CN117247588A - Coating composition for enhancing adhesive force of transparent polyimide film and application thereof - Google Patents
Coating composition for enhancing adhesive force of transparent polyimide film and application thereof Download PDFInfo
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- CN117247588A CN117247588A CN202311443289.XA CN202311443289A CN117247588A CN 117247588 A CN117247588 A CN 117247588A CN 202311443289 A CN202311443289 A CN 202311443289A CN 117247588 A CN117247588 A CN 117247588A
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- Prior art keywords
- polyimide film
- coating
- coating composition
- adhesive force
- agent
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 118
- 239000000853 adhesive Substances 0.000 title claims abstract description 52
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 52
- 239000008199 coating composition Substances 0.000 title claims abstract description 48
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 60
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 39
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 24
- 229920002635 polyurethane Polymers 0.000 claims abstract description 18
- 239000004814 polyurethane Substances 0.000 claims abstract description 18
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012948 isocyanate Substances 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 7
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 7
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical group C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims description 63
- 238000000576 coating method Methods 0.000 claims description 63
- 239000010410 layer Substances 0.000 claims description 40
- 239000002318 adhesion promoter Substances 0.000 claims description 35
- 239000002904 solvent Substances 0.000 claims description 26
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 22
- 239000000080 wetting agent Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 12
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 12
- 239000011247 coating layer Substances 0.000 claims description 12
- 229920000570 polyether Polymers 0.000 claims description 12
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 11
- 239000004593 Epoxy Substances 0.000 claims description 6
- 239000012792 core layer Substances 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- -1 polydimethylsiloxane Polymers 0.000 claims description 6
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 2
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 2
- 239000012964 benzotriazole Substances 0.000 claims description 2
- 229940097275 indigo Drugs 0.000 claims description 2
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 11
- 125000003700 epoxy group Chemical group 0.000 abstract description 7
- 230000003287 optical effect Effects 0.000 abstract description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 6
- 230000001965 increasing effect Effects 0.000 abstract description 3
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical group N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 34
- 239000000975 dye Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 13
- 238000001723 curing Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 238000013007 heat curing Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000011527 polyurethane coating Substances 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 239000001007 phthalocyanine dye Substances 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical group 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
-
- 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
-
- 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
- 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
- C09D7/65—Additives macromolecular
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
- G09F9/301—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements flexible foldable or roll-able electronic displays, e.g. thin LCD, OLED
-
- 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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- 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
Abstract
The invention relates to the technical field of coating compositions, and discloses a coating composition for enhancing adhesive force of a transparent polyimide film and application thereof, wherein the composition comprises polyurethane resin, an adhesive force promoter, a thermosetting agent and an auxiliary agent, wherein the polyurethane resin is hydroxyl-terminated polyurethane, the adhesive force promoter is bisphenol A type epoxy resin, and the thermosetting agent is isocyanate curing agent; the hydroxyl-terminated group of the polyurethane resin in the coating composition reacts with the isocyanic acid group of the thermosetting agent to improve the adhesive force of polyurethane, and simultaneously the hydroxyl and the epoxy group in the adhesive force promoter can react with the isocyanic acid group to form a tighter network structure, so that the adhesive force of the polyimide film is obviously improved by the organic combination of the hydroxyl-terminated group and the epoxy group; in addition, the coating composition can reduce the color difference value and the yellow value of the flexible display cover plate, the adhesive force of the polyimide film is not changed obviously after aging treatment, and the optical performance and the aging resistance are increased obviously.
Description
Technical Field
The invention relates to the technical field of coating compositions, in particular to a coating composition for enhancing adhesive force of a transparent polyimide film and application thereof.
