CN107778991B - Zirconium-free ultra-white water-based ceramic ink for ink-jet printing and preparation method thereof - Google Patents
Zirconium-free ultra-white water-based ceramic ink for ink-jet printing and preparation method thereof Download PDFInfo
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- 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
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
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Abstract
The invention relates to zirconium-free water-based ceramic ink for super-white ink-jet printing and a preparation method thereof. The invention adopts two inorganic white pigments, namely zinc oxide and hydroxyapatite nano powder to mix, and because the two powders have different particle characteristics, the interaction between the particles is weakened, thereby avoiding particle aggregation, the ceramic ink has uniform particle size under the action of a dispersing agent, the average particle size is less than 290nm, the ink has no demixing and sedimentation after standing for 8 days, the stability is good, the Hunter whiteness average value after being decorated on a glaze surface is more than 92, and the requirement of the ink for ceramic ink-jet printing is met.
Description
Technical Field
The invention relates to zirconium-free super-white ceramic ink and a preparation method thereof, which are mainly used for ceramic ink-jet printing and belong to the field of ceramic ink.
Background
The ceramic ink-jet printing technology is a non-contact printing technology without printing plate, and can directly image electronic images on the surface of ceramic, and through intelligent color matching, the patterns are well-arranged, and small-batch and multi-color tests or production can be completed in a short time. Compared with screen printing and roller printing, the ink-jet printing technology has the advantages of high efficiency, convenience, energy conservation and environmental protection, and is a ceramic decoration technology with high application value. Ceramic ink is the core of ceramic ink-jet printing technology, and there are more than 14 ceramic inks that have been successfully developed, including blue, brown, yellow, pink, etc. For example, the Chinese invention patent "a red ceramic ink for inkjet printing and a method for using the same" (CN 103045003A) discloses a red ceramic ink for inkjet printing, which is composed of a soluble metal complex and an organic solvent. The Chinese invention patent yellow ceramic ink for ink-jet printing (CN 103342917B) discloses yellow ceramic ink for ink-jet printing, which consists of inorganic pigment powder, a surfactant, a solvent and a dispersant. The Chinese invention patent (CN 106009897A) discloses a preparation method of blue ceramic ink for ink-jet printing.
At present, most researches on white ceramic ink are zirconium-containing and titanium-containing oily ink which takes organic matters as additives, and whiteness and stability are difficult to guarantee. For example, the Chinese invention patent "oil-based white ink for ink-jet recording" (CN 101027370B) discloses an oil-based white ink prepared by using titanium oxide as a ceramic coloring material and adding a resin, an organic solvent and a nonionic surfactant. The Chinese invention patent (CN 103224725B) discloses an oily white ink compounded by a plurality of oxides such as silicon oxide, aluminum oxide and the like. The oily ink has the problems of toxicity of organic solvents and the like, and the water-soluble organic solvent is the development direction of the ceramic ink in the future. The Chinese invention patent (CN 103804993B) discloses an aqueous white ink for preparing a zirconium oxide and silicon oxide mixed pigment by a sol-gel method. Zirconium oxide has the advantages of high whiteness, good stability and the like as a white material for ink-jet printing, but zirconium is easy to coexist with hafnium, hafnium has certain radioactivity, and the preparation cost of zirconium oxide is high, so that the development of white water-based ceramic ink with less zirconium or no zirconium has the significance of energy conservation and environmental protection.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides the ceramic ink for the ultra-white zirconium-free water-based ink-jet printing, which has high whiteness and good ink rheology and is suitable for ceramic ink-jet printing, and the preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the water-based ceramic ink is prepared by mixing and ball-milling nano zinc oxide powder and nano hydroxyapatite powder, adding a solvent and a dispersant, ball-milling and ultrasonically dispersing.
