CN116535966A - Rapidly-cured UV (ultraviolet) coating and preparation method thereof - Google Patents
Rapidly-cured UV (ultraviolet) coating and preparation method thereof Download PDFInfo
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- CN116535966A CN116535966A CN202310155028.1A CN202310155028A CN116535966A CN 116535966 A CN116535966 A CN 116535966A CN 202310155028 A CN202310155028 A CN 202310155028A CN 116535966 A CN116535966 A CN 116535966A
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- 238000000576 coating method Methods 0.000 title claims abstract description 111
- 239000011248 coating agent Substances 0.000 title claims abstract description 110
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 37
- 239000011347 resin Substances 0.000 claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 34
- 239000003960 organic solvent Substances 0.000 claims abstract description 27
- 239000003999 initiator Substances 0.000 claims abstract description 25
- 239000003085 diluting agent Substances 0.000 claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 11
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003848 UV Light-Curing Methods 0.000 claims abstract description 11
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 11
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- SLERPCVQDVNSAK-UHFFFAOYSA-N silver;ethyne Chemical compound [Ag+].[C-]#C SLERPCVQDVNSAK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 7
- OAZPGUICIFMRKI-UHFFFAOYSA-N 2-methylpropanedithioic acid Chemical compound CC(C)C(S)=S OAZPGUICIFMRKI-UHFFFAOYSA-N 0.000 claims abstract description 5
- FWGUGVZBOVCIPE-UHFFFAOYSA-N CC(C)CCCCC[Sn] Chemical compound CC(C)CCCCC[Sn] FWGUGVZBOVCIPE-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 9
- -1 isooctyl Chemical group 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 5
- VHEBAAOCLXOHJH-UHFFFAOYSA-J 2,2-bis(sulfanyl)acetate tin(4+) Chemical compound SC(C(=O)[O-])S.[Sn+4].SC(C(=O)[O-])S.SC(C(=O)[O-])S.SC(C(=O)[O-])S VHEBAAOCLXOHJH-UHFFFAOYSA-J 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- VOBUAPTXJKMNCT-UHFFFAOYSA-N 1-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound CCCCCC(OC(=O)C=C)OC(=O)C=C VOBUAPTXJKMNCT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 3
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 229920003180 amino resin Polymers 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- ITQUAQVSNXBITF-UHFFFAOYSA-N [C-]#[C-].[Ag+3].[N+](=O)([O-])[O-] Chemical compound [C-]#[C-].[Ag+3].[N+](=O)([O-])[O-] ITQUAQVSNXBITF-UHFFFAOYSA-N 0.000 claims 1
- 238000001723 curing Methods 0.000 abstract description 36
- 239000010410 layer Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 239000002344 surface layer Substances 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 5
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 238000005457 optimization Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 22
- 239000011241 protective layer Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 10
- 239000012752 auxiliary agent Substances 0.000 description 10
- 239000013530 defoamer Substances 0.000 description 6
- KKRZIRFDQPFVSE-UHFFFAOYSA-N diphenylmethanone 1H-imidazole Chemical compound C1(=CC=CC=C1)C(=O)C1=CC=CC=C1.N1C=NC=C1 KKRZIRFDQPFVSE-UHFFFAOYSA-N 0.000 description 6
- 238000001029 thermal curing Methods 0.000 description 6
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 5
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 239000002042 Silver nanowire Substances 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 229920003270 Cymel® Polymers 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 4
- NNZXHVCWBDQXLQ-UHFFFAOYSA-N silver acetylene nitrate Chemical compound [N+](=O)([O-])[O-].[Ag+].C#C NNZXHVCWBDQXLQ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000009477 glass transition Effects 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- HDGLPTVARHLGMV-UHFFFAOYSA-N 2-amino-4-(1,1,1,3,3,3-hexafluoropropan-2-yl)phenol Chemical compound NC1=CC(C(C(F)(F)F)C(F)(F)F)=CC=C1O HDGLPTVARHLGMV-UHFFFAOYSA-N 0.000 description 1
- NVKGJHAQGWCWDI-UHFFFAOYSA-N 4-[4-amino-2-(trifluoromethyl)phenyl]-3-(trifluoromethyl)aniline Chemical compound FC(F)(F)C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F NVKGJHAQGWCWDI-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 1
- 238000003811 acetone extraction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical group C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
Abstract
The invention provides a fast-curing UV coating and a preparation method thereof; the UV curing coating comprises the following raw materials in percentage by mass: 20-40% of resin, 10-25% of diluent, 1-5% of initiator, 0.005-0.05% of energy-containing compound gel, 30-60% of organic solvent, 0.5-2.5% of flatting agent and 0.05-0.2% of defoaming agent; the energetic compound gel comprises the following components in percentage by mass: 0.2 to 1.0 percent of ethyl cellulose, 0.005 to 0.05 percent of silver ethyne and silver nitrate and 0.002 to 0.2 percent of dimethyl dithio acetic acid isooctyl tin. The UV coating obtained by optimization can be polymerized rapidly, has both surface layer curing and deep curing, and can improve the adhesive force and chemical resistance of the film layer even under the condition of high-speed coating.
