CN111635666A - LED-UV (light-emitting diode-ultraviolet) cured environment-friendly high-temperature sintering varnish and preparation method thereof - Google Patents
LED-UV (light-emitting diode-ultraviolet) cured environment-friendly high-temperature sintering varnish and preparation method thereof Download PDFInfo
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- CN111635666A CN111635666A CN202010566141.5A CN202010566141A CN111635666A CN 111635666 A CN111635666 A CN 111635666A CN 202010566141 A CN202010566141 A CN 202010566141A CN 111635666 A CN111635666 A CN 111635666A
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- 239000002966 varnish Substances 0.000 title claims abstract description 76
- 238000005245 sintering Methods 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims description 21
- 229920000180 alkyd Polymers 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 23
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 23
- 239000003085 diluting agent Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 15
- 229920002635 polyurethane Polymers 0.000 claims abstract description 11
- 239000004814 polyurethane Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims description 132
- 239000000203 mixture Substances 0.000 claims description 87
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 38
- 239000002518 antifoaming agent Substances 0.000 claims description 29
- 239000002270 dispersing agent Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 26
- 239000013008 thixotropic agent Substances 0.000 claims description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 19
- 239000003921 oil Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 9
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- YMCOIFVFCYKISC-UHFFFAOYSA-N ethoxy-[2-(2,4,6-trimethylbenzoyl)phenyl]phosphinic acid Chemical compound CCOP(O)(=O)c1ccccc1C(=O)c1c(C)cc(C)cc1C YMCOIFVFCYKISC-UHFFFAOYSA-N 0.000 claims description 4
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 3
- KTALPKYXQZGAEG-UHFFFAOYSA-N 2-propan-2-ylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(C(C)C)=CC=C3SC2=C1 KTALPKYXQZGAEG-UHFFFAOYSA-N 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000007639 printing Methods 0.000 abstract description 27
- 238000001723 curing Methods 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000010023 transfer printing Methods 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000004880 explosion Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 238000002309 gasification Methods 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000003848 UV Light-Curing Methods 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 55
- 230000000052 comparative effect Effects 0.000 description 19
- 238000000034 method Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 11
- 230000001070 adhesive effect Effects 0.000 description 10
- 239000000853 adhesive Substances 0.000 description 8
- 239000001023 inorganic pigment Substances 0.000 description 6
- 238000007650 screen-printing Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009974 thixotropic effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000003849 aromatic solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002688 maleic acid derivatives Chemical class 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/104—Polyesters
- C09D11/105—Alkyd resins
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses an LED-UV cured environment-friendly high-temperature sintering varnish, which comprises the following raw material components in parts by mass: 25-60 parts of pure acrylic resin, 20-50 parts of polyurethane acrylic resin, 20-70 parts of reactive monomer diluent, 5-8 parts of photoinitiator and 3-8 parts of special alkyd resin. The environment-friendly high-temperature sintering varnish for LED-UV curing has good curing flexibility, good adhesiveness on the surface of a product, good bonding property, rapid decomposition and gasification, no ash content, rapid drying, no need of heating and drying, no phenomena of shrinkage deformation, explosion and the like of a coating film, clear pattern and effective improvement on the printing effect of water transfer printing.
Description
Technical Field
The invention relates to the technical field of printing ink, in particular to LED-UV (light-emitting diode-ultraviolet) cured environment-friendly high-temperature sintering ink mixing oil and a preparation method thereof.
Background
The varnish is a binder for printing ink on substrates such as glass, ceramics and the like. The printing ink is mainly prepared by dispersing and grinding ceramic pigment and ink mixing oil, and when the water transfer printing process is carried out, the prepared printing ink is printed on water transfer printing paper, then the printing ink is transferred onto substrates such as glass, ceramics and the like, and finally, bright patterns are obtained through high-temperature sintering. The traditional varnish is mainly composed of thermoplastic acrylic resin and aromatic solvent, so that the solid content of the ink prepared from the varnish is low, the curing time is long, the printing efficiency is influenced, the printing performance is poor, the printed pattern is unclear, the cohesiveness and the adhesive force are poor, and the solvent is toxic, so that the solvent is easy to volatilize, pollute the environment and influence the health of people.
