CN105198495A - Small-particle-diameter praseodymium zirconium yellow ceramic pigment and preparation method thereof - Google Patents
Small-particle-diameter praseodymium zirconium yellow ceramic pigment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a small-particle-diameter praseodymium zirconium yellow ceramic pigment which comprises the following components in percentage by weight: 3-6% of praseodymium oxide, 48-62% of zirconium oxide, 30-38% of silicon dioxide and 3-8% of a mineralizing agent, wherein the zirconium oxide selects the product which does not remove hafnium elements in the zirconium oxide production process, wherein the atom molar ratio of zirconium oxide to the hafnium elements is greater than 40:1; silicon dioxide selects silicon dioxide aerogel, wherein the BET specific surface area is 500-800 m<2>/g, the average particle diameter is 3-8 [mu]m, and the pore volume is 3-5. The praseodymium zirconium yellow pigment is small in particle diameter and relatively stable in structure, and is hard to damage in the ceramic ink preparation process. Meanwhile, the pigment is high in color strength in transparent glaze, and fine and smooth in color tone, and can be used as the high-grade ceramic pigment.
Description
Technical field
The present invention relates to a kind of ceramic pigment, be specifically related to yellow ceramic pigment of the less praseodymium zirconium of a kind of median size and preparation method thereof, and utilize this ceramic pigment to prepare the method for ceramic ink.
Background technology
Ceramic decoration ink is applied to all kinds of ceramic decoration technology, as traditional ceramic printing technology, ceramic decoration color ink jet printed technology (InkJetPrinting), ceramic ink jet printing technique etc.In general, the method for decorative porcelain is all the ceramic ink containing colorant or tinting material are printed on ceramic cooked flake by ink-jet or other printing modes, then through firing fixed pattern.By the shower nozzle aperture of ink-jet and the restriction of ink via system, in ceramic ink, pigment granules is sufficiently tiny of to ensure the smooth and easy of ink-jet.Depositing and the solids precipitation in use procedure for avoiding simultaneously, necessarily requiring pigment granules tiny.High-grade ceramic ink is fine and smooth just because of colorant, aberration is little and price is extremely expensive.Praseodymium zirconium yellow material is widely used in inorganic ceramic colorant field with the colour generation ability of the tone of its gracefulness and stability.When being applied in ceramic ink, praseodymium zirconium yellow material is also faced with the same Problems existing of colorant of other kinds: how to overcome aberration, how to promote the adhesivity of colorant, how to avoid the destruction to colorant grain pattern in ink preparation process.
If application number is for described in 201010104665.9 " a kind of preparation methods of Mn-Al red ceramic colorant " by name, choose reasonable component prescription, and in formula, add organic incendiary material, utilize low-temperature burning technique to prepare pigment color development and stablize.Fine size and the red pigment be evenly distributed.
Summary of the invention
For the ubiquitous problem of the ceramic pigment be applied in ceramic ink, the invention provides a kind of yellow ceramic pigment of praseodymium zirconium of small particle size, the praseodymium zirconium yellow material grain diameter not only burnt out is little, structure is more stable, makes it structure in the process preparing ceramic ink and is not easily destroyed.Meanwhile, this colorant is high in colour strength in transparent, and the fine and smooth no color differnece of tone, can be used as high-grade ceramic colorant and use.
Technical problem to be solved by this invention is achieved by the following technical programs:
1, composition of raw materials
Choose reasonable composition of raw materials is the inevitable choice preparing high-grade ceramic colorant.In the large-scale production of the yellow ceramic pigment of praseodymium zirconium, solid-phase synthesis is preparation method the most ripe.The reaction that the solid-phase synthesis being chief component with zirconium white, Praseodymium trioxide, silicon-dioxide and mineralizer occurs is:
SiO
2+ZrO
2→ZrSiO
4
In the reaction, mineralizer impels reaction to carry out smoothly as catalyzer, the Pr then in tinting material Praseodymium trioxide
4+ion enters ZrSiO
4in lattice, thus form sosoloid colorant.
The component of the yellow ceramic pigment of praseodymium zirconium in the present invention and weight percent corresponding to component are: Praseodymium trioxide 3-6%, zirconium white 48-62%, silicon-dioxide 30-40%, mineralizer 3-8%; Wherein zirconium white selects the product not removing hafnium element in zirconium white production process, and wherein zirconium white is greater than 40:1 with the atomic molar ratio of hafnium element; Silicon-dioxide selects aerosil, and its BET specific surface area is 500-800m
2/ g, median size is 3-8 μm, and volume of voids is 3-5.