Description
Technical Field
The invention belongs to the technical field of coating materials, and particularly relates to a rapidly-cured UV coating and a preparation method thereof.
Background
UV coating refers to a coating that is cured using UV radiation. The UV-curable coating can be applied to ink printing and exposed to UV radiation. Its solid content can be up to 100%, so that it has no volatile component and does not pollute environment. The high solids content also enables its application to very thin films. The UV-curable coating can also be applied to coating glass and plastics, wood, aluminum beverage bottles, and the like.
At present, the production efficiency of slit coating can be improved by improving the coating speed, but when the speed of a coating machine is improved, the UV curing efficiency can not meet the requirement, and the surface layer curing and the depth curing can not be simultaneously achieved, namely, the problem of poor curing depth effect is solved.
RTR (Roll ToRoll), namely a roll-to-roll slit coating technology, is a high-efficiency and high-precision online coating technology, and a coater speed is generally designed to be 1-32m/min. At present, the speed of a coating machine is generally 8-16m/min, the UV power of a UV protective layer is 65-75% when the UV protective layer is cured, and the corresponding UV curing power is increased to 80-90% when the speed of the coating machine is increased to 20-30 m/min. When the UV lamp is maintained at a high power output, negative effects such as coating popping, wrinkling, etc. can occur, while affecting the service life of the UV lamp. And under high machine speed, the surface layer curing and the deep curing cannot be simultaneously achieved, the curing efficiency of the protective layer is also reduced, and the adhesive force and the chemical resistance do not reach the standards.
Thus, a need exists for a fast curing UV coating.
Disclosure of Invention
Based on this, the invention aims to provide a fast-curing UV coating and a preparation method thereof. The UV coating can be polymerized rapidly, has both surface layer curing and deep curing, and ensures that the adhesive force and chemical resistance index meet the requirements while improving the curing efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme.
The UV curing coating comprises the following raw materials in percentage by mass: 20-40% of resin, 10-25% of diluent, 1-5% of initiator, 0.005-0.05% of energy-containing compound gel, 30-60% of organic solvent, 0.5-2.5% of flatting agent and 0.05-0.2% of defoaming agent;
the energetic compound gel comprises the following components in percentage by mass: 0.2 to 1.0 percent of ethyl cellulose, 0.005 to 0.05 percent of silver ethyne and silver nitrate and 0.002 to 0.2 percent of dimethyl dithio acetic acid isooctyl tin.
In some embodiments, the UV-curable coating comprises the following raw materials in mass percent: 25-40% of resin, 10-20% of diluent, 2-4% of initiator, 0.005-0.05% of energy-containing compound gel, 30-50% of organic solvent, 0.5-1.5% of flatting agent and 0.1-0.2% of defoaming agent.
In some embodiments, the energetic compound gel comprises the following components in mass percent: 0.5 to 0.8 percent of ethyl cellulose, 0.008 to 0.03 percent of silver ethyne and silver nitrate and 0.005 to 0.1 percent of dimethyl dithio acetic acid isooctyl tin.
In some embodiments, the solvent of the energetic compound gel is selected from alcoholic solvents; preferably, the solvent is at least one selected from absolute ethanol, isopropanol and n-butanol.