Disclosure of Invention
Aiming at the problems brought forward by the background technology, the invention aims to provide the LED-UV cured environment-friendly high-temperature sintering varnish, which has the advantages of good curing flexibility, good adhesion on the surface of a product, good bonding property, rapid decomposition and gasification, no ash content, rapid drying, no need of heating and drying, no phenomena of shrinkage deformation, explosion and the like of a coating film, clear pattern and effective improvement on the printing effect of water transfer printing.
The invention also aims to provide a preparation method of the LED-UV cured environment-friendly high-temperature sintering varnish, which is simple, and the prepared LED-UV cured environment-friendly high-temperature sintering varnish does not contain volatile organic solvents, can be rapidly cured, and has good curing flexibility, good adhesive property and good adhesiveness on the surface of a product.
In order to achieve the purpose, the invention adopts the following technical scheme:
the environment-friendly high-temperature sintering varnish capable of being cured by LED-UV comprises the following raw material components in parts by mass:
preferably, the special alkyd resin is a long-oil air-drying alkyd resin.
Preferably, the reactive monomer diluent comprises a mixture of two or more of 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate and trimethylolpropane triacrylate.
Preferably, the photoinitiator comprises three or more of monoacylphosphine, diacyl phosphine, ethyl 2,4, 6-trimethylbenzoylphenylphosphonate and 2-isopropylthioxanthone.
Preferably, the raw material components further comprise the following components in parts by mass:
0.2-1 part of a defoaming agent;
the defoaming agent is an organic silicon defoaming agent or a fluorine modified organic silicon defoaming agent.
Preferably, the raw material components further comprise the following components in parts by mass:
0.5-2 parts of a dispersing agent;
the dispersant is a polycarboxylic acid polymer dispersant or a polyacrylate dispersant.
Preferably, the raw material components further comprise the following components in parts by mass:
1-3 parts of a thixotropic agent;
the thixotropic agent is a polyamide thixotropic agent.
Preferably, the raw material components further comprise the following components in parts by mass:
0.1-2 parts of nano calcium carbonate
0.1-2 parts of nano aluminum oxide.
Preferably, the particle size of the nano calcium carbonate is 10-50 nm, and the particle size of the nano alumina is 10-50 nm.
The preparation method of the LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) stirring pure acrylic resin at a high speed, and then adding polyurethane acrylic resin, wherein the stirring speed is 1000-1200 r/min, and the stirring time is 40-50 min, so as to obtain a mixture A;
(2) mixing the defoaming agent and the dispersing agent at the mixing speed of 1200-1500 r/min and the mixing temperature of 50-55 ℃ for 40-50 min to obtain a mixture B;
(3) mixing an active monomer diluent and a photoinitiator at the mixing speed of 1000-1200 r/min and the mixing temperature of 50-55 ℃ for 30-40 min to obtain a mixture C;
(4) sequentially adding the mixture B, the thixotropic agent, the nano calcium carbonate and the nano aluminum oxide into the mixture A, wherein the mixing speed is 1200-1500 r/min, the mixing temperature is 45-50 ℃, and the mixing time is 50-70 min, so as to obtain a mixture D;
(5) adding the mixture C into the mixture D, wherein the mixing speed is 1200-1500 r/min, the mixing temperature is 45-50 ℃, and the mixing time is 15-25 min, so as to obtain a mixture E;
(6) adding the special alkyd resin into the mixture E, wherein the mixing speed is 500-800 r/min, the mixing temperature is 40-45 ℃, the mixing time is 15-25 min, standing for 7-9 h under a closed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
Compared with the prior art, the invention has the following beneficial effects:
by adding the special alkyd resin, the printing ink prepared by using the LED-UV cured environment-friendly high-temperature sintering varnish can be rapidly cured at a low temperature, has little smell and does not block the screen, and has little environmental pollution because of no volatile organic solvent. The environment-friendly high-temperature sintering varnish for curing the LED-UV is added, so that a cured film obtained after curing the prepared ink has good flexibility and curing flexibility, organic components in the ink cured film can be rapidly decomposed and gasified in the firing process at high temperature (500-900 ℃), ash content is not left, the ink cured film can be rapidly dried, heating and drying are not needed, the phenomena of shrinkage and deformation of a coating film, explosion and the like are avoided, the pattern is clear, the adhesiveness of the surface of a product is good, the bonding performance is good, large-area and multicolor overprinting can be realized, the printing effect of water transfer printing is effectively improved, and the production efficiency is greatly improved.
