CN105255257A - Thermosetting type glass screen printing ink and preparation method thereof - Google Patents
Thermosetting type glass screen printing ink and preparation method thereof Download PDFInfo
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- CN105255257A CN105255257A CN201510690149.1A CN201510690149A CN105255257A CN 105255257 A CN105255257 A CN 105255257A CN 201510690149 A CN201510690149 A CN 201510690149A CN 105255257 A CN105255257 A CN 105255257A
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Abstract
The invention discloses thermosetting type glass screen printing ink. The thermosetting type glass screen printing ink includes, by weight, 40%-65% of Evonik EP112 saturated polyester, 21%-45% of titanium dioxide TR-92, 0.5%-2.0% of fumed silica A-200, 10%-15% of methylated amino resin MF915, 1.0%-4.0% of adhesion promoters LTW, 0.5%-1.5% of antifoaming agents FOAMEXN, 0-1.0% of flatting agents BYK-310, 0-1.0% of brightening agents OB and 2%-6% of DBE solutions. A preparation method of the thermosetting type glass screen printing ink includes the steps that the saturated polyester, the titanium dioxide and the fumed silica are firstly stirred evenly, then the methylated amino resin, the adhesion promoters, the antifoaming agents, and/or the flatting agents, and/or the brightening agents are added into the mixture, and the DBE solutions are added finally. The thermosetting type glass screen printing ink has good adhesion, water resistance, acid and alkali resistance, cold and hot impact resistance, butanone dissolution resistance, fast yellowing resistance, high temperature yellowing resistance, flexibility, constructability and ultraviolet resistance.
Description
Technical field
The invention belongs to glass printing ink area, be specifically related to a kind of heat curing-type glass printing ink and preparation method thereof.
Background technology
Silk screen printing is a kind of ancient printing process, and the same with typography was the invention of Ancient Times in China, and printing technology picked by the folder that it originates from Qin-Han times, apart from the history of modern existing more than 2,000 year.Although the wire mark origin of China very early, but the development of modern fabrography is slow, and the wire mark country ratio of external advanced person, the state of the art of China also has certain difference, how much all there is the phenomenon of variable color in the ink be developed into, can not reach requirement completely when using.
Along with the increase of glass cross printing-ink products production and application quantity, organic solvent (VOC) pollution on the environment in ink, to the murder by poisoning of human body and the inflammable and explosive potential safety hazard caused more and more serious.
Also a lot of document and patent is had recent years to propose the waterborne glass ink of environmental protection.But these ink all also exist very large shortcoming: usual more than 600 DEG C of the temperature needed for high temperature sintering ink, consume energy very large; When dry solvent type ink is dry, have a large amount of VOC discharges, contaminate environment, time of drying is long simultaneously, a large amount of these not dry printed matters of space arrangement, even if ink is also easy to be rubbed after surface drying, needs could thoroughly parch in a week; Two component thermofixation glass ink needs the temperature-curable time of 30 minutes of 160 DEG C, and energy consumption is also very large, and the space taken is also very large; The glass ink relatively environmental protection of water-based, but solidifying the temperature being also wants about 160 DEG C, and the time of solidification also wants about 30 minutes, even longer.
Glass ink is mainly used in household electrical appliances and house ornamentation, and consumption is huge, and the main difficult point of research is at present the sticking power, resisting high-temperature yellowing, snappiness, application property, organic yellow sex change, resistance to butanone etc. of the sticking power of ink, poach postadhesion power, water soaking.
Summary of the invention
For above deficiency, the invention provides a kind of heat curing-type glass silk screen printing ink and preparation method thereof with good sticking power, water-fast, acid and alkali-resistance, cold-hot impact, the dissolving of resistance to butanone, organic yellow sex change, resisting high-temperature yellowing, snappiness, application property and anti-ultraviolet performance.
