that the additive amount of the high ductility hardened layer 1 of this comparative example is 0.5%, and the method for producing a hardened film is adjusted accordingly.
Comparative example 3
This comparative example is substantially the same as example 1 except that the polymer of 1 in the high ductility hardened layer of this comparative example is a urethane acrylate oligomer having sixteen functionality, and the method of producing the hardened film was adjusted accordingly.
Comparative example 4
This comparative example is substantially the same as example 1 except that the polymer of the primer layer 2 of this comparative example is a hexafunctional urethane acrylate oligomer and the method of preparing the cured film is adjusted accordingly.
Effects of the embodiment
The main properties of the films prepared in examples 1 to 3 and comparative examples 1 to 4 were measured, and the results are shown in table 1. The wear resistance is tested by a steel wool wear resistance tester, the load is 1kg, the higher the wear resistance frequency is, and the better the wear resistance effect is; the water contact angle is tested by adopting a water contact angle tester, and the higher the water contact angle is, the better the surface anti-fouling effect is; the elongation and the tensile strength are tested by a universal tester, and the higher the elongation is, the better the forming effect is relatively.
TABLE 1 results of performance test of films obtained in examples 1 to 3 and comparative examples 1 to 4
As can be seen from Table 1, since the composition ratios of the film layers and the preparation processes of examples 1 to 3 are within the ranges of the present invention, the properties of the obtained high ductility optically hardened film are within reasonable ranges.
In addition, compared with the example 1, the comparative example 1 has no base coating, so that the performances such as tear resistance and stretching are greatly influenced, and the water contact angle is obviously reduced due to the penetration of the surface auxiliary agent; comparative example 2 compared to example 1, the water contact angle and wear resistance were more seriously affected, indicating that the film properties were greatly affected by the addition amount of the additive of the high ductility hardened layer 1; compared with the example 1, the high-ductility hardened coating has high functionality, large shrinkage rate after film forming and easy internal shrinkage, so that the influence on the tear resistance and the tensile resistance is serious; comparative example 4 compared to example 1, the urethane acrylate oligomer used in the primer layer of comparative example 4 was hexafunctional and did not have the effect of transition modulus, resulting in a large difference in interlayer modulus and poor tear resistance.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also appreciate that they may make various changes, modifications, additions and substitutions within the spirit and scope of the invention.
Claims (9)
1. A high-ductility optical hardening film is characterized by comprising a high-ductility hardening layer (1), an undercoating layer (2) and a base material layer (3) which are sequentially laminated from top to bottom;
the high-ductility hardened layer (1) comprises 30-45% of hexa-functional unsaturated functional group polymer, 45-63% of solvent, 2-8% of initiator and 1-5% of additive in percentage by mass;
the additive is a leveling agent;
the leveling agent is a siloxane modified perfluoropolyether polymer;
the primer layer (2) comprises, by mass, 20% -55% of trifunctional or tetrafunctional unsaturated functional group polymer, 40% -75% of solvent and 2% -8% of initiator;
the polymer with unsaturated functional groups comprises any one or more of polyurethane acrylate oligomer, polyester acrylate oligomer and epoxy acrylate oligomer;
the base material layer (3) is a transparent base film layer, and the base material layer (3) is made of any one of PET, TAC, SRF, PI, TPU and COP.
2. The highly extensible optical cured film of claim 1, wherein the hexafunctional unsaturated functional polymer is a hexafunctional urethane acrylate oligomer.
3. The high ductility optical hardening film according to claim 1, wherein the solvent comprises one or more of isopropyl alcohol, acetone, methyl isobutyl ketone, methyl ethyl ketone, propylene glycol methyl ether, propylene glycol monobutyl ether, methyl acetate, ethyl acetate, and butyl acetate.
4. The highly extensible photohardenable film according to claim 1, wherein the initiator comprises one or two of 2,4, 6-trimethylbenzoyl diphenylphosphine oxide, 1-hydroxycyclohexylphenylketone, ethyl 2,4, 6-trimethylbenzoylphosphonate, 2-methyl-1- (4-methylthiophenyl) -2-morpholino-1-propanone, 2-isopropylthioxanthone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone, and phenylbis (2, 4, 6-trimethylbenzoyl) phosphine oxide.
5. The high ductility optically hardened film according to claim 1, wherein the trifunctional or tetrafunctional unsaturated functional polymer is a trifunctional or tetrafunctional urethane acrylate oligomer.
6. The high-ductility optically hardened film according to claim 1, wherein the thickness of the high-ductility hardened layer (1) is 1 to 10 μm, the thickness of the primer layer (2) is 0.1 to 10 μm, and the thickness of the base material layer (3) is 75 to 125 μm.
7. A method for preparing a high-ductility optically hardened film as claimed in any one of claims 1 to 6, comprising the steps of:
a first coating step: taking the coated substrate layer (3), coating a primer coating liquid on one surface of the upper layer of the substrate layer (3), heating by using an oven, volatilizing a solvent, and carrying out UV curing to obtain a primer coating (2);
a second coating step: when the first coating step is completed, a high-ductility hardening coating liquid is coated on the upper layer of the base coating layer (2), and after the high-ductility hardening coating liquid is heated by an oven and the solvent is evaporated, the high-ductility hardening layer (1) is obtained by UV curing.
8. The method for preparing the high-ductility optically hardened film according to claim 7, wherein in the first coating step, the primer layer (2) is coated by a dimple coating method, the rotation speed of a coating roller is 3 to 17m/min, the feeding speed of a base material is 5 to 25m/min, the oven temperature is 60 to 150 ℃, the curing time is 2 to 5min, and the UV curing energy is 100 to 300mJ/cm 2 。
9. The method for producing a high-ductility optically hardened film according to claim 7, wherein in the second coating step, the high-ductility hardened layer (1) is coated by a dimple coating method, the rotation speed of a coating roll is 3 to 17m/min, the feeding speed of a base material on which the undercoat layer (2) is coated is 5 to 25m/min, the oven temperature is 60 to 150 ℃, the curing time is 2 to 4min, and the UV curing energy is 100 to 600mJ/cm 2 。
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CN115926395A (en) * | 2022-12-28 | 2023-04-07 | 宁波惠之星新材料科技股份有限公司 | Optical film and preparation method thereof |
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