Detailed Description
The environment-friendly high-temperature sintering varnish capable of being cured by LED-UV comprises the following raw material components in parts by mass:
by adding the special alkyd resin, the printing ink prepared by using the LED-UV cured environment-friendly high-temperature sintering varnish can be rapidly cured at a low temperature, has little smell and no net blockage, and has little environmental pollution because of no volatile organic solvent. The environment-friendly high-temperature sintering varnish for curing the LED-UV is added, so that a cured film obtained after curing the prepared ink has good flexibility and curing flexibility, organic components in the ink cured film can be rapidly decomposed and gasified in the firing process at high temperature (500-900 ℃), ash content is not left, the ink cured film can be rapidly dried, heating and drying are not needed, the phenomena of shrinkage and deformation of a coating film, explosion and the like are avoided, the pattern is clear, the adhesiveness of the surface of a product is good, the bonding performance is good, large-area and multicolor overprinting can be realized, the printing effect of water transfer printing is effectively improved, and the production efficiency is greatly improved.
Preferably, the special alkyd resin is a long-oil air-drying alkyd resin.
The special alkyd resin is long-oil-degree air-drying alkyd resin, the long-oil-degree air-drying alkyd resin is used, in the process of screen printing of the ink prepared by using the LED-UV-cured environment-friendly high-temperature sintering varnish, the ink is easy to scrape off from a screen printing plate, the phenomenon of screen printing plate sticking is eliminated, the drying time of the ink is short, self-drying can be realized, in the subsequent sintering process, the phenomenon of violent burning or shrinkage is avoided, an ink curing film can be flatly stuck to the surface of a product and is slowly decomposed and burnt, and the adhesion performance is good.
Preferably, the reactive monomer diluent comprises a mixture of two or more of 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate and trimethylolpropane triacrylate.
Through adding the reactive monomer diluent, the viscosity of a system can be reduced, the use of a common solvent is avoided, the use of the solvent is easy to volatilize and solidify in the process of solidifying the printing ink prepared from the LED-UV solidified environment-friendly high-temperature sintering ink-adjusting oil, and the environmental pollution is caused.
Preferably, the photoinitiator comprises three or more of monoacylphosphine, diacyl phosphine, ethyl 2,4, 6-trimethylbenzoylphenylphosphonate and 2-isopropylthioxanthone.
By adding the photoinitiator, the ink prepared by using the LED-UV cured environment-friendly high-temperature sintering ink mixing oil is subjected to photocuring reaction after absorbing the irradiation of an LED-UV light source, and the cured ink is bright and bright in color, good in adhesive force and high in definition.
Preferably, the raw material components further comprise the following components in parts by mass:
0.2-1 part of a defoaming agent;
the defoaming agent is an organic silicon defoaming agent or a fluorine modified organic silicon defoaming agent.
By adding the defoaming agent, the condition that a large amount of bubbles are generated by mixing raw materials in the mixing preparation process of the LED-UV cured environment-friendly high-temperature sintering ink mixing oil to influence the mixing uniformity is avoided, and the defoaming agent can eliminate the bubbles generated in the screen printing process of ink prepared by using the LED-UV cured environment-friendly high-temperature sintering ink mixing oil, so that the printing definition and the printing effect are effectively improved.
Preferably, the raw material components further comprise the following components in parts by mass:
0.5-2 parts of a dispersing agent;
the dispersant is a polycarboxylic acid polymer dispersant or a polyacrylate dispersant.
