CN112251161A - Elastomer protective film with patterns and preparation method thereof - Google Patents
Elastomer protective film with patterns and preparation method thereof Download PDFInfo
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- CN112251161A CN112251161A CN202011226831.2A CN202011226831A CN112251161A CN 112251161 A CN112251161 A CN 112251161A CN 202011226831 A CN202011226831 A CN 202011226831A CN 112251161 A CN112251161 A CN 112251161A
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/29—Laminated material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C09J2475/00—Presence of polyurethane
- C09J2475/006—Presence of polyurethane in the substrate
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses an elastomer protective film with patterns and a preparation method thereof. The preparation method comprises the following steps: (1) hot-pressing the film with patterns and the elastomer base film to form a concave pattern surface layer; (2) coating a photo-curing coating composition and a photoinitiator on the other side surface of the elastomer base film with the concave pattern surface layer, and irradiating ultraviolet light at room temperature; (3) coating a back adhesive on the surface layer of the concave pattern, and baking and curing at 70-80 ℃ to obtain the self-repairing elastomer protective film with the pattern. The surface layer of the self-repairing elastomer protective film with the patterns has strong bonding force with the pattern layer, is not easy to fall off, has good surface friction resistance and good weather resistance, and has a self-repairing function.
Description
Technical Field
The invention relates to the field of film preparation, in particular to an elastomer protective film with patterns and a preparation method thereof.
Background
The existing multilayer film containing the polyurethane material layer is widely applied to the automobile industry, and with the improvement and the change of aesthetic abilities of people, single-tone products are increasingly unable to meet the aesthetic requirements of people, and the multilayer film with the pattern effect on the surface is hopefully prepared. Particularly, in the case of a paint protective film, it is necessary to form a pattern on the surface of the paint protective film for decorative effects.
However, it is difficult to prepare and maintain the pattern layer in the existing multilayer elastic film structure, because the elastic material can cause the pattern layer to be easily deformed or even disappear during the subsequent heat treatment, thereby limiting the application of the film with patterns on the surface.
Disclosure of Invention
In view of this, the invention provides a patterned elastomer protective film and a preparation method thereof. The surface layer of the self-repairing elastomer protective film with the patterns has strong bonding force with the pattern layer, is not easy to fall off, has good surface friction resistance and weather resistance, and has a self-repairing function.
The invention provides a preparation method of an elastomer protective film with patterns, which comprises the following steps:
(1) hot-pressing the patterned film with an elastomer (preferably Thermoplastic Polyurethane (TPU)) base film to form a concave patterned surface layer;
(2) coating a photo-curing coating composition and a photoinitiator on the other side surface of the elastomer base film with the concave pattern surface layer, and irradiating ultraviolet light at room temperature;
(3) coating a back adhesive on the surface layer of the concave pattern, and baking and curing at 70-80 ℃ to obtain the self-repairing elastomer protective film with the pattern;
the raw material formula of the photocureable coating composition comprises the following components in parts by weight: 10-20 parts of urethane acrylate, 3-5 parts of tridecyl methacrylate, 3-5 parts of 2- (perfluorooctyl) ethyl methacrylate, 2-4 parts of titanium compound, 1-3 parts of organic acid, 10-15 parts of styrene-butadiene-styrene block copolymer, 0.1-0.3 part of catalyst and 50-70 parts of solvent.
In the step (1), the pressure of hot pressing is preferably 3-8 Bar; the temperature is preferably 50 to 200 ℃, more preferably 80 to 150 ℃. The thickness of the concave pattern surface layer is preferably 20-30 micrometers.
Wherein the structural formula of the polyurethane acrylate is as follows:
wherein m is an integer of 3 to 6, n is an integer of 2 to 4, R1Is composed of
R2is-CH2CH2CH2-，R3Is composed of
R4is-CH2CH2-，R5is-CH3。
Among them, the photoinitiator is preferably one or more of 2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone and 1-hydroxycyclohexyl phenyl ketone.
Among them, the titanium compound is preferably n-butyl titanate and/or isopropyl titanate.