Background
The flexible display cover plate is a display component capable of being bent and folded, and the initial structure of the flexible display cover plate is a polyimide film and an ink layer coated on one side of the polyimide film; the main material of the polyimide film is fluoride modified polyimide, and the polyimide film is easy to damage in practical application due to low hardness of the polyimide film; therefore, in order to solve the above-mentioned problems, a new structure form of a cured layer-polyimide film-ink layer is proposed in the art, in which the hardness of the polyimide film is increased by the cured layer, which enables the polyimide film to maintain high flexibility while increasing its hardness.
The technical proposal is that the polyimide film is a fluoride modified polyimide film, the surface energy of the film is low, the film is difficult to wet and adhere, and the hardening layer is difficult to adhere on the surface of the polyimide film, so how to improve the adhesive force of the polyimide film becomes a key technology for solving the application problem of the hardening layer-polyimide film-ink layer structure; related technical schemes are disclosed at present, such as a precoating solution for enhancing the adhesive force of the surface of a transparent PI substrate and an application method thereof disclosed in publication No. CN110591471B, wherein the solution is characterized in that the surface of a polyimide film is eroded by a solvent to form a rough structure on the surface of the film, and then a high polymer material of a hardening layer is rooted in the rough structure, so that the adhesive force of the hardening layer and the polyimide film is improved.
During further research, those skilled in the art have found that the use of solvents alone has limited ability to improve adhesion of polyimide films; therefore, a new technical scheme capable of remarkably improving the adhesive force of the polyimide film is provided by the person in the art, such as an additional coating for a transparent polyimide film, a use method thereof and a cover plate film disclosed in publication No. CN114181420B, and the technical scheme takes polyurethane resin, a silane wetting agent, a photoinitiator and a solvent as raw materials to form an additional coating with high adhesive force between a hardening layer and the polyimide film, so that the adhesive force of the polyimide film is remarkably improved; by the scheme, how to select the raw materials of the additional coating is of great significance to improving the adhesive force of the polyimide film.
Disclosure of Invention
In order to improve the adhesive force of a polyimide film, the invention provides a coating composition for enhancing the adhesive force of a transparent polyimide film and application thereof, wherein the composition comprises polyurethane resin, an adhesive force promoter and a thermosetting agent, the polyurethane resin is hydroxyl-terminated polyurethane, the thermosetting agent is isocyanate curing agent, the adhesive force promoter is bisphenol A epoxy resin, the hydroxyl-terminated groups in the polyurethane resin and the thermosetting agent react with isocyanate groups to enable the polyurethane to be more firmly adhered to the surface of the polyimide film, the adhesive force of the polyurethane can be improved, the adhesive force promoter contains hydroxyl groups and epoxy groups, the hydroxyl groups and the epoxy groups can react with the isocyanate groups to form a tighter network structure, and the adhesive force of the coating composition is obviously improved by organic combination of the three, so that the adhesive force of the polyimide film to a hardened layer and an ink layer is obviously improved.
The specific technical scheme of the invention is as follows:
the coating composition for enhancing the adhesive force of the transparent polyimide film comprises the following raw materials in parts by mass: 10-30 parts of polyurethane resin, 1-2 parts of adhesion promoter, 1-2 parts of thermosetting agent and the balance of auxiliary agent; the polyurethane resin is hydroxyl-terminated polyurethane; the adhesion promoter is bisphenol A type epoxy resin; the thermosetting agent is isocyanate curing agent.
The invention provides a coating composition for enhancing the adhesive force of a polyimide film, which comprises polyurethane resin, an adhesive force promoter and a thermosetting agent, wherein the composition can form a layer of coating on the polyimide film, and the coating can remarkably enhance the adhesive force of the polyimide film; according to the invention, the polyurethane resin is selected as hydroxyl-terminated polyurethane, the thermosetting agent is isocyanate curing agent, the hydroxyl-terminated polyurethane can be firmly adhered to the surface of the polyimide film by reacting with isocyanate groups, the adhesive force between the polyimide film and a polyurethane coating can be improved, the bisphenol A epoxy resin is also added into the composition as an adhesive force promoter, the hydroxyl groups and the epoxy groups in the bisphenol A epoxy resin can react with the isocyanate groups in the thermosetting agent to form a tighter network structure, so that the adhesive force of the coating is further improved, the adhesive force of the coating formed by the coating composition is obviously improved by organically combining the polyurethane resin, the thermosetting agent and the adhesive force promoter, and the adhesive force of the polyimide film to a hardening layer and an ink layer is obviously improved by using the coating composition as a connecting layer.