By adding the dispersing agent, the dispersion uniformity of the raw materials of the LED-UV cured environment-friendly high-temperature sintering varnish during the mixing preparation process can be improved, the using effect of the LED-UV cured environment-friendly high-temperature sintering varnish can be improved, and after the inorganic pigment is mixed with the LED-UV cured environment-friendly high-temperature sintering varnish, the inorganic pigment can be more uniformly distributed in the varnish, so that the printing effect is effectively improved.
Preferably, the raw material components further comprise the following components in parts by mass:
1-3 parts of a thixotropic agent;
the thixotropic agent is a polyamide thixotropic agent.
By adding the thixotropic agent, the LED-UV cured environment-friendly high-temperature sintering ink mixing oil can obtain excellent thixotropic property, the fluidity of the LED-UV cured environment-friendly high-temperature sintering ink mixing oil can be adjusted, the thickening effect is achieved, the anti-settling and anti-sagging properties of the LED-UV cured environment-friendly high-temperature sintering ink mixing oil are endowed, and the adhesion of a cured film obtained after the prepared ink is cured on the surface of a product is good.
Preferably, the raw material components further comprise the following components in parts by mass:
0.1-2 parts of nano calcium carbonate
0.1-2 parts of nano aluminum oxide.
By adding the nano calcium carbonate and the nano aluminum oxide, the bonding property of the LED-UV cured environment-friendly high-temperature sintering varnish and the inorganic pigment can be improved, and the strength of the LED-UV cured environment-friendly high-temperature sintering varnish is improved, so that the flexibility of a curing film of the ink and the adhesive force on the surface of a product are improved.
Preferably, the particle size of the nano calcium carbonate is 10-50 nm, and the particle size of the nano alumina is 10-50 nm.
The particle size of the nano calcium carbonate is 10-50 nm, the particle size of the nano aluminum oxide is 10-50 nm, and due to the small particle size and the large specific surface area, the nano calcium carbonate and the nano aluminum oxide are added into the LED-UV cured environment-friendly high-temperature sintering varnish, so that the strength of the LED-UV cured environment-friendly high-temperature sintering varnish can be better improved, and the flexibility of an ink curing film and the adhesive force on the surface of a product are better.
The preparation method of the LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) stirring pure acrylic resin at a high speed, and then adding polyurethane acrylic resin, wherein the stirring speed is 1000-1200 r/min, and the stirring time is 40-50 min, so as to obtain a mixture A;
(2) mixing the defoaming agent and the dispersing agent at the mixing speed of 1200-1500 r/min and the mixing temperature of 50-55 ℃ for 40-50 min to obtain a mixture B;
(3) mixing an active monomer diluent and a photoinitiator at the mixing speed of 1000-1200 r/min and the mixing temperature of 50-55 ℃ for 30-40 min to obtain a mixture C;
(4) sequentially adding the mixture B, the thixotropic agent, the nano calcium carbonate and the nano aluminum oxide into the mixture A, wherein the mixing speed is 1200-1500 r/min, the mixing temperature is 45-50 ℃, and the mixing time is 50-70 min, so as to obtain a mixture D;
(5) adding the mixture C into the mixture D, wherein the mixing speed is 1200-1500 r/min, the mixing temperature is 45-50 ℃, and the mixing time is 15-25 min, so as to obtain a mixture E;
(6) adding the special alkyd resin into the mixture E, wherein the mixing speed is 500-800 r/min, the mixing temperature is 40-45 ℃, the mixing time is 15-25 min, standing for 7-9 h under a closed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
The LED-UV cured environment-friendly high-temperature sintering varnish prepared by the preparation method is simple in preparation method, does not contain volatile organic solvent, can be rapidly cured, and has good curing flexibility, good adhesive property and good adhesiveness on the surface of a product;
the special alkyd resin is added at the later stage, so that the special alkyd resin and the thixotropic agent are prevented from generating a crosslinking reaction, and the bonding property of the LED-UV cured environment-friendly high-temperature sintering varnish is reduced;
if the mixing speed and the mixing temperature in the step (2) are too low, the defoaming agent and the dispersing agent are not easily dispersed, and if the mixing speed and the mixing temperature in the step (2) are too high, the defoaming agent is easily caused to fail;
if the mixing speed and the mixing temperature in the step (4) are too high, the LED-UV cured environment-friendly high-temperature sintering varnish cannot obtain thixotropic property, so that the adhesion of a cured film obtained after the prepared varnish is cured on the surface of a product is poor.