Hafnium element is one of element common in Zirconium Ore, and hafnium element forms zircon-hafnon solid solution with the zr element in the form of perfect isomorphism displacement Zirconium Ore.In nature mineral, Zr and Hf atomic ratio mean value is about 50:1-20:1, and this ratio changes according to the difference of zircon raw ore kind.In the process of preparation pure zirconia, often want separating hafnium element, and very difficult both being separated, and the cost that also result in the high zirconia material of purity remains high.Prepare the yellow ceramic pigment of praseodymium zirconium zirconia material used many uses pure zirconia in prior art, as electric smelting zirconium or chemical zirconium, purity is more high better, affects reaction in solid phase synthesis to avoid foreign ion.The present inventor found through experiments, the product not removing hafnium element in zirconium white production process is used to replace high-purity mangesium oxide zirconium as zirconic source in the yellow ceramic pigment of praseodymium zirconium, zirconic cost can not only be reduced, and the reaction in solid phase synthesis is not affected, even to a certain extent to the Pr of tinting material Praseodymium trioxide
4+ion enters in lattice and forms sosoloid and have promoter action, macro manifestations is the colour generation ability that can promote praseodymium zirconium yellow material, but need controlled oxidization zirconium to be greater than 40:1 with the atomic molar ratio of hafnium element, hafnium constituent content too much has impact for colorant integral color, and can affect Pr
4+ion enters lattice colour developing.
The common quartz adopting aerosil to replace generally adopting in prior art in the present invention and zirconium white react, aerosil not only purity is high, and specific surface area is large, volume of voids is high, can contact reacts abundant with zirconium white, make to generate ZrSiO in solid phase
4reaction carry out more complete.The particle diameter of aerosil itself is little, and property is crisp, uses common grinding tank or other mechanical mill mode can be ground into finer and smoother powder, contributes to the refinement of colorant powder entirety.In the present invention, the aerosil BET specific surface area selected is 500-800m
2/ g, median size is 3-8 μm, and volume of voids is 3-5, these require for aerosil preparation comparatively easily reach, and for ceramic pigment production enough.Also specific surface area can be adopted larger, and the aerosil that volume of voids is larger, must consider the preparation cost of ceramic pigment.Aerosil in the present invention uses method conventional in prior art to prepare, and as utilized silicon sol aging, purifying in a solvent, or using sol-gel method, not repeating them here.
Ultra-fine quartz also can be selected in the source of silicon-dioxide, and it is that in the 1-5 μm of follow-up process of lapping of guarantee, colorant is organized and is not damaged that the granularity of ultrafine quartz powder need reach median size.
Further preferably, the component of the yellow ceramic pigment of praseodymium zirconium and weight percent corresponding to component are Praseodymium trioxide 3.5-4%, zirconium white 58-62%, aerosil 30-35%, mineralizer 3-6%.
Mineralizer plays vital effect in the building-up process of colorant, for improving the activity of reactant, reducing the synthesis temperature of colorant, is conducive to carrying out smoothly of reaction.In the present invention, mineralizer is preferably the mixture of ammonium chloride, barium fluoride and potassium silicofluoride, and its weight ratio is ammonium chloride 1: barium fluoride 2: potassium silicofluoride 1.5, and wherein barium fluoride can be replaced Sodium Fluoride, and potassium silicofluoride can be replaced Sodium Silicofluoride.The present inventor found through experiments, use the mineralizer of above-mentioned formula can reduce colorant calcining temperature, make colorant colour generation evenly.
Further optimization of C/C composites, also can add the cerium oxide or yttrium oxide that mass percent is 0.5-1% in the yellow ceramic pigment of above-mentioned praseodymium zirconium.Add appropriate cerium oxide or yttrium oxide can increase the yellow ceramic pigment of praseodymium zirconium in colour strength, make the color and luster of praseodymium zirconium yellow material more soft.
2, the preparation method of the yellow ceramic pigment of praseodymium zirconium
Step one, by Praseodymium trioxide, zirconium white, aerosil and mineralizer raw material pulverizing, to be ground to particle diameter be 1-3 μm, mixes after oven dry.