Wherein, the organic acid is preferably one or more of formic acid, acetic acid, propionic acid and butyric acid.
Among them, the catalyst is preferably one or more of iron silicide (FeSi), manganese silicide (MnSi), and cobalt silicide (CoSi). The catalyst plays a role in catalysis under the temperature condition of baking and curing, but does not play a role in catalysis under the light curing condition of ultraviolet irradiation, and the addition of the catalyst effectively realizes two times of curing reaction. In research, the particle size of the catalyst is preferably 50-100 nm; if the particle size is too small, particles cannot be formed, and the matching effect with nano-scale TiO2 particles formed after the titanium compound is hydrolyzed is not good; too large particle size affects the catalytic performance of the catalyst, resulting in poor curing effect of the bake cure.
Wherein, the solvent is preferably one or more of ethanol, isopropanol and n-butanol.
Preferably, the raw material formula of the photo-curing coating composition comprises the following components in parts by weight: 10-20 parts of urethane acrylate, 3-5 parts of tridecyl methacrylate, 3-5 parts of 2- (perfluorooctyl) ethyl methacrylate, 2-4 parts of titanium compound, 1-3 parts of organic acid, 10-15 parts of styrene-butadiene-styrene block copolymer, 0.1-0.3 part of catalyst and 50-70 parts of solvent.
The invention realizes the improvement of the adhesive property and the mechanical property of the protective film by curing reaction at two times and adopting a specific curing coating formula. In addition, the titanium compound has the characteristics of strong penetrability and easy hydrolysis, the titanium compound permeates into the concave patterns in a solution form to form a compact film layer in the coating process, and the adhesive nano-grade TiO2 particles are formed under the action of ultraviolet curing, so that the flat concave pattern structure is densely filled, and a flat and smooth protective film coating is further formed through subsequent baking and curing, so that the adhesive property of the protective film coating is improved.
Wherein the intensity of the ultraviolet irradiation is preferably 200 to 1500mJ/cm2。
The time for curing by ultraviolet irradiation is preferably 10 to 120 seconds.
The baking and curing time is preferably 3-5 minutes.
The invention also provides the elastomer protective film with the patterns, which is prepared by the preparation method.
In the present invention, the room temperature is 10 to 30 ℃.
The positive progress effect achieved by the invention is as follows: the surface layer of the self-repairing elastomer protective film with the patterns has strong bonding force with the pattern layer, is not easy to fall off, has good surface friction resistance and weather resistance, and has a self-repairing function.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The self-repairing test method comprises the following steps: after brushing the surface of the film with a straight wire brush, it was observed whether the brush marks automatically disappeared within 1 hour or disappeared under a heat source (e.g., hot water pouring). If the material can disappear, the material is considered to have a self-repairing function.
Gloss evaluation method: the flexible polymer substrate coated with the self-repairing coating is adhered to a ferrous metal plate, and the gloss of the surface of the material is observed from the front side and the side (45 degrees). The surface is smooth and reflective, the reverse image is clear and sharp, the gloss is considered to be excellent, otherwise, the gloss is considered to be poor.
Stain resistance evaluation method: marking the surface of the coating by using a 6881 black oily marking pen, placing for 1 day after the mark is dried, directly wiping by using a piece of mirror wiping paper or wiping by dipping the mirror wiping paper in absolute alcohol, and observing the clearing condition of the mark. The stain resistance is considered to be excellent if the mark can be completely wiped off without leaving a mark. If the mark is not erasable, the stain resistance is considered poor. Stain resistance is considered good if the mark can be wiped off, but there is a small amount of marking.
Elongation at break test method: cutting the material to be measured into sample strips with the specification of 5 cm (length) and 2 cm (width), marking the length of the middle 2 cm, forcibly stretching the sample strips to two sides until cracks appear, measuring the length L1 of the marked part at the moment, and then calculating the elongation at break according to the following formula.