The technical scheme that the present invention takes is: a kind of heat curing-type glass silk screen printing ink, and by weight percentage, this heat curing-type glass silk screen printing ink raw materials comprises following raw material:
Above-mentioned heat curing-type glass silk screen printing ink preparation method comprises the following steps:
A () by the saturated polyester of formula ratio, titanium dioxide, aerosil heated and stirred 30 ~ 50 minutes, and is crushed to below particle diameter 10um, obtain mixture one;
B () thing one to be mixed is cooled to 25 ~ 32 DEG C, continue to add the methyl-etherified aminoresin of formula ratio, adhesion promoter and defoamer, heated and stirred 30 ~ 50 minutes;
C () finally adds the DBE solvent of formula ratio, heated and stirred, after 20 ~ 40 minutes, is cooled to 25 ~ 32 DEG C, crosses 200 mesh sieves, can obtain heat curing-type glass silk screen printing ink;
The Heating temperature of each step is 50 ~ 80 DEG C above, is conducive to the abundant mixing of each raw material like this.
Further, also comprise in described step (b) and add whitening agent, and/or flow agent.
Described step (a) specifically comprises the following steps: stirred with the speed of 300 ~ 700 revs/min by the saturated polyester of formula ratio, add the titanium dioxide of formula ratio, aerosil successively, with the stir speed (S.S.) heated and stirred 30 ~ 50 minutes of 700 ~ 1200 revs/min, and be crushed to below particle diameter 10um, obtain mixture one;
Described step (b) specifically comprises the following steps: thing one to be mixed is cooled to 25 ~ 32 DEG C, under the stir speed (S.S.) of 100 ~ 300 revs/min, continue to add the methyl-etherified aminoresin of formula ratio, adhesion promoter and defoamer, with the speed heated and stirred 30 ~ 50 minutes of 300-700 rev/min;
Described step (c) specifically comprises the following steps: under the stir speed (S.S.) of 100 ~ 300 revs/min, continue to add DBE solvent, with 100 ~ 300 revs/min of stir speed (S.S.) heated and stirred after 20 ~ 40 minutes, be cooled to 25 ~ 32 DEG C, cross 200 mesh sieves, heat curing-type glass silk screen printing ink can be obtained.
The viscosity of described heat curing-type glass silk screen printing ink is 25000-30000mPa.S/25 DEG C.
In above-mentioned formula, saturated polyester can play increase sticking power, improves the effects such as snappiness; Methyl-etherified aminoresin is used as linking agent, has the effect making glass silk screen printing ink have excellent gloss, tint retention, hardness, resistance to chemical reagents, water-fast and weather resisteant etc.
Titanium dioxide is indispensable white pigment in senior ink, the durable nondiscoloration of the ink containing titanium dioxide, and surface wettability is good, is easy to dispersion.
DBE solvent is the biodegradable environment protection type high-boiling-point solvent of a kind of energy, there is good levelling property, the glossiness of ink can be improved, improve snappiness and the sticking power of paint film, reduce the surface imperfection such as tangerine peel, pin hole, flake, crater, with vibrin, poly-aminoresin, acrylic resin, epoxy resin etc., there is good dissolving power.
Aerosil mainly plays the effect of thickening and thixotroping in ink, can form good nano-particle network in system, when after applying shearing force, network is destroyed, and after shearing force eliminates, network can recover rapidly again, thus plays the effect of thickening, thixotroping and anti-settling.
Advantage of the present invention: have selected a performance preferably model be win wound EP112 saturated polyester resin as main body, make glass silk screen printing ink have snappiness and resistance to excessive baking performance; And have selected methyl-etherified aminoresin as linking agent, ensure that drying property and the water tolerance of system; Add adhesion promoter LTW in addition and can solve the sticking power of ink for screen printing in glass local, the resisting high-temperature yellowing in addition for film also has good effect.