The technical solution of the present invention is further explained by the following embodiments.
The following examples and comparative examples used the starting materials:
the pure acrylic resin and the polyurethane acrylic resin are conventional raw materials sold in the market;
reactive monomer diluent: a mixture of 1, 6-hexanediol diacrylate and dipropylene glycol diacrylate;
photoinitiator (2): a mixture of monoacylphosphine, diacylphosphine, and ethyl 2,4, 6-trimethylbenzoylphenylphosphonate;
special alkyd resin: long oil air-drying alkyd resin with model number 389-9;
defoaming agent: commercially available silicone defoamers;
dispersing agent: commercially available polyacrylate dispersants;
thixotropic agent: commercially available polyamide thixotropic agents;
nano calcium carbonate, nano alumina: the particle size of the commercially available nano calcium carbonate and nano aluminum oxide is 30nm respectively.
Example 1
A preparation method of LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) according to the mass parts, 50 parts of pure acrylic resin is stirred at a high speed, and then 30 parts of polyurethane acrylic resin is added, wherein the stirring speed is 1000r/min, and the stirring time is 30min, so that a mixture A is obtained;
(2) mixing 30 parts of reactive monomer diluent and 5 parts of photoinitiator at the mixing speed of 1000r/min and the mixing temperature of 50 ℃ for 35min to obtain a mixture B;
(3) and adding 5 parts of special alkyd resin into the mixture B, mixing at the speed of 600r/min and the temperature of 45 ℃ for 20min, standing for 8h under a sealed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
Example 2
A preparation method of LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) according to the mass parts, stirring 40 parts of pure acrylic resin at a high speed, then adding 30 parts of polyurethane acrylic resin, wherein the stirring speed is 1200r/min, and the stirring time is 40min, so as to obtain a mixture A;
(2) mixing 60 parts of reactive monomer diluent and 8 parts of photoinitiator at the mixing speed of 1100r/min and the mixing temperature of 55 ℃ for 30min to obtain a mixture B;
(3) adding 0.5 part of defoaming agent into the mixture A, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 55min to obtain a mixture C;
(4) adding the mixture B into the mixture C, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 15min, so as to obtain a mixture D;
(5) and adding 8 parts of special alkyd resin into the mixture D, mixing at the speed of 600r/min and the temperature of 40 ℃ for 20min, standing for 7h under a sealed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
Example 3
A preparation method of LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) according to the mass parts, stirring 40 parts of pure acrylic resin at a high speed, then adding 30 parts of polyurethane acrylic resin, wherein the stirring speed is 1200r/min, and the stirring time is 40min, so as to obtain a mixture A;
(2) mixing 1 part of defoaming agent and 1 part of dispersing agent at the mixing speed of 1300r/min, the mixing temperature of 50 ℃ and the mixing time of 40min to obtain a mixture B;
(3) mixing 60 parts of reactive monomer diluent and 8 parts of photoinitiator at the mixing speed of 1100r/min and the mixing temperature of 55 ℃ for 30min to obtain a mixture C;
(4) adding the mixture B into the mixture A, and mixing at the speed of 1300r/min and the temperature of 47 ℃ for 55min to obtain a mixture D;
(5) adding the mixture C into the mixture D, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 15min, so as to obtain a mixture E;
(6) and adding 8 parts of special alkyd resin into the mixture E, mixing at the speed of 600r/min and the temperature of 40 ℃ for 20min, standing for 7h under a sealed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
Example 4
A preparation method of LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) according to the mass parts, stirring 40 parts of pure acrylic resin at a high speed, then adding 30 parts of polyurethane acrylic resin, wherein the stirring speed is 1200r/min, and the stirring time is 40min, so as to obtain a mixture A;
(2) mixing 1 part of defoaming agent and 1 part of dispersing agent at the mixing speed of 1300r/min, the mixing temperature of 50 ℃ and the mixing time of 40min to obtain a mixture B;
