CN110607093A - Solvent-free glass screen printing ink and preparation method thereof - Google Patents
Solvent-free glass screen printing ink and preparation method thereof Download PDFInfo
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- CN110607093A CN110607093A CN201910990211.7A CN201910990211A CN110607093A CN 110607093 A CN110607093 A CN 110607093A CN 201910990211 A CN201910990211 A CN 201910990211A CN 110607093 A CN110607093 A CN 110607093A
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- 239000011521 glass Substances 0.000 title claims abstract description 48
- 238000007650 screen-printing Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims description 14
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 238000000227 grinding Methods 0.000 claims abstract description 30
- 239000006229 carbon black Substances 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000003822 epoxy resin Substances 0.000 claims abstract description 16
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 16
- 239000004593 Epoxy Substances 0.000 claims abstract description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 10
- 239000000440 bentonite Substances 0.000 claims abstract description 9
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 9
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims description 40
- 238000001723 curing Methods 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 claims description 3
- 239000012776 electronic material Substances 0.000 claims description 3
- UIDDPPKZYZTEGS-UHFFFAOYSA-N 3-(2-ethyl-4-methylimidazol-1-yl)propanenitrile Chemical group CCC1=NC(C)=CN1CCC#N UIDDPPKZYZTEGS-UHFFFAOYSA-N 0.000 claims description 2
- 238000007639 printing Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000006058 strengthened glass Substances 0.000 abstract description 2
- 239000000976 ink Substances 0.000 description 56
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000012360 testing method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 7
- 239000004744 fabric Substances 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 6
- 239000003973 paint Substances 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000000178 monomer Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 125000003700 epoxy group Chemical group 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 229920003180 amino resin Polymers 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 238000000016 photochemical curing Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 238000004383 yellowing Methods 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a solvent-free glass silk-screen printing ink which comprises a component A and a component B, wherein the component A is prepared by adding epoxy resin, a dispersing agent, carbon black, organic bentonite, an epoxy silane coupling agent, a defoaming agent and a leveling agent in different process stages, dispersing at a high speed, grinding and stirring; the component B is prepared by an aminosilane coupling agent and an imidazole epoxy curing agent through stirring. The invention has the following advantages: high solid content without solvent; the curing speed is low at normal temperature, so that the waste of the printing ink is reduced; can be applied to various strengthened glass white sheets.
Description
Technical Field
The invention relates to the technical field of screen printing ink, in particular to solvent-free glass screen printing ink and a preparation method thereof.
Background
In the prior art, Chinese patent application with publication number CN109181405A discloses UV-LED glass ink and a preparation method thereof, wherein the glass ink is prepared by taking polyester acrylate, difunctional urethane acrylate and hexafunctional urethane acrylate as main raw materials, adding an active monomer, a filling agent, a photoinitiator, an auxiliary agent and silicon dioxide, and uniformly mixing and grinding the raw materials. The glass ink has the characteristics of high curing speed and high curing efficiency, and the glass ink with different appearance effects can be prepared by adjusting the composition of the filler. The invention also provides a using method of the UV-LED glass ink, which comprises the steps of adopting 250-mesh 300-mesh screen printing, controlling the thickness of the ink layer to be 10-30 mu m, carrying out photocuring after printing is finished, wherein the curing time is 40-60s, the glass ink has short curing time and good curing effect, a glass product cannot be yellowed, and the body of an operator cannot be damaged due to over-strong illumination in the photocuring process. The UV printing ink has insufficient covering power, obviously poorer chemical resistance performance indexes, and the monomer used in the UV printing ink has greater irritation to skin, especially low molecular weight monomer; in addition, the production and storage of UV inks is particularly sensitive to light and is prone to failure during storage.
In the prior art, the invention disclosed in the chinese patent application with publication number CN109535818A provides a water-based glass screen printing ink, which is composed of the following components in parts by weight: 30-55 wt% of acrylic resin, 4-12 wt% of amino resin, 10-35 wt% of pigment, 3-10 wt% of filler, 0.5-5 wt% of cosolvent, 0.5-3 wt% of assistant and 15-40 wt% of water. Meanwhile, a preparation method of the water-based glass silk-screen printing ink is also provided. The water-based glass silk-screen printing ink disclosed by the invention is less in volatile matter, strong in adhesive force, good in water boiling resistance, acid and alkali resistance, yellowing resistance and solvent resistance; meanwhile, the coating film after screen printing has high glossiness, no solvent residue, environmental friendliness and no harm to human bodies; the preparation method for preparing the water-based glass silk-screen printing ink is simple and easy to operate. The ink has insufficient covering power, various chemical resistance performance indexes cannot completely meet market requirements, and the stability of the amino resin in a system is poor, so that failure in the storage process is easily caused.