Elongation at break (%) - (L1-2)/2
Example 1
The preparation method of the self-repairing polyurethane elastomer protective film with the patterns comprises the following steps:
(1) hot-pressing the film with patterns and a Thermoplastic Polyurethane (TPU) base film to form a concave pattern surface layer; the hot pressing pressure is 5Bar, the temperature is 50 ℃, and the thickness of the concave pattern surface layer is 20 microns;
(2) coating a photo-curing coating composition and a photoinitiator on the other side surface of the thermoplastic polyurethane base film with the concave pattern surface layer, and irradiating the other side surface of the thermoplastic polyurethane base film with the ultraviolet light at room temperature for 10 s; the intensity of ultraviolet irradiation is 300mJ/cm2；
(3) Coating gum on the surface layer of the concave pattern, baking and curing for 3 minutes at 70 ℃ to obtain the self-repairing polyurethane elastomer protective film with the pattern;
the raw material formula of the photocureable coating composition comprises the following components in parts by weight: 10 parts of urethane acrylate, 3 parts of tridecyl octyl methacrylate, 3 parts of 2- (perfluorooctyl) ethyl methacrylate, 2 parts of titanium compound, 1 part of organic acid, 10 parts of styrene-butadiene-styrene block copolymer, 0.1 part of catalyst and 50 parts of solvent.
The structural formula of the polyurethane acrylate is as follows:
wherein m is 3, n is 2, R1Is composed of
R2is-CH2CH2CH2-，R3Is composed of
R4is-CH2CH2-，R5is-CH3。
Wherein the photoinitiator is 2, 4, 6-trimethylbenzoyl-diphenyl phosphorus oxide; the titanium compound is n-butyl titanate; the organic acid is formic acid; the catalyst is iron silicide (FeSi); the solvent is ethanol.
The self-repairing polyurethane elastomer protective film with the patterns prepared in the embodiment has the following properties:
(1) the surface coating film has good adhesion fastness with the pattern surface layer, is not easy to fall off, and the hundred-grid test reaches 5B;
(2) the scratch resistance is good, and the No. 0000 steel wire is loaded with 1kg and rubbed back and forth for more than 1000 times without scars;
(3) the protective film has excellent self-repairing performance, the elongation at break reaches 125%, the gloss is excellent, and the stain resistance is good;
(4) the weather resistance is good, and after the weather resistance cycle is repeated for 300 times, no crack or local peeling is still observed on the surface of the coating.
Example 2
The preparation method of the self-repairing polyurethane elastomer protective film with the patterns comprises the following steps:
(1) hot-pressing the film with patterns and a Thermoplastic Polyurethane (TPU) base film to form a concave pattern surface layer; the hot pressing pressure is 8Bar, the temperature is 80 ℃, and the thickness of the concave pattern surface layer is 30 microns;
(2) coating a photo-curing coating composition and a photoinitiator on the other side surface of the thermoplastic polyurethane base film with the concave pattern surface layer, and irradiating the other side surface of the thermoplastic polyurethane base film with the ultraviolet light at room temperature for 120 s; the intensity of ultraviolet irradiation was 1500mJ/cm2；
(3) Coating gum on the surface layer of the concave pattern, baking and curing for 5 minutes at 80 ℃ to obtain the self-repairing polyurethane elastomer protective film with the pattern;
the raw material formula of the photocureable coating composition comprises the following components in parts by weight: 20 parts of urethane acrylate, 5 parts of tridecyl methacrylate, 5 parts of 2- (perfluorooctyl) ethyl methacrylate, 4 parts of titanium compound, 3 parts of organic acid, 15 parts of styrene-butadiene-styrene block copolymer, 0.3 part of catalyst and 70 parts of solvent.
The structural formula of the polyurethane acrylate is as follows:
wherein m is 6, n is 4, R1Is composed of
R2is-CH2CH2CH2-，R3Is composed of
R4is-CH2CH2-，R5is-CH3。
Wherein the photoinitiator is 2-hydroxy-2-methyl-1-phenyl-1-acetone; the titanium compound is isopropyl titanate; the organic acid is acetic acid; the catalyst is manganese silicide (MnSi); the solvent is isopropanol.