In some embodiments, the energetic compound gel is prepared as follows: preparing ethyl cellulose solution, adding silver acetylene and silver nitrate, then adding isooctyl dimethyl dimercaptoacetate tin, and continuously stirring when the system temperature is not higher than 35 ℃ to obtain the energetic compound gel.
In some embodiments, the silver acetylide and silver nitrate are added 1-3 times; and/or, adding the isooctyl dimethyl dimercaptoacetate tin in 2-4 times.
In some embodiments, the resin is selected from at least one of an amino resin and a urethane acrylic resin; and/or the diluent is at least one selected from alkoxylated hexanediol diacrylate, monoacrylate of methoxy polyethylene glycol, trimethylolpropane formal acrylate and dodecyl acrylate; and/or the initiator is selected from at least one of a photoinitiator and a thermal initiator; and/or the organic solvent is selected from at least one of an alcohol organic solvent, a ketone organic solvent and an ether organic solvent.
Preferably, the resin is selected from at least one of urethane acrylate mixture 73NS, urethane acrylic CN704, urethane acrylic CN966J75NS, urethane acrylic UV65, 2' -bis (trifluoromethyl) - (1, 1' -diphenyl) -4,4' -diamine (TFMB), 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane (6 FAP), cymel 1158.
Preferably, the photoinitiator is selected from at least one of the initiators with trade names 184, 1173, ITX, TPO; the thermal initiator is at least one selected from radical initiators such as imidazole diphenyl ketone, AIBN and the like.
Preferably, the leveling agent is selected from acrylic resin type leveling agents.
Preferably, the defoamer is selected from at least one of polymers and silicone-based defoamers.
In some embodiments, the UV curable coating is applied at a speed of 20 to 30m/min and a UV power on of 50 to 80%.
The invention also provides a preparation method of the UV coating, which comprises the following steps: (1) Introducing N into the container 2 Sequentially adding the resin, the diluent and the organic solvent under the protection of nitrogen, and stirring until the resin, the diluent and the organic solvent are fully dissolved; (2) Dropwise adding the leveling agent, the defoaming agent and the initiator while stirring, and continuously stirring; (3) And adding the energetic compound gel, and continuing stirring to obtain the UV curing coating.
In some embodiments, the temperature at which stirring is continued in step (2) is below 30 ℃.
In some embodiments, the stirring in step (3) is continued at a rotational speed of 200-500 rpm for a period of 30-60 minutes.
The invention provides a UV coating, wherein when the UV coating passes through an ultraviolet curing system at different machine speeds, a photoinitiator is decomposed to generate cations to initiate prepolymer polymerization; on the one hand, the energetic compound is decomposed and detonated under the irradiation of ultraviolet light to generate a large amount of heat, so that the thermal initiator is decomposed to generate free radicals, and polymerization is further initiated. The UV coating does not need external heating to promote and maintain curing, and forms a cycle, so that enough heat is ensured in the polymerization curing process, and the polymerization process is continuously diffused from the surface to the inside until all prepolymers are polymerized. The UV coating does not require the addition of heating equipment (thermal curing) to promote and maintain continuous high machine speed curing, but rather initiates rapid polymerization of the system by the energy generated by the energetic compound "detonation".
The UV coating can be polymerized rapidly, has both surface layer curing and deep curing, and can improve the adhesive force and chemical resistance of a film layer even under the condition of high-speed coating.
Detailed Description
The experimental methods of the present invention, in which specific conditions are not specified in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The various chemicals commonly used in the examples are commercially available.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having" and any variations thereof, are intended to cover a non-exclusive inclusion. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to the elements or modules listed but may alternatively include additional steps not listed or inherent to such process, method, article, or device.
In the present invention, the term "plurality" means two or more. "and/or", describes an association relationship of an association object, and indicates that there may be three relationships, for example, a and/or B, and may indicate: a exists alone, A and B exist together, and B exists alone. The character "/" generally indicates that the context-dependent object is an "or" relationship.
The following description is made with reference to specific embodiments.