Preferably, the molecular weight of the adhesion promoter is less than or equal to 800 g/mol, the epoxy value is more than 0.44, and the molecular weight of the polyurethane resin is 50000-100000 g/mol.
Preferably, the auxiliary agent comprises the following components in parts by mass: 0.2-0.3 part of wetting agent, 0.05-0.1 part of leveling agent, 0.05-0.1 part of dye, 0.1-0.2 part of ultraviolet absorber and 90-110 parts of solvent.
Preferably, the wetting agent is a polyether modified polyorganosiloxane.
Preferably, the leveling agent is polyether modified polydimethylsiloxane.
The leveling agent can enable the coating composition to form a flat, smooth and uniform coating after being cured, ensure the flatness of the additional coating and ensure the quality of the finally manufactured flexible display cover plate.
Preferably, the dye includes one of phthalocyanine-based dye, azo dye and indigo-based dye.
The dye provided by the invention is blue dye, so that a coating formed by the composition after curing is blue, and the color difference value and the yellow index of the polyamide film can be effectively reduced.
Preferably, the ultraviolet absorber comprises one or more of a benzophenone ultraviolet absorber, a benzotriazole ultraviolet absorber and a triazine ultraviolet absorber.
The ultraviolet absorber can enable a coating formed by the coating composition to have an anti-aging function, can ensure that the adhesive force of the coating formed by the coating composition is not changed obviously under long-time ultraviolet aging treatment, and obviously improves the anti-aging performance of a flexible display cover plate manufactured by applying the coating composition.
Preferably, the solvent comprises the following components in parts by weight: 1 dimethylacetamide and propylene glycol methyl ether acetate.
The application of the coating composition for enhancing the adhesive force of the transparent polyimide film in preparing the flexible display cover plate comprises the following steps:
step 1: adding polyurethane resin, a thermosetting agent, an adhesion promoter, a wetting agent, a leveling agent, a dye and an ultraviolet absorber into a solvent, and stirring to prepare a coating, wherein the stirring conditions comprise: stirring at 100-110 ℃ for 1-1.2 h;
step 2: coating the coating paint on the two side surfaces of the polyimide film, baking to prepare the polyimide film with an additional coating, wherein the coating thickness is 50-200 nm, and the baking conditions comprise: the temperature is 80-160 ℃ and the time is 5-10 min;
step 3: and coating a layer of hardening liquid and a layer of printing ink on two sides of the polyimide film with the additional coating respectively to prepare the flexible display cover plate.
The invention also provides an application method of the coating composition for enhancing the adhesive force of the transparent polyimide film in preparing the display cover plate, the method is simple in process and easy to industrially popularize, in addition, the method researches the process raw materials and conditions, wherein the adhesive force and the haze have great influence on the prepared flexible display cover plate, so that proper raw material proportion and process conditions need to be controlled to ensure that the adhesive force and the haze of the flexible display cover plate can meet application requirements.
Preferably, the flexible display cover plate comprises a polyimide film of a core layer, a coating layer attached to two side surfaces of the polyimide film, and an ink layer and a hardening layer attached to the surface of the coating layer and positioned on the opposite side of the polyimide film.