According to the scheme, the average grain size of the nano zinc oxide powder is 21.9-61.8 nm, and the nano zinc oxide powder is prepared by the following method: adding triammonium citrate powder into a zinc acetate solution with the concentration of 0.1-0.3 mol/L, uniformly stirring to obtain a transparent solution, adding absolute ethyl alcohol to obtain a zinc hydroxide suspension, adjusting the pH value of the zinc hydroxide suspension to 8-10 by using an ammonia water solution, heating the zinc hydroxide suspension at 60-80 ℃ for 2-4 h to obtain sol, drying the sol, and calcining to obtain nano zinc oxide powder.
According to the scheme, the mass ratio of the zinc acetate to the triammonium citrate in the transparent solution is 50-60: 40 to 50.
According to the scheme, the drying temperature is 80-100 ℃, the drying time is 5-10 hours, the calcining temperature is 500-700 ℃, and the calcining time is 8-12 hours.
According to the scheme, the average grain size of the nano hydroxyapatite powder is 21.9-61.8 nm, and the nano hydroxyapatite powder is prepared by the following method: mixing Ca (NO)3)2Solution and (NH)4)2HPO4And mixing the solutions to obtain a mixed solution, adjusting the pH value of the mixed solution to 8-10 by using an ammonia water solution, heating the mixed solution at 60-80 ℃ for 2-4 h to obtain gel, drying the gel, and calcining to obtain nano hydroxyapatite powder.
According to the scheme, the Ca (NO)3)2Solution and (NH)4)2HPO4The volume concentration of the solution is 40-60%.
According to the scheme, the drying temperature is 80-100 ℃, the drying time is 5-10 hours, the calcining temperature is 600-700 ℃, and the calcining time is 8-12 hours.
The invention also provides a preparation method of the zirconium-free water-based ceramic ink for super white ink-jet printing, which comprises the following steps: mixing nano zinc oxide powder and nano hydroxyapatite powder according to a mass ratio of 10-90: 10-90, mixing, performing ball milling for 3-6 hours to obtain composite powder, adding a solvent and a dispersing agent into the obtained composite powder, performing ball milling and mixing for 2-4 hours to obtain a suspension, and performing ultrasonic dispersion on the suspension uniformly to obtain the white ceramic ink.
Preferably, the solvent is ethanol, and the dispersant is one or a mixture of any two or more of polyethylene glycol, sodium dodecyl benzene sulfonate, povidone K30 and glycerol in any proportion.
Preferably, the mass percentages of the composite powder, the solvent and the dispersant in the suspension are as follows: 30-40% of composite powder, 50-60% of solvent and 5-10% of dispersing agent.
Preferably, the ultrasonic dispersion time is 30-60 min.
The invention adopts a sol-gel method to prepare nano zinc oxide and nano hydroxyapatite powder with uniform size and high purity, and then adds a solvent, a suspension, a dispersant and the like to prepare the zirconium-free and heavy metal-free water-based ceramic ink for super-white ink-jet printing. The hydroxyapatite can effectively inhibit the zinc oxide from growing in the calcining process, and the mixing of the two nano-powders can play the roles of reflecting and scattering light to the maximum extent, so that the whiteness of the hydroxyapatite is equivalent to that of a white material containing zirconium. Meanwhile, the additive is selected and added to play a good role in resisting precipitation, promoting suspension and keeping whiteness, for example, STTP can eliminate electrostatic attraction among powder particles, increase repulsive force, break micelle agglomeration, release wrapped free water, reduce viscosity of glaze slip and increase rheological property, and finally the ceramic ink for ultrawhite zirconium-free water-based inkjet printing, which is suitable for ceramic inkjet printing, is obtained.
The invention has the beneficial effects that:
1. according to the invention, two inorganic nano zinc oxide and hydroxyapatite powder are mixed, and because the two powder particles have different characteristics, hydroxyl exists in the hydroxyapatite and is easy to react with an organic additive to form surface coating, so that the interaction among the particles is weakened, and the attractive force among the hydroxyapatite particles is further weakened by taking ethanol as a solvent, so that the particle aggregation is avoided, therefore, under the action of a dispersing agent, the ceramic ink has uniform particle size, the average particle size is less than 290nm, after standing for 8 days, the ink has no layering and sedimentation, the stability is good, the Hunter whiteness average value after being decorated on a glaze surface is greater than 92, and the requirement of the ink for ceramic ink-jet printing is met.