The effect of cooperatively interacting of each component above, obtain the heat curing-type glass silk screen printing ink with good sticking power, water-fast, acid and alkali-resistance, cold-hot impact, the dissolving of resistance to butanone, organic yellow sex change, resisting high-temperature yellowing, snappiness, application property and anti-ultraviolet performance, this ink for screen printing environmental protection, raw material low cost, fire-retardant, be applicable to promoting the use of on a large scale.In addition, aqueous thermosetting glass printing ink preparation method of the present invention is simple, meets industrial production.
Embodiment
Raw material used in the present invention is all that sale producer from the market directly buys and obtains.
A kind of heat curing-type glass silk screen printing ink, by weight percentage, comprises following raw material, as shown in table 1:
Table 1
| Material name | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Saturated polyester wins wound EP112 | 65％ | 50％ | 40％ | 40％ |
| Titanium dioxide TR-92 | 21％ | 30％ | 30.5％ | 45％ |
| Aerosil A-200 | 0.5％ | 1.0％ | 2％ | 0.5％ |
| Methyl-etherified aminoresin MF915 | 10％ | 12％ | 15％ | 10％ |
| Adhesion promoter enlightening height LTW | 1％ | 2％ | 4％ | 1％ |
| Defoamer FOAMEX N | 0.5％ | 1％ | 1.5％ | 0.5％ |
| Flow agent BYK-310 | 0 | 1％ | 0 | 0.5％ |
| Whitening agent OB | 0 | 0 | 1％ | 0.5％ |
| DBE solvent | 2％ | 3％ | 6％ | 2％ |
Embodiment 1
A kind of heat curing-type glass silk screen printing ink, its raw material is as shown in the embodiment 1 in table 1:
Above-mentioned heat curing-type glass silk screen printing ink preparation method is:
(a) by the saturated polyester of formula ratio with the speed of 300 revs/min stir, add titanium dioxide and aerosil while stirring, under the speed of 700 revs/min 50 DEG C stir 30 minutes, and grind to particle diameter be below 10um;
B () is cooled to 25 DEG C after, under the stir speed (S.S.) of 100 revs/min, add methyl-etherified aminoresin, adhesion promoter, defoamer successively, under the speed of 700 revs/min, 50 DEG C are stirred 30 minutes;
C () adds DBE solvent under the stir speed (S.S.) of 100 revs/min, stir 30 minutes at 60 DEG C of temperature, and through 200 mesh screen after being cooled to 25 DEG C, packaging, recording system viscosity is 25000mPa.S/25 DEG C.
Embodiment 2
A kind of heat curing-type glass silk screen printing ink, its raw material as shown in table 1, embodiment 2:
Above-mentioned heat curing-type glass silk screen printing ink preparation method is:
(a) by the saturated polyester of formula ratio with the speed of 400 revs/min stir, add titanium dioxide and aerosil while stirring, under the speed of 850 revs/min 60 DEG C stir 35 minutes, and grind to particle diameter be below 10um;
B () is cooled to 28 DEG C after, under the stir speed (S.S.) of 200 revs/min, add methyl-etherified aminoresin, adhesion promoter, defoamer and flow agent successively, under the speed of 500 revs/min, 60 DEG C are stirred 40 minutes;
C () adds DBE solvent under the stir speed (S.S.) of 200 revs/min, at 50 DEG C of temperature stir 35 minutes, be cooled to 28 DEG C, after through 200 mesh screen, packaging, recording system viscosity is 27000mPa.S/25 DEG C.
Embodiment 3
A kind of heat curing-type glass silk screen printing ink, its raw material is as shown in the embodiment 3 in table 1:
Above-mentioned heat curing-type glass silk screen printing ink preparation method is:
(a) by the saturated polyester of formula ratio with the speed of 500 revs/min stir, add titanium dioxide and aerosil while stirring, under the speed of 950 revs/min 70 DEG C stir 50 minutes, and grind to particle diameter be below 10um;
B () is cooled to 30 DEG C after, under the stir speed (S.S.) of 300 revs/min, add methyl-etherified aminoresin, adhesion promoter, defoamer and whitening agent successively, stir 30 minutes the speed 80 DEG C of 300 revs/min;
C () adds DBE solvent under the stir speed (S.S.) of 300 revs/min, at 50 DEG C of temperature stir 25 minutes, be cooled to 28 DEG C, after through 200 mesh screen, packaging, recording system viscosity is 30000mPa.S/25 DEG C.