(3) mixing 60 parts of reactive monomer diluent and 8 parts of photoinitiator at the mixing speed of 1100r/min and the mixing temperature of 55 ℃ for 30min to obtain a mixture C;
(4) sequentially adding the mixture B and 2 parts of thixotropic agent into the mixture A, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 55min, so as to obtain a mixture D;
(5) adding the mixture C into the mixture D, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 15min, so as to obtain a mixture E;
(6) and adding 8 parts of special alkyd resin into the mixture E, mixing at the speed of 600r/min and the temperature of 40 ℃ for 20min, standing for 7h under a sealed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
Example 5
A preparation method of LED-UV cured environment-friendly high-temperature sintering varnish comprises the following steps:
(1) according to the mass parts, stirring 40 parts of pure acrylic resin at a high speed, then adding 30 parts of polyurethane acrylic resin, wherein the stirring speed is 1200r/min, and the stirring time is 40min, so as to obtain a mixture A;
(2) mixing 1 part of defoaming agent and 1 part of dispersing agent at the mixing speed of 1300r/min, the mixing temperature of 50 ℃ and the mixing time of 40min to obtain a mixture B;
(3) mixing 60 parts of reactive monomer diluent and 8 parts of photoinitiator at the mixing speed of 1100r/min and the mixing temperature of 55 ℃ for 30min to obtain a mixture C;
(4) sequentially adding the mixture B, 2 parts of thixotropic agent, 1 part of nano calcium carbonate and 1 part of nano aluminum oxide into the mixture A, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 55min, so as to obtain a mixture D;
(5) adding the mixture C into the mixture D, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 15min, so as to obtain a mixture E;
(6) and adding 8 parts of special alkyd resin into the mixture E, mixing at the speed of 600r/min and the temperature of 40 ℃ for 20min, standing for 7h under a sealed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
Comparative example 1
Example 5 was selected for comparison, the special alkyd resin in the raw material components of this comparative example was changed to rosin-modified maleic acid resin, and the remaining raw material formulation and preparation method were consistent with example 5, to obtain a varnish.
Comparative example 2
Example 5 is selected for comparison, 2 parts by mass of the special alkyd resin is added in the comparative example, and the formula and the preparation method of the other raw materials are the same as those in example 5, so that the varnish is prepared.
Comparative example 3
Example 5 was selected for comparison, the particle size of the added nano calcium carbonate and nano alumina in this comparative example was 5 μm, and the formulation and preparation method of the other raw materials were the same as those in example 5, to obtain a varnish.
Comparative example 4
Example 5 was chosen for comparison and a process for preparing a varnish comprising the steps of:
(1) according to the mass parts, stirring 40 parts of pure acrylic resin at a high speed, and then adding 30 parts of polyurethane acrylic resin and 8 parts of special alkyd resin, wherein the stirring speed is 1200r/min, and the stirring time is 40min, so as to obtain a mixture A;
(2) mixing 1 part of defoaming agent and 1 part of dispersing agent at the mixing speed of 1300r/min, the mixing temperature of 50 ℃ and the mixing time of 40min to obtain a mixture B;
(3) mixing 60 parts of reactive monomer diluent and 8 parts of photoinitiator at the mixing speed of 1100r/min and the mixing temperature of 55 ℃ for 30min to obtain a mixture C;
(4) sequentially adding the mixture B, 2 parts of thixotropic agent, 1 part of nano calcium carbonate and 1 part of nano aluminum oxide into the mixture A, wherein the mixing speed is 1300r/min, the mixing temperature is 47 ℃, and the mixing time is 55min, so as to obtain a mixture D;
(5) and adding the mixture C into the mixture D, mixing at the speed of 1300r/min and the temperature of 47 ℃ for 15min, standing for 7h under a sealed condition, and naturally cooling to room temperature to obtain the ink-mixing oil.