2. The preparation process of the ultra-white zirconium-free ceramic ink is simple, wherein the calcination temperature of the composite white pigment is only 600-700 ℃, and the zirconia pigment is prepared by burning at the high temperature of 1500 ℃ in the prior art. Therefore, the cost of the white ceramic ink is only 1/3-1/2 of zirconium-containing ink.
Drawings
FIG. 1 is an XRD spectrum of a composite white pigment of zinc oxide and hydroxyapatite prepared in example 1 of the present invention;
FIG. 2 is a graph showing a particle size distribution of the ceramic ink prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1
The preparation method of the zirconium-free ultra-white water-based ceramic ink for ink-jet printing comprises the following specific steps:
1) preparation of composite white pigment
Preparation of nano zinc oxide powder
Adding triammonium citrate powder into a zinc acetate solution with the concentration of 0.1mol/L, magnetically stirring and mixing for 30min to obtain a transparent solution, adding absolute ethyl alcohol to obtain a zinc hydroxide suspension, adding 5 volume percent of ammonia water to adjust the pH value to 8, carrying out water bath at 80 ℃ for 2h to obtain sol, drying at 80 ℃ for 8h in an electric heating constant temperature drying oven, and calcining at 500 ℃ for 12h in a resistance furnace to obtain nano zinc oxide powder.
The mass fraction of zinc acetate in the transparent solution is 60%, and the mass fraction of triammonium citrate is 40%.
Preparation of nano hydroxyapatite powder
Mixing Ca (NO)3)2And (NH)4)2HPO4Mixing the solution for 30min to obtain a mixed solution, adjusting the pH to 8 with 5% ammonia water by volume percentage, carrying out water bath at 60 ℃ for 2h to obtain gel, drying at 80 ℃ for 5h in an electrothermal constant-temperature drying oven, and calcining at 600 ℃ for 9h in a resistance furnace to obtain nano hydroxyapatite powder.
Ca (NO) in the above mixed solution3)2Solution and (NH)4)2HPO4The volume percentages of the solutions were all 50%.
Preparation of composite powder of nano zinc oxide and hydroxyapatite
Mixing the nano zinc oxide and the nano hydroxyapatite powder obtained in the first step and the second step by mass percent: 70% of zinc oxide and 30% of hydroxyapatite are mixed and ball milled for 3 hours to obtain the composite white pigment.
2) Preparation of white ceramic ink
And (4) adding a solvent and a dispersing agent into the composite powder obtained in the third step to obtain a mixture, performing ball milling and mixing for 2 hours to obtain a suspension, and performing ultrasonic treatment in an ultrasonic cleaner for 30min to obtain the white ceramic ink.
The solvent is ethanol, and the dispersant is 1:1 mixture of polyethylene glycol and glycerol. Wherein the amount of the composite powder accounts for 40 percent of the total mass of the mixture, the addition amount of the solvent accounts for 55 percent of the total mass of the mixture, and the addition amount of the dispersant accounts for 5 percent of the total mass of the mixture.
As shown in fig. 1, which is an XRD spectrum of the composite white pigment of zinc oxide and hydroxyapatite prepared in this example, it can be seen that the crystals of zinc oxide and hydroxyapatite are relatively intact. Fig. 2 is a particle size distribution diagram of the ceramic ink prepared in this example, and it can be seen that the particle sizes of the powders in the ceramic ink are uniform and normally distributed.
Tests prove that the average grain size of the nano zinc oxide and hydroxyapatite composite powder is 33nm, the average grain size of the prepared white ceramic ink is 290nm, and the Hunter whiteness after being decorated on a glaze surface is 93, so that the ink meets the requirements of ink for ceramic ink-jet printing.