The self-repairing polyurethane elastomer protective film with the patterns prepared in the embodiment has the following properties:
(1) the surface coating film has good adhesion fastness with the pattern surface layer, is not easy to fall off, and the hundred-grid test reaches 5B;
(2) the scratch resistance is good, and the No. 0000 steel wire is loaded with 1kg and rubbed back and forth for more than 1000 times without scars;
(3) the protective film has excellent self-repairing performance, the elongation at break reaches 115%, the gloss is excellent, and the stain resistance is good;
(4) the weather resistance is good, and after the weather resistance cycle is repeated for 300 times, no crack or local peeling is still observed on the surface of the coating.
Claims (10)
1. A preparation method of an elastomer protective film with patterns comprises the following steps:
(1) hot-pressing the film with patterns and the elastomer base film to form a concave pattern surface layer;
(2) coating a photo-curing coating composition and a photoinitiator on the other side surface of the elastomer base film with the concave pattern surface layer, and irradiating ultraviolet light at room temperature;
(3) coating a back adhesive on the surface layer of the concave pattern, and baking and curing at 70-80 ℃ to obtain the elastomer protective film with the pattern;
the raw material formula of the photocureable coating composition comprises the following components in parts by weight: 10-20 parts of urethane acrylate, 3-5 parts of tridecyl methacrylate, 3-5 parts of 2- (perfluorooctyl) ethyl methacrylate, 2-4 parts of titanium compound, 1-3 parts of organic acid, 10-15 parts of styrene-butadiene-styrene block copolymer, 0.1-0.3 part of catalyst and 50-70 parts of solvent.
2. The method of claim 1, wherein the elastomer is a thermoplastic polyurethane.
3. The preparation method according to claim 1, wherein in the step (1), the pressure of the hot pressing is 3-8 Bar; the temperature is 50-200 ℃, preferably 80-150 ℃; the thickness of the concave pattern surface layer is 20-30 microns.
4. The method of claim 1, wherein the urethane acrylate has the formula:
wherein m is an integer of 3 to 6, n is an integer of 2 to 4, R1Is composed of
R2is-CH2CH2CH2-，R3Is composed of
R4is-CH2CH2-，R5is-CH3。
5. The method of claim 1, wherein the photoinitiator is one or more of 2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone and 1-hydroxycyclohexylphenylketone.
6. The process according to claim 1, wherein the titanium compound is n-butyl titanate and/or isopropyl titanate; the organic acid is one or more of formic acid, acetic acid, propionic acid and butyric acid; the catalyst is one or more of iron silicide, manganese silicide and cobalt silicide; the particle size of the catalyst is preferably 50 to 100 nm.
7. The method of claim 1, wherein the light curable coating composition comprises the following components in parts by weight: 10-20 parts of urethane acrylate, 3-5 parts of tridecyl methacrylate, 3-5 parts of 2- (perfluorooctyl) ethyl methacrylate, 2-4 parts of titanium compound, 1-3 parts of organic acid, 10-15 parts of styrene-butadiene-styrene block copolymer, 0.1-0.3 part of catalyst and 50-70 parts of solvent.
8. The method according to claim 1, wherein the intensity of the ultraviolet light irradiation is 200 to 1500mJ/cm2(ii) a The ultraviolet light irradiation curing time is 10-120 seconds.
9. The method according to claim 1, wherein the baking time is 3 to 5 minutes.
10. A textured elastomer protective film produced by the production method according to any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114479707A (en) * | 2022-02-26 | 2022-05-13 | 浙江世窗光学薄膜制造有限公司 | Polyurethane multilayer film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479707A (en) * | 2022-02-26 | 2022-05-13 | 浙江世窗光学薄膜制造有限公司 | Polyurethane multilayer film and preparation method thereof |
| CN114479707B (en) * | 2022-02-26 | 2023-03-14 | 浙江世窗光学薄膜制造有限公司 | Polyurethane multilayer film and preparation method thereof |
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| CN112251161B (en) | 2022-05-31 |
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