In general, the main directions of the environmental-friendly glass ink in the prior art are water-based ink, UV ink, high solid content and the like. The covering power and various chemical resistance indexes of the existing UV ink are obviously insufficient, and the monomers used in the UV ink have greater irritation to skin, especially low molecular weight monomers, and cause damage to the health of production workers in a dust-free printing workshop. The printing property of the existing water-based ink is inferior to that of solvent-based ink (the surface tension of water is large), various chemical resistance performance indexes can not completely meet the market demand, the stability of amino resin in a system is poor, failure in the storage process is easy to cause, and the defect that the water-based ink can not be completely prepared exists.
Disclosure of Invention
The invention aims to provide the solvent-free glass silk-screen printing ink which can be applied to glass silk-screen printing, can be mixed for use for more than 8 hours under the condition of not changing the existing printing process and can reduce ink waste.
The invention also aims to provide a preparation method of the solvent-free glass silk-screen printing ink.
In order to achieve the above purpose, the invention provides the following technical scheme: the solvent-free glass silk-screen printing ink comprises resin, carbon black, an auxiliary agent and the like, and is prepared from the following components in parts by weight:
the component A comprises:
the component B comprises:
5-15 parts of amino silane coupling agent
85-95 parts of imidazole epoxy curing agent.
The epoxy resin can be one of NPEL128 epoxy resin produced by Nanya electronic materials (Kunshan) Co., Ltd or GELR128 epoxy resin produced by Hongchang electronic materials Co., Ltd; the 128 epoxy resin has excellent mechanical properties, chemical resistance, heat resistance and the like after being cured.
The dispersant may be Solsperse 20000 hyperdispersant from Lubrizol. The active ingredient of the dispersant is 100%, and the dispersant has good dispersibility on carbon black and excellent stability at high temperature in an epoxy system.
The carbon BLACK may be carbon BLACK manufactured by Degussa corporation (Evonik Degussa) having a SPECIAL BLACK 4A model. The carbon black has low oil absorption, can be used for preparing ink with high carbon black content, and has excellent insulating property after high-temperature dispersion.
The epoxy Silane coupling agent may be Silquest A-187 Silane (gamma-glycidoxypropyltrimethoxysilane) from Momentive group, or KBM-403 epoxy Silane coupling agent from shin-Etsu chemical industries, Inc. The active component of the epoxy silane coupling agent is more than 98 percent, and the epoxy propoxy and methoxy groups are contained, so that the water resistance of the coating and the adhesive force on a glass substrate can be obviously improved.
The organobentonite may be Claytone APA organobentonite from ByK, Germany; the organic bentonite can improve the thixotropy of the ink and reduce the undesirable phenomena of shrinkage cavity or tooth edge and the like.
The organic matting powder may be PERGAPAK M6 from Yabao corporation, USA; the organic extinction powder has stable gloss in a system, and the extinction effect caused by the influence of a silane coupling agent such as silicon dioxide extinction powder can not occur.
The leveling agent may be DC 57 from Dow Corning corporation (Dow Corning); the leveling agent is a non-reactive ethylene glycol copolymer surfactant with 100% active concentration.
The antifoaming agent may be TSA-750S from Meiji chart of Japan; the TSA-750S belongs to dimethyl silane modified defoaming emulsion with 100 percent of effective components.
The aminosilane coupling agent may be Z-6020 by Dow Corning corporation (Dow Corning) or Silquest A-1120Silane, Momentive, New materials group; the active ingredient of the amino silane coupling agent is 99 percent, is diamino functional group silane, can react with epoxy resin and glass base material, and obviously improves the adhesive force and water resistance.
The imidazole curing agent may be 1-cyanoethyl-2-ethyl-4-methylimidazole, and is preferably 2E4MZ or 2E4MZ-CN available from Kabushiki Kaisha. The imidazole curing agent has the advantages of small dosage, long applicable period, medium-temperature curing, small volatility, low toxicity or no toxicity, and excellent performance of cured products.