Embodiment 4
A kind of heat curing-type glass silk screen printing ink, its raw material is as shown in the embodiment 4 in table 1:
Above-mentioned heat curing-type glass silk screen printing ink preparation method is:
(a) by the saturated polyester of formula ratio with the speed of 700 revs/min stir, add titanium dioxide and aerosil while stirring, under the speed of 1200 revs/min 80 DEG C stir 40 minutes, and grind to particle diameter be below 10um;
B () is cooled to 32 DEG C after, under the stir speed (S.S.) of 170 revs/min, add methyl-etherified aminoresin, adhesion promoter, defoamer, flow agent and whitening agent successively, under the speed of 450 revs/min, 60 DEG C are stirred 50 minutes;
C () adds DBE solvent under the stir speed (S.S.) of 170 revs/min, at 50 DEG C of temperature stir 40 minutes, be cooled to 32 DEG C, after through 200 mesh screen, packaging, recording system viscosity is 28500mPa.S/25 DEG C.
Comparative example 1
A kind of heat curing-type glass silk screen printing ink, by weight percentage, comprises following raw material, as shown in table 2:
Table 2
| Material name | Content |
| Saturated polyester is with moral AK3130 | 50％ |
| Titanium dioxide TR-92 | 30％ |
| Aerosil A-200 | 1.0％ |
| Methyl-etherified aminoresin Ineos MF915 | 12％ |
| Adhesion promoter enlightening height LTW | 2％ |
| Defoamer FOAMEX N | 1.0％ |
| Flow agent BYK-310 | 1.0％ |
| DBE solvent | 3％ |
Above-mentioned heat curing-type glass silk screen printing ink preparation method is with embodiment 2.
Comparative example 2
A kind of heat curing-type glass silk screen printing ink, by weight percentage, comprises following raw material, as shown in table 3:
Table 3
| Name of material | Content |
| Saturated polyester wins wound EP112 | 40％ |
| Titanium dioxide TR-92 | 30.5％ |
| Aerosil A-200 | 2.0％ |
| Butylated amino resin ten thousand coloured silk 301 | 15％ |
| Adhesion promoter LTW | 4％ |
| Defoamer FOAMEX N | 1.5％ |
| Whitening agent OB | 1％ |
| DBE solvent | 6％ |
Above-mentioned heat curing-type glass silk screen printing ink preparation method is with embodiment 3.
Comparative example 3
A kind of heat curing-type glass silk screen printing ink, by weight percentage, comprises following raw material, as shown in table 3:
Table 4
| Name of material | Content |
| Saturated polyester wins wound EP112 | 40％ |
| Titanium dioxide TR-92 | 45％ |
| Aerosil A-200 | 0.5％ |
| Benzene is for aminoresin ten thousand coloured silk 401 | 10％ |
| Adhesion promoter LTW | 1.0％ |
| Defoamer FOAMEX N | 0.5％ |
| Flow agent BYK-310 | 0.5％ |
| Whitening agent OB | 0.5％ |
| DBE solvent | 2％ |
Above-mentioned heat curing-type glass silk screen printing ink preparation method is with embodiment 4.
The inspecting standard of each embodiment and comparative example is as follows above:
1. system and environmental requirement: ink system is single-component, long response time thermofixation glass private type, environmental protection numerical value meets European Union's household electrical appliance objectionable impurities limitation standard.
2. outward appearance: necessary free from dust, particle, impurity in container; Color marks color designation with in packaging, model conforms to; Ink mobility will be got well, and can not become to draw skin shape or solidification glue connection; Tenderly white, have opacifying property, heat (190 DEG C) does not distil, variable color of not gasifying, and meets light (high light three days sunlight exposures or 1000W ultraviolet lighting are apart from 50cm, 6h) and does not turn yellow.