Compared with the prior art, the invention has the following technical effects:
(1) The polyurethane resin in the composition provided by the invention is hydroxyl-terminated polyurethane, the thermosetting agent is isocyanate curing agent, the adhesion promoter is bisphenol A epoxy resin, and the hydroxyl-terminated of the polyurethane resin reacts with the isocyanate group of the thermosetting agent to enable the polyurethane coating to be more firmly adhered to the surface of the polyimide film, so that the adhesion of the polyurethane coating is obviously improved; in addition, the hydroxyl and epoxy groups of the adhesion promoter can also react with the isocyanate groups of the thermosetting agent to form a more compact network structure, and the organic combination of the hydroxyl and epoxy groups can further improve the adhesion of the polyurethane coating;
(2) The dye in the coating composition can reduce the color difference value and the yellow value of the flexible display cover plate, and can obviously improve the optical performance of the flexible display cover plate; the ultraviolet absorber in the coating composition can improve the ageing resistance of the polyurethane coating, and the adhesion of the polyimide film is not changed obviously after ageing treatment;
(3) The invention also provides an application method of the coating composition for enhancing the adhesive force of the transparent polyimide film, the method enables the adhesive force and the haze of the flexible display cover plate to meet the actual application requirements by controlling proper raw material proportion and process conditions, and the method has simple process and is easy for industrialized popularization.
Detailed Description
The invention is further described below with reference to examples.
Example 1:
the coating composition for enhancing the adhesive force of the transparent polyimide film comprises the following raw materials in parts by mass: 10 parts of polyurethane resin, 1.5 parts of adhesion promoter, 1 part of heat curing agent, 0.2 part of wetting agent, 0.05 part of leveling agent, 0.05 part of dye, 0.1 part of ultraviolet absorber and 100 parts of solvent; the polyurethane resin is a Shenghao RL9100 polyurethane, and the molecular weight of the polyurethane resin is 50000-100000 g/mol; the adhesion promoter is epoxy resin E-44 (6101), the molecular weight of the adhesion promoter is less than or equal to 800 g/mol, and the epoxy value is more than 0.41; the heat curing agent is isocyanate curing agent HF-1990, the wetting agent is polyether modified polyorganosiloxane, the leveling agent is polyether modified polydimethylsiloxane, the dye is phthalocyanine dye BGS, the ultraviolet absorber is Basoff UV327, and the solvent is prepared from the following components in parts by weight: 1 dimethylacetamide and propylene glycol methyl ether acetate;
the application of the coating composition for enhancing the adhesive force of the transparent polyimide film in preparing the flexible display cover plate comprises the following steps:
step 1: adding polyurethane resin, a thermosetting agent, an adhesion promoter, a wetting agent, a leveling agent, a dye and an ultraviolet absorber into a solvent, and stirring to prepare a coating, wherein the stirring conditions comprise: stirring temperature is 100 ℃, and stirring time is 1 h;
step 2: coating the coating paint on the two side surfaces of the polyimide film, baking to prepare the polyimide film with an additional coating, wherein the polyimide film is a fluorine modified polyimide film, the coating thickness is 100 nm, and the baking conditions comprise: 80. baking at 160deg.C for 5 min, and baking at 160deg.C for 5 min;
step 3: coating a layer of hardening liquid and a layer of printing ink on two sides of the polyimide film with the additional coating respectively to prepare a flexible display cover plate; the flexible display cover plate comprises a polyimide film of a core layer, a coating layer attached to the two side surfaces of the polyimide film, an ink layer and a hardening layer attached to the surface of the coating layer and positioned on the opposite side of the polyimide film.
Example 2:
in example 2, the polyurethane resin was 20 parts by mass compared with example 1, and the other conditions were the same as in example 1.
Example 3:
the polyurethane resin in example 3 was 30 parts by mass compared with example 1, and the other conditions were the same as in example 1.