The preparation method of the solvent-free glass silk-screen printing ink comprises the following steps:
component A
Premixing: adding epoxy resin and a dispersant into a dispersion cylinder, uniformly stirring, then adding carbon black and organic bentonite, and dispersing for 25-30 minutes at the rotation speed of 800-;
a first grinding stage: grinding for 3-4 times until the fineness is less than 8 um;
and (3) dispersion treatment: the dispersion speed is controlled to be 500-1800 rpm, the epoxy silicon-oxygen coupling agent is added, the stirring speed is controlled to be 1200-1800rpm, the dispersion time is 1-3 hours, the temperature is controlled to be 100-120 ℃, the dispersion is cooled to room temperature after dispersion, and the high-speed dispersion has the advantages that the dispersant completely coats the carbon black at the temperature (100-120 ℃) so as to isolate the carbon black particles and insulate the carbon black particles;
a second grinding stage: if the organic matting powder is added during stirring, grinding until the fineness is less than 12 um; then adding the flatting agent and the defoaming agent in sequence and stirring uniformly;
packaging: the ink was filtered through a 200 mesh filter cloth as required and contained in a 1L paint can.
The component B comprises:
mixing: imidazole curing agent and amino silane coupling agent are added according to the proportion, stirred evenly and filled in a plastic bottle of 100 ml.
The use process method of the solvent-free glass silk-screen printing ink comprises the following steps: the ratio of the component A to the component B is 10: 0.5-3; stirring AB evenly, standing for 5-10 minutes, curing and baking at 150-180 ℃ for 15-30 minutes. Preferably, the practical proportion of the component A and the component B is 10: 1.
After being printed on all mirror silver of the tempered glass and completely baked, the solvent-free glass silk-screen printing ink disclosed by the invention passes a water boiling 2-hour test and various environment tests (including a high-temperature high-humidity test, a cold and hot impact test, a 96-hour UV illumination test, a salt spray resistance test, an alcohol wiping resistance test and a sweat resistance test), and the test results are summarized as follows: the coverage rate is high, the OD value of 420-mesh printing reaches more than 5.0, and the LED point light source test is carried out: the phenomena of light transmission, pinholes, sand holes, tooth edges and the like are avoided; the insulation property is good, and the insulation property is excellent under 1000V voltage; the roughness Rz of the printing ink is less than or equal to 5 mu m; and the authentication is controlled by halogen, REACH and ROHS.
Compared with the prior art, the invention has the beneficial effects that: the high solid content does not cause solvent volatilization, and the health of operating personnel is not damaged; the curing speed is low at normal temperature, so that the waste of the ink is reduced (the AB component of the conventional ink needs to be replaced after being mixed and used for 4 hours, and the product can be used for more than 8 hours); the glass can be specially applied to various strengthened glass white sheets (optical glass lenses such as mobile phone lenses, touch screen (capacitive screen) lenses, medical lenses and the like).
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
TABLE 1 shows solvent-free glass screen inks of examples 1-6
The preparation method of the solvent-free glass silk-screen printing ink comprises the following steps:
component A
Premixing: adding epoxy resin and a dispersing agent into a dispersion cylinder, uniformly stirring, then adding carbon black and organic bentonite, and dispersing for 26 minutes at the rotating speed of 9009 rpm;
a first grinding stage: grinding for 3 times until the fineness is less than 8 um;
and (3) dispersion treatment: the dispersing speed is controlled to be 5505rpm, epoxy group silica coupling agent is added, the stirring speed is controlled to be 1300rpm, the dispersion is carried out for 15 hours, the temperature is controlled to be 105 ℃, and the dispersion is cooled to room temperature after the dispersion, the high-speed dispersion has the advantage that the carbon black is completely coated by the dispersing agent at the temperature, so that the carbon black particles are isolated and insulated;
a second grinding stage: if the organic matting powder is added during stirring, grinding until the fineness is less than 12 um; then adding the flatting agent and the defoaming agent in sequence and stirring uniformly;
packaging: the ink was filtered through a 200 mesh filter cloth as required and contained in a 1L paint can.
The component B comprises:
mixing: imidazole curing agent and amino silane coupling agent are added according to the proportion, stirred evenly and filled in a plastic bottle of 100 ml.
Preferably, the preparation method of the solvent-free glass screen printing ink comprises the following steps:
component A
Premixing: adding epoxy resin and a dispersing agent into a dispersion cylinder, uniformly stirring, then adding carbon black and organic bentonite, and dispersing for 29 minutes at the rotating speed of 1100 rpm;
a first grinding stage: grinding for 4 times until the fineness is less than 8 um;
and (3) dispersion treatment: the dispersing speed is controlled to be 650rpm, the epoxy group silica coupling agent is added, the stirring speed is controlled to be 1700rpm, the dispersion is carried out for 3 hours, the temperature is controlled to be 115 ℃, the dispersion is cooled to room temperature, and the high-speed dispersion has the advantages that the carbon black is completely coated by the dispersing agent at the temperature, so that the carbon black particles are isolated and insulated;
a second grinding stage: if the organic matting powder is added during stirring, grinding until the fineness is less than 12 um; then adding the flatting agent and the defoaming agent in sequence and stirring uniformly;
packaging: the ink was filtered through a 200 mesh filter cloth as required and contained in a 1L paint can.