Example 1
The present example provides a UV coating, which is prepared by the following method:
s1 preparation of energetic Compound gel
Ethyl cellulose STD-1006g and 1000g absolute ethyl alcohol were sequentially added to a three-necked flask equipped with a thermometer and a magnetic stirrer to prepare an organic solution, followed by adding silver acetylene nitrate (Ag) in a total amount of 0.1g in 2 times 2 C 2 ·AgNO 3 ) The solution gradually changed to orange-yellow viscous during the addition. And adding isooctyl dimethyl dithioglycolate tin with the total amount of 1g for three times, continuously stirring for 0.5h at the reaction temperature of not higher than 35 ℃, and standing for later use.
And S2, pre-calculating and weighing the resin and the auxiliary agent according to the proportion, and sequentially adding the resin and the auxiliary agent into the mixture and stirring the mixture uniformly.
Filling N into clean and dry 1000m L three-mouth bottle 2 Under the protection of nitrogen, 70420 parts of resin CN, 115820 parts of resin Cymel, 20 parts of trimethylolpropane formal acrylate serving as a diluent and 35 parts of organic solvent, wherein the organic solvent is a mixed solvent prepared from isopropanol, methyl isobutyl ketone and propylene glycol methyl ether in a mass ratio of 1:1:1; stirring at 500rpm for 30min, and dissolving thoroughly.
S3, dropwise adding 0.8 part of acrylic leveling agent, 0.2 part of defoamer, 11732 parts of initiator and 2 parts of initiator imidazole benzophenone into the resin solution prepared in the S2 while stirring in sequence; stirring was continued for 30 minutes, and the temperature during stirring was controlled below 30 ℃.
S4: finally, 0.005 part of the energetic compound gel prepared in the step S1 is added, and the stirring speed is controlled at 300rpm for 50 minutes. The UV coating is prepared.
Coating the UV coating on the conductive layer to obtain a protective layer:
1: uniformly coating silver nanowire slurry on the surface of a flexible base film in a slit coating mode, wherein the coating speed is 10-20 m/min, the curing temperature is 70-130 ℃, and a uniform conductive film is formed.
2: and (2) uniformly coating the UV coating on the surface of the flexible conductive film prepared in the step (1) in a slit coating mode, wherein the coating speed is 25m/min, the UV power is opened to 70%, and a uniform protective layer is formed after UV and thermal curing.
Example 2
The present example provides a UV coating, which is prepared by the following method:
s1 preparation of energetic Compound gel
Ethyl cellulose STD-1008g and 1000g absolute ethyl alcohol were sequentially added to a three-neck flask equipped with a thermometer and a magnetic stirrer to prepare an organic solution, and then silver acetylene nitrate (Ag) was added in 2 times in a total amount of 0.15g 2 C 2 ·AgNO 3 ) The solution gradually changed to orange-yellow viscous during the addition. And adding isooctyl dimethyl dithioglycolate tin with the total amount of 1.2g for three times, continuously stirring for 0.5h at the reaction temperature of not higher than 35 ℃, and standing for later use.
And S2, pre-calculating and weighing the resin and the auxiliary agent according to the proportion, and sequentially adding the resin and the auxiliary agent into the mixture and stirring the mixture uniformly.
Filling N into clean and dry 1000m L three-mouth bottle 2 Sequentially adding 15 parts of resin CN966J75NS, 15 parts of resin 6FAP, 20 parts of diluent dodecyl acrylate and 45 parts of organic solvent under the protection of nitrogen for 20min, wherein the organic solvent is a mixed solution prepared from isopropanol, methyl isobutyl ketone and propylene glycol methyl ether in a mass ratio of 1:1:1; stirring at 500rpm for 30min, and dissolving thoroughly.
S3, dropwise adding 0.9 part of acrylic leveling agent, 0.1 part of defoamer, 11731.5 parts of initiator and 1.5 parts of initiator imidazole benzophenone into the resin solution prepared in the S2 while stirring in sequence; stirring was continued for 30 minutes, and the temperature during stirring was controlled below 30 ℃.
S4: finally, 0.025 parts of the energetic compound gel prepared in the step S1 is added, and the stirring speed is controlled to be 300rpm for 50 minutes. The UV coating is prepared.