3. the shelf lives: under normal temperature, do not open former ink the quality guaranteed period be more than or equal to 12 months, open after or be in harmonious proportion ink the quality guaranteed period be more than or equal to 6 months.
4. be adapted to the performance of printing: the pure ink of silk-screen is adjusted to good dispersity when viscosity is 2500mpa.s ± 300mpa.s printing, and levelling property is moderate, and thixotropy is moderate, coating uniform, without obvious tangerine peel, without pinprick bubble, no ink spot existence.10 times printings at 30 seconds/time, interval are without dry net phenomenon (80 to 350 order polyester half tones can cross net smoothly).
5. be adapted to solidify the performance of drying; Infrared photothermal curing oven, equilibrium region temperature 170 DEG C ± 5 DEG C (glass coating is apart from top 100mm spatial dimension air themperature), 5 minutes interlayer used times, thorough solidification 10 minutes (the lifting warm area time separately calculates), after solidification, interlayer reaches half-dried, back cover reaches and solidifies commissure completely, and solvent noresidue is not after-tacked.Ink coating should without variable color, non-carbonized phenomenon, the above-mentioned condition of test drying baker temperature reference.
6. hardness: 1H Mitsubishi pencil load 500 grams test, the ink coating of glass should without indenture, disrepair phenomenon.
7. sticking power: after the ink original color coat curing oven 24h of glass, hundred lattice methods of testing should without chip obscission, mixed ink coating grid Ying≤15% area obscission.
8. water boiling resistance: exemplar is positioned in 98 DEG C ± 2 DEG C neutral hot water tanks to take out after 1 hour and dries, tested after 2 hours, and the ink coating face of glass should without expansion, without peeling, without obscission; When coating has mist to become, have after 24 hours and obviously alleviate thin out phenomenon.
9. acid resistance: the H of 5%
2sO
4spot test observation test after 16 hours, free of pinholes bubble is answered in the ink coating face of glass, and without expanding, without peeling, without obscission, front is without metachromatism;
10. alkali resistance: NaOH spot test observation test after 16 hours of 5%, free of pinholes bubble is answered in the ink coating face of glass, and without expanding, without peeling, without obscission, front is without metachromatism;
11. dissolubility resistents: alcohol is stained with by cotton, cotton is stained with butanone parcel 1Kg balance weights, wiping more than 15 times back and forth, the ink coating face of tested glass should without dissolving, and without fading, without expanding, nothing is damaged, without separation phenomenon.
12. cold-hots impact: high-low temperature test chamber sets 60 DEG C ± 5 DEG C and places 2 hours, and place 2 hours for-25 DEG C ± 2 DEG C, this is a circulation, do 5 rear tests of circulation; The ink coating face of glass does not come off, without be full of cracks, and color and standard no significant difference; After coating paste specify glue, adhesive tape and foamed material position, from glass front observation can not there is metachromatism.
13. wet fastnesss: climatic chamber design temperature 60 DEG C ± 5 DEG C, humidity 85 DEG C ± 5 DEG C, take out test after 96 hours, the ink coating face of glass does not come off, without be full of cracks, color and standard no significant difference; After coating paste specify glue, adhesive tape and foamed material position, from glass front observation can not there is metachromatism.
14. anti-ultraviolet properties: 1000W ultraviolet lamp, range 50cm, test after placing 6h, the ink coating face of glass does not come off, without be full of cracks, color and standard no significant difference; After coating paste specify glue, adhesive tape and foamed material position, from glass front observation can not there is metachromatism.