Example 4:
the coating composition for enhancing the adhesive force of the transparent polyimide film comprises the following raw materials in parts by mass: 20 parts of polyurethane resin, 1.5 parts of adhesion promoter, 1.4 parts of heat curing agent, 0.26 part of wetting agent, 0.07 part of leveling agent, 0.07 part of dye, 0.16 part of ultraviolet absorber and 100 parts of solvent; the polyurethane resin is a Shenghao RL9100 polyurethane, and the molecular weight of the polyurethane resin is 50000-100000 g/mol; the adhesion promoter is epoxy resin E-44 (6101), the molecular weight of the adhesion promoter is less than or equal to 800 g/mol, and the epoxy value is more than 0.41; the heat curing agent is isocyanate curing agent HF-1990, the wetting agent is polyether modified polyorganosiloxane, the leveling agent is polyether modified polydimethylsiloxane, the dye is phthalocyanine dye BGS, the ultraviolet absorber is Basoff UV327, and the solvent is 2 in parts by weight: 1 dimethylacetamide and propylene glycol methyl ether acetate;
the application of the coating composition for enhancing the adhesive force of the transparent polyimide film in preparing the flexible display cover plate comprises the following steps:
step 1: adding polyurethane resin, a thermosetting agent, an adhesion promoter, a wetting agent, a leveling agent, a dye and an ultraviolet absorber into a solvent, and stirring to prepare a coating, wherein the stirring conditions comprise: stirring temperature is 100 ℃, and stirring time is 1 h;
step 2: coating the coating paint on the two side surfaces of the polyimide film, baking to prepare the polyimide film with an additional coating, wherein the polyimide film is a fluorine modified polyimide film, the coating thickness is 100 nm, and the baking conditions comprise: 80. baking at 160deg.C for 5 min, and baking at 160deg.C for 5 min;
step 3: coating a layer of hardening liquid and a layer of printing ink on two sides of the polyimide film with the additional coating respectively to prepare a flexible display cover plate; the flexible display cover plate comprises a polyimide film of a core layer, a coating layer attached to the two side surfaces of the polyimide film, an ink layer and a hardening layer attached to the surface of the coating layer and positioned on the opposite side of the polyimide film.
Example 5:
compared with example 4, the solvent in example 5 has a mass ratio of 3:1 dimethylacetamide and propylene glycol methyl ether acetate, the other conditions were the same as in example 4.
Example 6:
compared with example 4, the solvent in example 6 has a mass ratio of 4:1 dimethylacetamide and propylene glycol methyl ether acetate, the other conditions were the same as in example 4.
Example 7:
the coating composition for enhancing the adhesive force of the transparent polyimide film comprises the following raw materials in parts by mass: 20 parts of polyurethane resin, 1.5 parts of adhesion promoter, 1.6 parts of heat curing agent, 0.28 part of wetting agent, 0.1 part of leveling agent, 0.1 part of dye, 0.2 part of ultraviolet absorber and 100 parts of solvent; the polyurethane resin is a Shenghao RL9100 polyurethane, and the molecular weight of the polyurethane resin is 50000-100000 g/mol; the adhesion promoter is epoxy resin E-44 (6101), the molecular weight of the adhesion promoter is less than or equal to 800 g/mol, and the epoxy value is more than 0.41; the heat curing agent is isocyanate curing agent HF-1990, the wetting agent is polyether modified polyorganosiloxane, the leveling agent is polyether modified polydimethylsiloxane, the dye is phthalocyanine dye BGS, the ultraviolet absorber is Basoff UV327, and the solvent is prepared from the following components in parts by weight: 1 dimethylacetamide and propylene glycol methyl ether acetate;
the application of the coating composition for enhancing the adhesive force of the transparent polyimide film in preparing the flexible display cover plate comprises the following steps:
step 1: adding polyurethane resin, a thermosetting agent, an adhesion promoter, a wetting agent, a leveling agent, a dye and an ultraviolet absorber into a solvent, and stirring to prepare a coating, wherein the stirring conditions comprise: stirring temperature is 100 ℃, and stirring time is 1 h;
step 2: coating the coating paint on the two side surfaces of the polyimide film, baking to prepare the polyimide film with an additional coating, wherein the polyimide film is a fluorine modified polyimide film, the coating thickness is 50 nm, and the baking conditions comprise: 80. baking at 160deg.C for 5 min, and baking at 160deg.C for 5 min;
step 3: coating a layer of hardening liquid and a layer of printing ink on two sides of the polyimide film with the additional coating respectively to prepare a flexible display cover plate; the flexible display cover plate comprises a polyimide film of a core layer, a coating layer attached to the two side surfaces of the polyimide film, an ink layer and a hardening layer attached to the surface of the coating layer and positioned on the opposite side of the polyimide film. .