Coating the UV coating on the conductive layer to obtain a protective layer:
1: uniformly coating silver nanowire slurry on the surface of a flexible base film in a slit coating mode, wherein the coating speed is 10-20 m/min, the curing temperature is 70-130 ℃, and a uniform conductive film is formed.
2: and (2) uniformly coating the UV coating on the surface of the flexible conductive film prepared in the step (1) in a slit coating mode, wherein the coating speed is 25m/min, the UV power is opened to 70%, and a uniform protective layer is formed after UV and thermal curing.
Example 3
The present example provides a UV coating, which is prepared by the following method:
s1 preparation of energetic Compound gel
Ethyl cellulose STD-1007g and 1000g absolute ethyl alcohol were sequentially added to a three-necked flask equipped with a thermometer and a magnetic stirrer to prepare an organic solution, followed by adding silver acetylene nitrate (Ag) in a total amount of 0.12g in 2 times 2 C 2 ·AgNO 3 ) The solution gradually changed to orange-yellow viscous during the addition. And adding isooctyl dimethyl dithioglycolate tin with the total amount of 1.1g for three times, continuously stirring for 0.5h at the reaction temperature of not higher than 35 ℃, and standing for later use.
And S2, pre-calculating and weighing the resin and the auxiliary agent according to the proportion, and sequentially adding the resin and the auxiliary agent into the mixture and stirring the mixture uniformly.
Filling N into clean and dry 1000m L three-mouth bottle 2 Sequentially adding 6517.5 parts of resin UV, 25 parts of resin cymel115817.5 parts of diluent alkoxylated hexanediol diacrylate and 35 parts of organic solvent under the protection of nitrogen for 20min, wherein the organic solvent is a mixed solution prepared from isopropanol, methyl isobutyl ketone and propylene glycol methyl ether in a volume ratio of 1:1:1; stirring at 500rpm for 30min, and dissolving thoroughly.
S3, dropwise adding 0.8 part of acrylic leveling agent, 0.2 part of defoamer, 11732 parts of initiator and 2 parts of initiator imidazole benzophenone into the resin solution prepared in the S2 while stirring in sequence; stirring was continued for 30 minutes, and the temperature during stirring was controlled below 30 ℃.
S4: finally, 0.05 part of the energetic compound gel prepared in the step S1 is added, and the stirring speed is controlled to be 300rpm for 50 minutes. The UV coating is prepared.
Coating the UV coating on the conductive layer to obtain a protective layer:
1: uniformly coating silver nanowire slurry on the surface of a flexible base film in a slit coating mode, wherein the coating speed is 10-20 m/min, the curing temperature is 70-130 ℃, and a uniform conductive film is formed.
2. And (2) uniformly coating the UV coating on the surface of the flexible conductive film prepared in the step (1) in a slit coating mode, wherein the coating speed is 25m/min, the UV power is opened to 70%, and a uniform protective layer is formed after UV and thermal curing.
Comparative example 1
This comparative example provides a UV coating which was prepared in the same manner as example 1 except that the formulation did not include the energetic compound gel, as follows:
and S1, pre-calculating and weighing the resin and the auxiliary agent according to the proportion, and sequentially adding the resin and the auxiliary agent into the mixture and stirring the mixture uniformly.
Filling N into clean and dry 1000m L three-mouth bottle 2 Under the protection of nitrogen, 70420 parts of resin CN, 115820 parts of resin Cymel, 20 parts of trimethylolpropane formal acrylate serving as a diluent and 35 parts of organic solvent, wherein the organic solvent is a mixed solvent prepared from isopropanol, methyl isobutyl ketone and propylene glycol methyl ether in a mass ratio of 1:1:1; stirring at 500rpm for 30min to dissolve thoroughly;
s2, dropwise adding 0.8 part of acrylic leveling agent, 0.2 part of defoamer, 11732 parts of initiator and 2 parts of initiator imidazole benzophenone into the resin solution prepared in the step S1 under stirring; stirring was continued for 30 minutes, and the temperature during stirring was controlled below 30 ℃.
Coating the UV coating on the conductive layer to obtain a protective layer:
1: uniformly coating silver nanowire slurry on the surface of a flexible base film in a slit coating mode, wherein the coating speed is 10-20 m/min, the curing temperature is 70-130 ℃, and a uniform conductive film is formed.