Examples 1-5 and comparative examples 1-4 performance testing:
the varnish prepared in examples 1 to 5 and comparative examples 1 to 4 was mixed with an inorganic pigment (red zircon iron) at a ratio of 0.8:1, stirred uniformly, and then ground with a grinder to a fineness of 20 μm or less to obtain an ink, which was then screen-printed:
1. printing the ink on the water transfer printing paper by using a 300-mesh silk screen;
2. curing with a mixed LED-UV light source with wavelengths of 365nm, 385nm and 395 nm;
3. printing the cured printing ink by using an 80-mesh screen printing plate;
4. the dried pattern and the cover oil are pasted on a workpiece through a water transfer printing and pattern pasting process and then sintered at a high temperature of 850 ℃.
(1) Adhesion test
The inks prepared in the examples and the comparative examples are pasted on a ceramic device by the water transfer printing process, and the adhesion test of the ink is carried out on the obtained ceramic device sample by using ISO 2409-2007 paint and varnish grid test, wherein the ISO grade is 1-5, and the higher the grade is, the worse the adhesion of the ink is.
(2) Flexibility test
The inks prepared in the examples and the comparative examples were applied to tinplate by the above-mentioned water transfer process, and the flexibility of the ink was measured according to GB/T1731-93 "paint film flexibility measuring method".
(3) Gloss measurement
The inks obtained in the respective examples and comparative examples were printed on white paper, and measured for gloss according to the national Standard GB9754-88 "measurement of 20 °, 60 °, 85 ° specular gloss of colored paint films of colored paints and varnishes containing no metallic pigment", and measured for gloss using a gloss measuring instrument (WGG 6060 ° gloss measuring instrument, manufactured by Shanghai Xinrui instruments Co., Ltd.).
The results of the performance tests of the examples and comparative examples are shown in table 1 below:
TABLE 1 Performance test of examples and comparative examples
From the test results, the ink prepared by using the LED-UV cured environment-friendly high-temperature sintering varnish prepared in the embodiments 1 to 5 has strong adhesive force, good flexibility and good glossiness, the ink prepared by using the LED-UV cured environment-friendly high-temperature sintering varnish prepared in the embodiments 1 to 5 can realize low-temperature rapid curing by adding the special alkyd resin, and the cured film obtained by curing the prepared ink has good flexibility and curing flexibility by adding the LED-UV cured environment-friendly high-temperature sintering varnish, and the adhesion property and the bonding property of the surface of a product are good, the printed pattern effect is clear, and the glossiness is good;
in the embodiment 2, the defoaming agent is added, so that bubbles generated in the mixing preparation process of the LED-UV cured environment-friendly high-temperature sintering varnish can be eliminated, the uniformity of raw material mixing is improved, bubbles generated in the screen printing process of ink prepared by using the LED-UV cured environment-friendly high-temperature sintering varnish can be eliminated, and the printing definition and the printing effect are effectively improved; in the embodiment 3, the defoaming agent and the dispersing agent are added, so that the raw materials are good in dispersion uniformity in the mixing preparation process, and the inorganic pigment can be more uniformly distributed in the varnish after the inorganic pigment is mixed with the varnish, so that the printing effect is effectively improved; example 4, a defoaming agent, a dispersing agent and a thixotropic agent are added, so that the environment-friendly high-temperature sintering varnish cured by LED-UV can obtain excellent thixotropic property, and a cured film obtained after the prepared varnish is cured has good adhesion on the surface of a product; in the embodiment 5, the defoaming agent, the dispersing agent, the thixotropic agent, the nano calcium carbonate and the nano aluminum oxide are added, so that the strength of the environment-friendly high-temperature sintering varnish for LED-UV curing is improved, the flexibility of a cured ink film and the adhesive force of the surface of a product are improved, and the printing ink has high adhesive force, the best flexibility and the best glossiness.
Comparative example 1 because no special alkyd resin was used, the ink was prepared by adding varnish, so that the adhesion of the cured film obtained after curing the prepared ink was significantly poor, and the cured film had poor flexibility, poor gloss and poor printing effect;
comparative example 2 because the amount of the special alkyd resin used was too small, the addition of the varnish resulted in a weaker adhesion of the cured film obtained after curing of the ink than in example 5, and also resulted in poorer flexibility and gloss, and poorer printing effect;
comparative example 3 since the added nano calcium carbonate and nano alumina have excessively large particle sizes, it is difficult to improve the strength of the varnish, the varnish was added to prepare an ink, so that the flexibility of the cured film obtained after curing the prepared ink was inferior to that of example 5, and the large-particle-size raw material deteriorated the glossiness of the ink.