Example 8:
in comparison with example 7, the coating thickness in example 8 was 100 nm, and the other conditions were the same as in example 7.
Example 9:
in comparison with example 7, the coating thickness in example 9 was 200 nm, and the other conditions were the same as in example 7.
Example 10:
the coating composition for enhancing the adhesive force of the transparent polyimide film comprises the following raw materials in parts by mass: 20 parts of polyurethane resin, 1 part of adhesion promoter, 2 parts of thermosetting agent, 0.3 part of wetting agent, 0.1 part of leveling agent, 0.1 part of dye, 0.2 part of ultraviolet absorber and 100 parts of solvent; the polyurethane resin is a Shenghao RL9100 polyurethane, and the molecular weight of the polyurethane resin is 50000-100000 g/mol; the adhesion promoter is epoxy resin E-44 (6101), the molecular weight of the adhesion promoter is less than or equal to 800 g/mol, and the epoxy value is more than 0.41; the heat curing agent is isocyanate curing agent HF-1990, the wetting agent is polyether modified polyorganosiloxane, the leveling agent is polyether modified polydimethylsiloxane, the dye is phthalocyanine dye BGS, the ultraviolet absorber is Basoff UV327, and the solvent is prepared from the following components in parts by weight: 1 dimethylacetamide and propylene glycol methyl ether acetate;
the application of the coating composition for enhancing the adhesive force of the transparent polyimide film in preparing the flexible display cover plate comprises the following steps:
step 1: adding polyurethane resin, a thermosetting agent, an adhesion promoter, a wetting agent, a leveling agent, a dye and an ultraviolet absorber into a solvent, and stirring to prepare a coating, wherein the stirring conditions comprise: stirring temperature is 100 ℃, and stirring time is 1 h;
step 2: coating the coating paint on the two side surfaces of the polyimide film, baking to prepare the polyimide film with an additional coating, wherein the polyimide film is a fluorine modified polyimide film, the coating thickness is 100 nm, and the baking conditions comprise: 80. baking at 160deg.C for 5 min, and baking at 160deg.C for 5 min;
step 3: coating a layer of hardening liquid and a layer of printing ink on two sides of the polyimide film with the additional coating respectively to prepare a flexible display cover plate; the flexible display cover plate comprises a polyimide film of a core layer, a coating layer attached to the two side surfaces of the polyimide film, an ink layer and a hardening layer attached to the surface of the coating layer and positioned on the opposite side of the polyimide film.
Example 11:
in example 11, the adhesion promoter was 1.5 parts by mass as compared with example 10, except that the other conditions were the same as in example 10.
Example 12:
in example 12, the adhesion promoter was 2 parts by mass as compared with example 10, and the other conditions were the same as in example 10.
Comparative example 1:
in comparison with example 1, the coating composition for enhancing the adhesion of the transparent polyimide film was not used in comparative example 1, and the other conditions were the same as in example 1.
Comparative example 2:
in comparative example 2, the polyurethane was 5 parts by mass as compared with example 1, and the other conditions were the same as in example 1.
Comparative example 3:
the polyurethane of comparative example 3 was 40 parts by mass compared with example 1, and the other conditions were the same as in example 1.
Comparative example 4:
compared to example 1, the solvent mass ratio 1 in comparative example 4:1 dimethylacetamide and propylene glycol methyl ether acetate, the other conditions were the same as in example 1.