Example 2
The preparation method of the zirconium-free ultra-white water-based ceramic ink for ink-jet printing comprises the following specific steps:
1) preparation of composite white pigment
Preparation of nano zinc oxide powder
Adding triammonium citrate powder into a zinc acetate solution with the concentration of 0.3mol/L, magnetically stirring and mixing for 50min to obtain a transparent solution, adding absolute ethyl alcohol to obtain a zinc hydroxide suspension, adding 6 volume percent ammonia water to adjust the pH value to 10, carrying out water bath at 60 ℃ for 4h to obtain sol, drying at 100 ℃ for 5h in an electric heating constant-temperature drying oven, and calcining at 700 ℃ for 8h in a resistance furnace to obtain nano zinc oxide powder.
The mass fraction of zinc acetate in the transparent solution is 40%, and the mass fraction of triammonium citrate is 60%.
Preparation of nano hydroxyapatite powder
Mixing Ca (NO)3)2And (NH)4)2HPO4Mixing the solution for 30min to obtain a mixed solution, adjusting the pH to 9 with 5% ammonia water by volume percentage, carrying out water bath at 70 ℃ for 3h to obtain gel, drying at 100 ℃ for 5h in an electrothermal constant-temperature drying oven, and calcining at 500 ℃ for 12h in a resistance furnace to obtain nano hydroxyapatite powder.
Ca (NO) in the above mixed solution3)2The volume percentage of the solution is 60%, (NH)4)2HPO4The volume percentage of the solution was 40%.
Preparation of composite powder of nano zinc oxide and hydroxyapatite
Mixing the nano zinc oxide and the nano hydroxyapatite powder obtained in the first step and the second step by mass percent: 50% of zinc oxide and 50% of hydroxyapatite are mixed and ball-milled for 4 hours to obtain the composite white pigment.
2) Preparation of white ceramic ink
And (4) adding a solvent and a dispersing agent into the composite powder obtained in the third step to obtain a mixture, performing ball milling and mixing for 3 hours to obtain a suspension, and performing ultrasonic treatment in an ultrasonic cleaner for 50min to obtain the white ceramic ink.
The solvent is ethanol, and the dispersant is a mixture of polyethylene glycol, sodium dodecyl benzene sulfonate and povidone K30, which respectively account for 30%, 30% and 40%. Wherein the amount of the composite powder accounts for 30 percent of the total mass of the mixture, the addition amount of the solvent accounts for 60 percent of the total mass of the mixture, and the addition amount of the dispersant accounts for 10 percent of the total mass of the mixture.
Tests prove that the average grain size of the nano zinc oxide and hydroxyapatite composite powder is 42nm, the average grain size of the prepared white ceramic ink is 275nm, and the Hunter whiteness after being decorated on a glaze surface is 92, so that the ink meets the requirements of ink for ceramic ink-jet printing.
Claims (9)
1. The zirconium-free ultra-white water-based ceramic ink for ink-jet printing is characterized in that: the water-based ceramic ink is prepared by mixing and ball-milling nano zinc oxide powder and nano hydroxyapatite powder, adding a solvent and a dispersant, ball-milling and ultrasonically dispersing;
the preparation method comprises the following steps: mixing nano zinc oxide powder and nano hydroxyapatite powder according to a mass ratio of 10-90: 10-90, mixing, performing ball milling for 3-6 hours to obtain composite powder, adding a solvent and a dispersing agent into the obtained composite powder, performing ball milling and mixing for 2-4 hours to obtain a suspension, and performing ultrasonic dispersion on the suspension uniformly to obtain white ceramic ink;
the solvent is ethanol; the dispersing agent is one or a mixture of more than two of polyethylene glycol, sodium dodecyl benzene sulfonate, povidone K30 and glycerol in any proportion.