2. And (2) uniformly coating the UV coating on the surface of the flexible conductive film prepared in the step (1) in a slit coating mode, wherein the coating speed is 25m/min, the UV power is opened to 70%, and a uniform protective layer is formed after UV and thermal curing.
Comparative example 2
This comparative example provides a UV coating which is prepared in the same manner as example 1 except that the amount of the energetic compound gel in the formulation is different, as follows:
s1 preparation of energetic Compound gel
Ethyl cellulose STD-1006g and 1000g absolute ethyl alcohol were sequentially added to a three-necked flask equipped with a thermometer and a magnetic stirrer to prepare an organic solution, followed by adding silver acetylene nitrate (Ag) in a total amount of 0.1g in 2 times 2 C 2 ·AgNO 3 ) The solution gradually changed to orange-yellow viscous during the addition. And adding isooctyl dimethyl dithioglycolate tin with the total amount of 1g for three times, continuously stirring for 0.5h at the reaction temperature of not higher than 35 ℃, and standing for later use.
And S2, pre-calculating and weighing the resin and the auxiliary agent according to the proportion, and sequentially adding the resin and the auxiliary agent into the mixture and stirring the mixture uniformly.
Filling N into clean and dry 1000m L three-mouth bottle 2 Under the protection of nitrogen, 70420 parts of resin CN, 115820 parts of resin Cymel, 20 parts of trimethylolpropane formal acrylate serving as a diluent and 35 parts of organic solvent, wherein the organic solvent is a mixed solvent prepared from isopropanol, methyl isobutyl ketone and propylene glycol methyl ether in a volume ratio of 1:1:1; stirring at 500rpm for 30min, and dissolving thoroughly.
S3, dropwise adding 0.8 part of acrylic leveling agent, 0.2 part of defoamer, 11732 parts of initiator and 2 parts of initiator imidazole benzophenone into the resin solution prepared in the S2 while stirring in sequence; stirring was continued for 30 minutes, and the temperature during stirring was controlled below 30 ℃.
S4: finally, 0.1 part of the energetic compound gel prepared in the step S1 is added, and the stirring speed is controlled to be 300rpm for 50 minutes. The UV coating is prepared.
Coating the UV coating on the conductive layer to obtain a protective layer:
1: uniformly coating silver nanowire slurry on the surface of a flexible base film in a slit coating mode, wherein the coating speed is 10-20 m/min, the curing temperature is 70-130 ℃, and a uniform conductive film is formed.
2: and (2) uniformly coating the UV coating on the surface of the flexible conductive film prepared in the step (1) in a slit coating mode, wherein the coating speed is 25m/min, the UV power is opened to 70%, and a uniform protective layer is formed after UV and thermal curing.
The properties of the protective layer-containing conductive films obtained by the preparation of the UV coating materials described in the above examples and comparative examples were examined as follows:
the light transmittance and haze test method of the transparent conductive film comprises the following steps: BYK permeates the haze meter.
Adhesion force: the 3M610 tape was continuously adhered and torn off 3 times with a hundred knives.
Solvent resistance: soaking in ethanol and IPA under different conditions.
Curing efficiency: the curing efficiency was tested by acetone extraction, g=w1/w0×100% of curing efficiency.
(G: curing efficiency; W1: mass before extraction of cured film: G; W0: mass after extraction of cured film: G).
Glass transition temperature: thermo-mechanical analysis TMA.
Tensile strength & elastic modulus & elongation at break: test Standard GB/T1040.3-2006 section 3 determination of Plastic tensile Properties: the method in test conditions for thin plastics and flakes requires detection.
The test results are shown in Table 1 and Table 2:
TABLE 1
TABLE 2
The results in Table 1 show that the protective layers (examples 1-3) obtained by preparing the UV coating of the invention have good transmittance, adhesion and solvent resistance, and lower haze. The addition of an excess of the energetic compound gel to the UV coating of comparative example 2 resulted in reduced adhesion and solvent resistance and increased haze without the addition of the energetic compound gel to the UV coating of comparative example 1. The UV coatings of comparative examples 1 and 2 were shown to have poor curing effect at high coating speeds, and the adhesion and chemical resistance of the film layers were not satisfactory.