Carry out above-mentioned performance test to the heat curing-type glass silk screen printing ink that above each embodiment and comparative example obtain, its performance test results is as shown in table 5:
Table 5
| Performance perameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Outward appearance | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified |
| Shelf lives | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified |
| Be adapted to the performance of printing | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified |
| The performance that solidification is dried | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Hardness (H) | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Sticking power (level) | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Water boiling resistance | Qualified | Qualified | Qualified | Qualified | Defective | Defective | Defective |
| Acid resistance | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Alkali resistance | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Dissolubility resistent | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Cold-hot impacts | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
| Wet fastness | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Defective |
| Anti-ultraviolet property | Qualified | Qualified | Qualified | Qualified | Qualified | Defective | Qualified |
Above-mentioned reference embodiment is to the detailed description of this heat curing-type glass silk screen printing ink and preparation method thereof; illustrative instead of determinate; several embodiments can be listed according to institute's limited range; therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
Claims (7)
1. a heat curing-type glass silk screen printing ink, is characterized in that, described heat curing-type glass silk screen printing ink, by weight percentage, comprises following raw material:
2. a preparation method for heat curing-type glass silk screen printing ink as claimed in claim 1, it is characterized in that, described preparation method comprises the following steps:
A () by the saturated polyester of formula ratio, titanium dioxide, aerosil heated and stirred 30 ~ 50 minutes, and is crushed to below particle diameter 10um, obtain mixture one;
B () thing one to be mixed is cooled to 25 ~ 32 DEG C, continue to add the methyl-etherified aminoresin of formula ratio, adhesion promoter and defoamer, heated and stirred 30 ~ 50 minutes;
C () finally adds the DBE solvent of formula ratio, heated and stirred, after 20 ~ 40 minutes, is cooled to 25 ~ 32 DEG C, crosses 200 mesh sieves, can obtain heat curing-type glass silk screen printing ink;
The Heating temperature of each step is 50 ~ 80 DEG C above.
3. the preparation method of heat curing-type glass silk screen printing ink according to claim 2, is characterized in that: also comprise in described step (b) and add whitening agent and/or flow agent.
4. the preparation method of the heat curing-type glass silk screen printing ink according to Claims 2 or 3, it is characterized in that, described step (a) specifically comprises the following steps: stirred with the speed of 300 ~ 700 revs/min by the saturated polyester of formula ratio, add the titanium dioxide of formula ratio, aerosil successively, with the stir speed (S.S.) heated and stirred 30 ~ 50 minutes of 700 ~ 1200 revs/min, and be crushed to below particle diameter 10um, obtain mixture one.
5. the preparation method of the heat curing-type glass silk screen printing ink according to Claims 2 or 3, it is characterized in that, described step (b) specifically comprises the following steps: thing one to be mixed is cooled to 25 ~ 32 DEG C, under the stir speed (S.S.) of 100 ~ 300 revs/min, continue to add the methyl-etherified aminoresin of formula ratio, adhesion promoter and defoamer, with the speed heated and stirred 30 ~ 50 minutes of 300-700 rev/min.
6. the preparation method of the heat curing-type glass silk screen printing ink according to Claims 2 or 3, it is characterized in that, described step (c) specifically comprises the following steps: under the stir speed (S.S.) of 100 ~ 300 revs/min, continue to add DBE solvent, with 100 ~ 300 revs/min of stir speed (S.S.) heated and stirred after 20 ~ 40 minutes, be cooled to 25 ~ 32 DEG C, cross 200 mesh sieves, heat curing-type glass silk screen printing ink can be obtained.
7. the preparation method of the heat curing-type glass silk screen printing ink according to Claims 2 or 3, is characterized in that: the viscosity of described heat curing-type glass silk screen printing ink is 25000-30000mPa.S/25 DEG C.
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Denomination of invention: Thermosetting type glass screen printing ink and preparation method thereof Effective date of registration: 20190725 Granted publication date: 20180413 Pledgee: Huizhou Merchants Bank Wuhu three mountain branch Pledgor: WUHU CHUNFENG NEW MATERIAL CO., LTD. Registration number: 2019340000415 |