2. The aqueous ceramic ink for zirconium-free ultra-white inkjet printing according to claim 1, wherein: the average grain size of the nano zinc oxide powder is 21.9-61.8 nm, and the nano zinc oxide powder is prepared by the following method: adding triammonium citrate powder into a zinc acetate solution with the concentration of 0.1-0.3 mol/L, uniformly stirring to obtain a transparent solution, adding absolute ethyl alcohol to obtain a zinc hydroxide suspension, adjusting the pH value of the zinc hydroxide suspension to 8-10 by using an ammonia water solution, heating the zinc hydroxide suspension at 60-80 ℃ for 2-4 h to obtain sol, drying the sol, and calcining to obtain nano zinc oxide powder.
3. The aqueous ceramic ink for zirconium-free ultra-white inkjet printing according to claim 2, characterized in that: the mass ratio of the zinc acetate to the triammonium citrate in the transparent solution is 50-60: 40 to 50.
4. The aqueous ceramic ink for zirconium-free ultra-white inkjet printing according to claim 2, characterized in that: the drying temperature is 80-100 ℃, the drying time is 5-10 h, the calcining temperature is 500-700 ℃, and the calcining time is 8-12 h.
5. The aqueous ceramic ink for zirconium-free ultra-white inkjet printing according to claim 1, wherein: the average grain size of the nano hydroxyapatite powder is 21.9-61.8 nm, and the nano hydroxyapatite powder is prepared by the following method: mixing Ca (NO)3)2Solution and (NH)4)2HPO4And mixing the solutions to obtain a mixed solution, adjusting the pH value of the mixed solution to 8-10 by using an ammonia water solution, heating the mixed solution at 60-80 ℃ for 2-4 h to obtain gel, drying the gel, and calcining to obtain nano hydroxyapatite powder.
6. The aqueous ceramic ink for zirconium-free ultra-white inkjet printing according to claim 5, wherein: the Ca (NO)3)2Solution and (NH)4)2HPO4The volume concentration of the solution is 40-60%.
7. The aqueous ceramic ink for zirconium-free ultra-white inkjet printing according to claim 5, wherein: the drying temperature is 80-100 ℃, the drying time is 5-10 h, the calcining temperature is 600-700 ℃, and the calcining time is 8-12 h.
8. A method for preparing the zirconium-free water-based ceramic ink for ultra-white ink-jet printing according to any one of claims 1 to 7, which is characterized by comprising the following steps: mixing nano zinc oxide powder and nano hydroxyapatite powder according to a mass ratio of 10-90: 10-90, mixing, performing ball milling for 3-6 hours to obtain composite powder, adding a solvent and a dispersing agent into the obtained composite powder, performing ball milling and mixing for 2-4 hours to obtain a suspension, and performing ultrasonic dispersion on the suspension uniformly to obtain the white ceramic ink.
9. The preparation method according to claim 8, wherein the mass percentages of the composite powder, the solvent and the dispersant in the suspension are as follows: 30-40% of composite powder, 50-60% of solvent and 5-10% of dispersing agent.
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CN109535846A (en) * | 2018-12-21 | 2019-03-29 | 湖北工业大学 | A kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink |
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CN103224725A (en) * | 2013-04-08 | 2013-07-31 | 佛山市道氏科技有限公司 | White glaze printing ink for ceramic ink-jet printing and preparation method thereof |
CN103804993A (en) * | 2013-11-27 | 2014-05-21 | 佛山市明朝科技开发有限公司 | Extra-white aqueous ceramic ink-jet ink and preparation method thereof |
KR20150057718A (en) * | 2013-11-20 | 2015-05-28 | 주식회사 엘지생활건강 | Solid coating preparation for tooth whitening |
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CN103224725A (en) * | 2013-04-08 | 2013-07-31 | 佛山市道氏科技有限公司 | White glaze printing ink for ceramic ink-jet printing and preparation method thereof |
KR20150057718A (en) * | 2013-11-20 | 2015-05-28 | 주식회사 엘지생활건강 | Solid coating preparation for tooth whitening |
CN103804993A (en) * | 2013-11-27 | 2014-05-21 | 佛山市明朝科技开发有限公司 | Extra-white aqueous ceramic ink-jet ink and preparation method thereof |
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