In comparative example 4, the special alkyd resin is added in step (1), so that the special alkyd resin and the thixotropic agent are subjected to a crosslinking reaction, and the varnish is added, so that the adhesive force of a cured film obtained after the prepared ink is cured is obviously poor, the flexibility and the glossiness are poor, and the printing effect is poor.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. The environment-friendly high-temperature sintering varnish capable of being cured by LED-UV is characterized by comprising the following raw material components in parts by mass:
2. the LED-UV cured environment-friendly high-temperature sintering varnish according to claim 1, wherein the special alkyd resin is a long-oil air-drying alkyd resin.
3. The LED-UV cured environmentally friendly high temperature sintering varnish of claim 1, wherein the reactive monomer diluent comprises a mixture of two or more of 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate, and trimethylolpropane triacrylate.
4. The LED-UV cured environmentally friendly high temperature sintering varnish of claim 1, wherein the photoinitiator comprises a mixture of three or more of monoacylphosphine, diacyl phosphine, ethyl 2,4, 6-trimethylbenzoylphenylphosphonate, and 2-isopropylthioxanthone.
5. The LED-UV cured environment-friendly high-temperature sintering varnish according to claim 1, characterized by further comprising the following raw material components in parts by mass:
0.2-1 part of a defoaming agent;
the defoaming agent is an organic silicon defoaming agent or a fluorine modified organic silicon defoaming agent.
6. The LED-UV cured environment-friendly high-temperature sintering varnish according to claim 5, characterized by further comprising the following raw material components in parts by mass:
0.5-2 parts of a dispersing agent;
the dispersant is a polycarboxylic acid polymer dispersant or a polyacrylate dispersant.
7. The LED-UV cured environment-friendly high-temperature sintering varnish according to claim 6, characterized by further comprising the following raw material components in parts by mass:
1-3 parts of a thixotropic agent;
the thixotropic agent is a polyamide thixotropic agent.
8. The LED-UV cured environment-friendly high-temperature sintering varnish according to claim 7, characterized by further comprising the following raw material components in parts by mass:
0.1-2 parts of nano calcium carbonate
0.1-2 parts of nano aluminum oxide.
9. The LED-UV cured environment-friendly high-temperature sintering varnish according to claim 8, wherein the nano calcium carbonate has a particle size of 10-50 nm, and the nano alumina has a particle size of 10-50 nm.
10. The preparation method of the LED-UV cured environment-friendly high-temperature sintering varnish as claimed in claim 9, characterized by comprising the following steps:
(1) stirring pure acrylic resin at a high speed, and then adding polyurethane acrylic resin, wherein the stirring speed is 1000-1200 r/min, and the stirring time is 40-50 min, so as to obtain a mixture A;
(2) mixing the defoaming agent and the dispersing agent at the mixing speed of 1200-1500 r/min and the mixing temperature of 50-55 ℃ for 40-50 min to obtain a mixture B;
(3) mixing an active monomer diluent and a photoinitiator at the mixing speed of 1000-1200 r/min and the mixing temperature of 50-55 ℃ for 30-40 min to obtain a mixture C;
(4) sequentially adding the mixture B, the thixotropic agent, the nano calcium carbonate and the nano aluminum oxide into the mixture A, wherein the mixing speed is 1200-1500 r/min, the mixing temperature is 45-50 ℃, and the mixing time is 50-70 min, so as to obtain a mixture D;
(5) adding the mixture C into the mixture D, wherein the mixing speed is 1200-1500 r/min, the mixing temperature is 45-50 ℃, and the mixing time is 15-25 min, so as to obtain a mixture E;
(6) adding the special alkyd resin into the mixture E, wherein the mixing speed is 500-800 r/min, the mixing temperature is 40-45 ℃, the mixing time is 15-25 min, standing for 7-9 h under a closed condition, and naturally cooling to room temperature to obtain the LED-UV cured environment-friendly high-temperature sintering varnish.
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