Comparative example 5:
compared to example 1, the solvent mass ratio 1 in comparative example 5: 0, and propylene glycol methyl ether acetate, the other conditions were the same as in example 1.
Comparative example 6:
in comparative example 6, the coating thickness was 30nm as compared with example 1, and the other conditions were the same as in example 1.
Comparative example 7:
in comparative example 7, the coating thickness was 300nm as compared with example 1, and the other conditions were the same as in example 1.
Comparative example 8:
in comparison with example 1, no adhesion promoter was added in comparative example 8, and the other conditions were the same as in example 1.
Comparative example 9:
in comparative example 9, the adhesion promoter was 3 parts by mass as compared with example 1, and the other conditions were the same as in example 1.
Test case
The flexible display cover sheets prepared in examples 1 to 12 and comparative examples 1 to 9 were tested for performance, and test items include: optical properties, adhesion and aging resistance;
the optical performance testing method comprises the following steps: the optical performance is detected by using a light splitting tester, the test object is a polyimide film with an additional coating, and the test indexes comprise: transmittance (y), color difference value (b), yellow Index (YI), and haze;
the adhesive force testing method comprises the following steps: hundred knife test, 3M610 tape;
the aging performance testing method comprises the following steps: setting 8 ageing cycles, each cycle for 12 hours, wherein the ageing cycle conditions comprise: 8h ultraviolet light irradiation (UV-A, 340 nm, 0.63W/m) 2 Moisture exposure at 80 ℃ and 4 h;
table 1 coating composition component ratios and coating thicknesses of examples 1 to 12 and comparative examples 1 to 9
Table 2 flexible display cover sheet performance test results for examples 1 to 12 and comparative examples 1 to 9
As shown in tables 1 and 2, the optical properties of examples 1 to 12 of the present invention satisfy the application requirements and the adhesion of the polyimide film to the cured layer and the ink layer is high, and furthermore, the adhesion of the polyimide film after the aging treatment of the flexible cover sheets of examples 1 to 12 is not significantly changed and the aging resistance is significantly improved.
From the results of example 1 and comparative example 1, it can be seen that the coating composition of the present invention is not used in comparative example 1, the adhesion of comparative example 1 is significantly lower than that of example 1, and the color difference value and yellow index of comparative example 1 are significantly higher than those of example 1, and from the above results, the coating composition provided by the present invention can significantly improve the adhesion of polyimide film, and at the same time, can also significantly reduce the color difference value and yellow index of flexible display cover plate, and improve the optical properties of flexible display cover plate.
As can be seen from the results of example 1, comparative example 2 and comparative example 3, the use proportion of the raw materials of the polyurethane has a large influence on the adhesion of the polyimide film and the haze of the flexible display cover plate, if the proportion of the raw materials of the polyurethane is too small, the adhesion promotion effect of the polyimide film is not obvious, and if the proportion of the raw materials of the polyurethane resin is too large, the haze of the flexible display cover plate is obviously improved, and the application requirements cannot be met.
As can be seen from the results of example 1, comparative example 4 and comparative example 5, the ratio of dimethylacetamide and propylene glycol methyl ether acetate in the solvent has a great influence on the adhesion of the polyimide film and the haze of the flexible display cover plate, and if the ratio of dimethylacetamide is too small, the adhesion improvement effect of the polyimide film is not remarkable, and if the ratio of dimethylacetamide is too large, the haze of the flexible display cover plate is remarkably improved, so that the application requirements cannot be met.
As can be seen from the results of example 1, comparative example 6 and comparative example 7, the coating thickness of the coating composition has a large influence on the adhesion of the polyimide film and the haze of the flexible display cover plate, and if the coating thickness is too small, the adhesion promotion effect of the polyimide film is not remarkable, and if the coating thickness is too small, the haze of the flexible display cover plate is remarkably improved, and the application requirements cannot be met.