As is clear from the results in Table 2, the protective layers (examples 1 to 3) obtained by preparing the UV coating according to the invention have better mechanical properties (tensile strength & elastic modulus & elongation at break) and higher glass transition temperature. Comparative example 1 is a gel without the energetic compound according to the invention, with reduced mechanical properties and glass transition temperature; the gel of comparative example 2, which contains an excessive amount of the energetic compound, has a reduced elongation at break. Compared to example 1, comparative example 1 has significantly lower curing efficiency than example 1 at the same coater speed and distance (oven and UV system length), indicating that comparative example 1 has a lower curing speed than example 1 and requires a longer curing time to achieve the same curing efficiency.
In conclusion, the UV coating obtained by optimization can be polymerized rapidly, has both surface layer curing and deep curing, and can improve the adhesive force and chemical resistance of the film layer even under the condition of high-speed coating.
The technical features of the above embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (9)
1. The UV coating is characterized by comprising the following raw materials in percentage by mass: 20-40% of resin, 10-25% of diluent, 1-5% of initiator, 0.005-0.05% of energy-containing compound gel, 30-60% of organic solvent, 0.5-2.5% of flatting agent and 0.05-0.2% of defoaming agent;
the energetic compound gel comprises the following components in percentage by mass: 0.2 to 1.0 percent of ethyl cellulose, 0.005 to 0.05 percent of silver ethyne and silver nitrate and 0.002 to 0.2 percent of dimethyl dithio acetic acid isooctyl tin.
2. The UV-coating according to claim 1, wherein the UV-curable coating comprises the following raw materials in mass percent: 25-40% of resin, 10-20% of diluent, 2-4% of initiator, 0.005-0.05% of energy-containing compound gel, 30-50% of organic solvent, 0.5-1.5% of flatting agent and 0.1-0.2% of defoaming agent.
3. The UV coating of claim 1, wherein the energetic compound gel comprises the following components in mass percent: 0.5 to 0.8 percent of ethyl cellulose, 0.008 to 0.03 percent of silver ethyne and silver nitrate and 0.005 to 0.1 percent of dimethyl dithio acetic acid isooctyl tin.
4. The UV coating of claim 1, wherein the solvent of the energetic compound gel is selected from the group consisting of alcoholic solvents; preferably, the solvent is at least one selected from absolute ethanol, isopropanol and n-butanol.
5. The UV coating of claim 1, wherein the energetic compound gel is prepared by the following method: preparing ethyl cellulose solution, adding silver acetylene and silver nitrate, then adding isooctyl dimethyl dimercaptoacetate tin, and continuously stirring when the system temperature is not higher than 35 ℃ to obtain the energetic compound gel.
6. The UV coating according to claim 5, wherein the silver acetylide nitrate is added 1-3 times; and/or, adding the isooctyl dimethyl dimercaptoacetate tin in 2-4 times.
7. The UV coating of claim 1, wherein the resin is selected from at least one of an amino resin and a urethane acrylic resin; and/or the diluent is at least one selected from alkoxylated hexanediol diacrylate, monoacrylate of methoxy polyethylene glycol, trimethylolpropane formal acrylate and dodecyl acrylate; and/or the initiator is selected from at least one of a photoinitiator and a thermal initiator; and/or the organic solvent is selected from at least one of an alcohol organic solvent, a ketone organic solvent and an ether organic solvent.
8. The UV coating according to claim 1, wherein the UV curable coating has a coating speed of 20 to 30m/min and a UV power on of 50 to 80%.
9. The method of preparing a UV-coating according to any one of claims 1 to 8, wherein the method comprises the steps of: (1) Introducing N into the container 2 Sequentially adding the resin, the diluent and the organic solvent under the protection of nitrogen, and stirring until the resin, the diluent and the organic solvent are fully dissolved; (2) Dropwise adding the leveling agent, the defoaming agent and the initiator while stirring, and continuously stirring; (3) And adding the energetic compound gel, and continuing stirring to obtain the UV curing coating.
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