The component B comprises:
mixing: imidazole curing agent and amino silane coupling agent are added according to the proportion, stirred evenly and filled in a plastic bottle of 100 ml.
Most preferably, the preparation method of the solvent-free glass screen printing ink comprises the following steps:
component A
Premixing: adding epoxy resin and a dispersing agent into a dispersion cylinder, uniformly stirring, then adding carbon black and organic bentonite, and dispersing for 28 minutes at the rotating speed of 1000 rpm;
a first grinding stage: grinding for 3 times in a three-roller machine until the fineness is less than 8 um;
and (3) dispersion treatment: the rotating speed of the dispersion machine is controlled to be 600rpm, the epoxy group silica coupling agent is added, the stirring speed is controlled to be 1500rpm, the dispersion is carried out for 2 hours, the temperature is controlled to be 110 ℃, the dispersion is cooled to room temperature after the dispersion, and the high-speed dispersion has the advantage that the dispersion agent completely coats the carbon black at the temperature (110 ℃) so that the carbon black particles are isolated and insulated;
a second grinding stage: if the organic matting powder is added during stirring, grinding the mixture in a three-roller machine until the fineness of the mixture is less than 12 um; then sequentially adding a flatting agent and a defoaming agent into the dispersion cylinder and uniformly stirring;
packaging: the ink was filtered through a 200 mesh filter cloth as required and contained in a 1L paint can.
The component B comprises:
mixing: imidazole curing agent and amino silane coupling agent are added according to the proportion, stirred evenly and filled in a plastic bottle of 100 ml.
The use process method of the solvent-free glass silk-screen printing ink comprises the following steps: the ratio of the component A to the component B is 10: 2; stirring AB evenly, standing for 6-8 minutes, curing and baking at the temperature of 160-170 ℃ for 20-25 minutes. Preferably, the using process method of the solvent-free glass silk-screen printing ink comprises the following steps: the ratio of the component A to the component B is 10: 1; and stirring the AB uniformly, standing for 7 minutes, and curing and baking at 165 ℃ for 23 minutes.
Example 7
The solvent-free glass silk-screen printing ink is prepared from the following components in parts by weight:
the component A comprises:
the component B comprises:
Z-6020 10
2E4MZ 90
the preparation method of the solvent-free glass silk-screen printing ink comprises the following steps:
component A
Premixing: adding NPEL128 epoxy resin and Solsperse 20000 dispersing agent into a dispersion cylinder, uniformly stirring, then adding SPECIAL BLACK 4A carbon BLACK and BYK Additives Gmbh organic bentonite, and dispersing for 30 minutes at the rotating speed of 1000 rpm;
a first grinding stage: grinding for 4 times in a three-roller machine until the fineness is less than 8 um;
and (3) dispersion treatment: adding Silquest A-187 Silane epoxy silicone coupling agent while stirring, controlling the stirring speed at 1500rpm, dispersing for 2 hours, controlling the temperature at 110 ℃, and cooling to room temperature after dispersing;
a second grinding stage: continuously grinding in a three-roller machine, and sequentially adding a DC 57 leveling agent and a TSA-750S defoaming agent into a dispersion cylinder and uniformly stirring;
packaging: the ink was filtered through a 200 mesh filter cloth as required and contained in a 1L paint can.
The component B comprises:
mixing: adding Z-6020 imidazole curing agent and 2E4MZ aminosilane coupling agent according to the proportion, stirring uniformly, and filling into a 100ml plastic bottle.
And (3) performance testing:
the AB components are uniformly mixed according to the ratio of 100: 15, printed by a 350-mesh screen plate and baked for 30 minutes at 180 ℃ and then tested to have the following properties:
example 8
The solvent-free glass silk-screen printing ink comprises the following raw materials in parts by weight:
the component A comprises:
the component B comprises:
Z-6020 10
2E4MZ 90
the preparation method of the solvent-free glass silk-screen printing ink comprises the following steps:
component A
Premixing: adding NPEL128 epoxy resin and Solsperse 20000 dispersing agent into a dispersion cylinder, uniformly stirring, then adding SPECIAL BLACK 4A carbon BLACK and BYK Additives Gmbh organic bentonite, and dispersing for 30 minutes at the rotating speed of 1000 rpm;
a first grinding stage: grinding for 4 times in a three-roller machine until the fineness is less than 8 um;
and (3) dispersion treatment: adding Silquest A-187 Silane epoxy group silica coupling agent while stirring, controlling the stirring speed at 1500rpm to disperse for 2 hours, controlling the temperature at 120 ℃, and cooling to room temperature after dispersion;
a second grinding stage: adding PERGOPAK M6 organic matting powder while stirring, and grinding in a three-roller machine until the fineness is less than 12 um; sequentially adding a DC 57 leveling agent and a TSA-750S defoaming agent into a dispersion cylinder and uniformly stirring;
packaging: the ink was filtered through a 200 mesh filter cloth as required and contained in a 1L paint can.