From the results of example 1 and comparative example 8, it can be seen that the adhesion of the polyimide film is significantly lower than that of example 1 when no adhesion promoter is added to the coating composition of comparative example 8, and from the above results, it can be seen that the adhesion promoter has an extremely significant promoting effect on the coating composition provided by the present invention; in addition, as can be seen from the results of example 1 and comparative example 9, the adhesion promoter was not significantly improved in the accelerating effect on the coating composition after the use amount was excessively large, which means that the adhesion promoter was used in a certain proportion range to have a high accelerating effect, and in addition, the excessive addition of the adhesion promoter resulted in the improvement of the stiffness of the whole film, which affects the use of the polyimide film.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent transformation of the above embodiment according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. The coating composition for enhancing the adhesive force of the transparent polyimide film is characterized by comprising the following raw materials in parts by mass: 10-30 parts of polyurethane resin, 1-2 parts of adhesion promoter, 1-2 parts of thermosetting agent and the balance of auxiliary agent; the polyurethane resin is hydroxyl-terminated polyurethane; the adhesion promoter is bisphenol A type epoxy resin; the thermosetting agent is isocyanate curing agent.
2. The coating composition for enhancing adhesion of a transparent polyimide film according to claim 1, wherein the adhesion promoter has a molecular weight of 800 g/mol or less and an epoxy value of > 0.41, and the polyurethane resin has a molecular weight of 50000-100000 g/mol.
3. The coating composition for enhancing the adhesion of a transparent polyimide film according to claim 1, wherein the auxiliary agent comprises, in parts by mass: 0.2-0.3 part of wetting agent, 0.05-0.1 part of leveling agent, 0.05-0.1 part of dye, 0.1-0.2 part of ultraviolet absorber and 90-110 parts of solvent.
4. A coating composition for enhancing adhesion of a transparent polyimide film as recited in claim 3, wherein said wetting agent is a polyether modified polyorganosiloxane.
5. A coating composition for enhancing adhesion of a transparent polyimide film as recited in claim 3, wherein said leveling agent is a polyether modified polydimethylsiloxane.
6. A coating composition for enhancing adhesion of a transparent polyimide film according to claim 3, wherein said dye comprises one of phthalocyanine-based dye, azo-based dye and indigo-based dye.
7. The coating composition for enhancing an adhesion of a transparent polyimide film according to claim 3, wherein the ultraviolet absorber comprises one or more of a benzophenone-based ultraviolet absorber, a benzotriazole-based ultraviolet absorber and a triazine-based ultraviolet absorber.
8. The coating composition for enhancing the adhesion of a transparent polyimide film according to claim 3, wherein the solvent comprises the following components in parts by weight: 1 dimethylacetamide and propylene glycol methyl ether acetate.
9. Use of the coating composition for enhancing adhesion of transparent polyimide film according to any one of claims 1 to 8 for the preparation of flexible display cover sheets, comprising the steps of:
step 1: adding polyurethane resin, a thermosetting agent, an adhesion promoter, a wetting agent, a leveling agent, a dye and an ultraviolet absorber into a solvent, and stirring to prepare a coating, wherein the stirring conditions comprise: stirring at 100-110 ℃ for 1-1.2 h;
step 2: coating the coating paint on the two side surfaces of the polyimide film, baking to prepare the polyimide film with an additional coating, wherein the coating thickness is 50-200 nm, and the baking conditions comprise: the temperature is 80-160 ℃ and the time is 5-10 min;
step 3: and coating a layer of hardening liquid and a layer of printing ink on two sides of the polyimide film with the additional coating respectively to prepare the flexible display cover plate.
10. The use according to claim 9, wherein the flexible display cover comprises a polyimide film of the core layer, a coating layer attached to both side surfaces of the polyimide film, and an ink layer and a hardened layer attached to the surface of the coating layer and located on opposite sides of the polyimide film.
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