The component B comprises:
mixing: adding Z-6020 imidazole curing agent and 2E4MZ aminosilane coupling agent according to the proportion, stirring uniformly, and filling into a 100ml plastic bottle.
And (3) performance testing:
the AB components are uniformly mixed according to the ratio of 100: 10, printed by a 350-mesh screen plate and baked for 30 minutes at 180 ℃ and then tested to have the following properties:
the results of the performance tests of other examples of the present invention were substantially identical to the results of examples 7 and 8 described above, all having the unexpected effects described as the advantageous effects of the present invention.
In general, the invention achieves the effect of solvent-free volatilization by using resin, auxiliary agent and the like with 100 percent of solid content or active ingredients; the use time of the printing ink is 8 hours by using the imidazole latent curing agent, and the carbon black achieves the insulation effect by the production process treatment. The product has better performance than solvent type glass printing ink sold in the market, has no toxicity, does not pollute the environment and harm the human health, and has low requirements on the fire prevention and explosion prevention grade in the production, use and storage processes.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention should not be limited thereby, and all equivalent changes and modifications made in the spirit of the present invention and the contents of the specification are included in the scope of the present invention.
Claims (11)
1. The solvent-free glass silk-screen printing ink is characterized by comprising the following components in parts by weight:
the component A comprises:
the component B comprises:
5-15 parts of amino silane coupling agent
85-95 parts of imidazole epoxy curing agent.
2. The solvent-free glass screen printing ink as claimed in claim 1, wherein the epoxy resin is one of NPEL128 epoxy resin manufactured by south asia electronic materials (kunshan) limited or GELR128 epoxy resin manufactured by marchand electronic materials ltd.
3. The solvent-free glass screen printing ink as claimed in claim 1, wherein the dispersant is Solsperse 20000 ultra-dispersant from Luobo Runz.
4. The solventless glass screen ink of claim 1 wherein the carbon BLACK is degussa type specific BLACK 4A carbon BLACK.
5. The solvent-free glass screen printing ink according to claim 1, wherein the epoxy Silane coupling agent is Silquest A-187 Silane from Michigan advanced materials group or KBM-403 epoxy Silane coupling agent from shin-Etsu chemical industries, Ltd.
6. The solventless glass screen ink of claim 1 wherein the organobentonite is Claytone APA organobentonite from Bicke, Germany.
7. The solventless glass screen printing ink of claim 1 wherein the organic matting powder is PERGAPAK M6 from Abauba, USA.
8. The solvent-free glass screen printing ink as claimed in claim 1, wherein the leveling agent is DC 57 of dow corning corporation; the antifoaming agent is TSA-750S from Japan Meiji chart.
9. The solvent-free glass screen printing ink as claimed in claim 1, wherein the aminosilane coupling agent is Z-6020 by Dow Corning company or Silquest A-1120Silane of Michigan advanced materials group.
10. The solvent-free glass screen printing ink according to claim 1, wherein the imidazole curing agent is 1-cyanoethyl-2-ethyl-4-methylimidazole.
11. The preparation method of the solvent-free glass screen printing ink as claimed in claim 1, wherein the method comprises the following steps:
component A
Premixing: adding epoxy resin and a dispersant into a dispersion cylinder, uniformly stirring, then adding carbon black and organic bentonite, and dispersing for 25-30 minutes at the rotation speed of 800-;
a first grinding stage: grinding for 3-4 times until the fineness is less than 8 um;
and (3) dispersion treatment: the dispersion speed is controlled to be 500-1800 rpm, the epoxy silicon-oxygen coupling agent is added, the stirring speed is controlled to be 1200-1800rpm, the dispersion time is 1-3 hours, the temperature is controlled to be 100-120 ℃, and the epoxy silicon-oxygen coupling agent is cooled to the room temperature after the dispersion;
a second grinding stage: if the organic matting powder is added during stirring, grinding until the fineness is less than 12 um; then adding the flatting agent and the defoaming agent in sequence and stirring uniformly;
the component B comprises:
mixing: imidazole curing agent and amino silane coupling agent are added according to the proportion and stirred evenly.
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| CN110607093B (en) | 2022-04-12 |
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