In prior art in the past, the raw material particle size adopted is large and size-grade distribution is wide, make the colorant particle diameter after firing also large, size-grade distribution is also wide, causes the follow-up grain pattern destroying colorant in the process of lapping preparing ceramic ink, causes that colorant colour killing is serious, color development is shallow.In the solution of the present invention, the raw material particle size difference of employing is little, narrow particle size distribution, and makes colorant powder raw material easily be milled to less particle diameter due to the characteristic of aerosil.
Step 2, is positioned over the raw material mixed in saggar and calcines, and calcining temperature is 1000-1200 DEG C, and the time controling of temperature-rise period is 2-3h, and temperature is incubated 2-3h after rising to calcining temperature, and that takes out that namely saggar obtain the yellow ceramic pigment of praseodymium zirconium burns till product.Because the particle diameter of Pigment Material is less, thus colorant calcining time can proper extension to ensure the abundance in reaction times.General ceramic pigment calcining temperature is more than 1200 DEG C, in the present invention, because with the addition of suitable mineralizer, calcining temperature can be controlled as 1000-1200 DEG C.
Step 3, will burn till product grinding evenly in step 2, by washed with de-ionized water 3-4 time, dries, obtains required praseodymium zirconium Huang ceramic pigment.Prepare grinding plant in the process of praseodymium zirconium yellow material and use common grinding pot, also can use the lapping mode in other conventional colorant preparation process.
Above-mentioned praseodymium zirconium yellow material grain diameter is 1-3 μm, Stability Analysis of Structures, again grinds and also can not affect its structure.
3, the preparation method that the yellow ceramic pigment of above-mentioned praseodymium zirconium prepares ceramic ink is applied
Yellow for praseodymium zirconium ceramic pigment is added in the solvent of ceramic ink with weight percent 20-40%, after mixing, this ink is ground to colorant particle diameter and is less than 1 μm and namely obtains required ink.Further preferably, the yellow ceramic pigment of praseodymium zirconium is added in the solvent of ceramic ink with weight percent 35-40%.
The preparation method of ceramic ink has dispersion method, sol-gel method, reverse microemulsion method etc., no matter any preparation method, and the praseodymium zirconium yellow material in the present invention all can be used as tinting material and uses.Because obtained praseodymium zirconium yellow material grain diameter is 1-3 μm, the pigment granules in ink controls to be less than 1 μm can meet service requirements, so the milling time prepared in ink process is short, can not damages the weave construction of pigment granules thus affect hair color effect.
The present invention has following beneficial effect:
1, the yellow ceramic pigment of the praseodymium zirconium in the present invention controls and gradation grinding through strict raw material, can be 1-3 μm by size controlling, the colorant particle diameter burnt out is not only little, and structure is more stable, and in the process of the corresponding ceramic ink of preparation, its structure is not easily destroyed.
2, in the present invention, zirconium white selects the product not removing hafnium element in zirconium white production process, can reduce the cost of the yellow ceramic pigment of praseodymium zirconium.
3, the yellow ceramic pigment of the praseodymium zirconium in the present invention is that colour strength is high, the fine and smooth no color differnece of tone, can be used as high-grade ceramic colorant and uses.
4, yellow ceramic pigment preparation technology is simple for the praseodymium zirconium in the present invention, and use conventional solid synthesis method, applicable conventional plant carries out large-scale production.
Embodiment
Below by embodiment, content of the present invention is conducted further description.
The Praseodymium trioxide adopted in embodiment and zirconium white are commercially available, and wherein zirconium white selects the product not removing hafnium element in zirconium white production process, and wherein zirconium white is greater than 40:1 with the atomic molar ratio of hafnium element.Selected aerosil BET specific surface area is 700m
2/ g, median size is 3 μm, and volume of voids is 3.Mineralizer used is the mixture of ammonium chloride, barium fluoride and potassium silicofluoride, and its weight ratio is ammonium chloride 1: barium fluoride 2: potassium silicofluoride 1.5.
The preparation method of the yellow ceramic pigment of praseodymium zirconium is as follows:
Step one, by Praseodymium trioxide, zirconium white, aerosil and mineralizer raw material pulverizing, to be ground to particle diameter be 1 μm, mixes after oven dry;
Step 2, is positioned over the raw material mixed in saggar and calcines, and calcining temperature is 1000 DEG C, and the time controling of temperature-rise period is 3h, and temperature is incubated 2h after rising to calcining temperature, and that takes out that namely saggar obtain the yellow ceramic pigment of praseodymium zirconium burns till product;
Step 3, will burn till product grinding evenly in step 2, by washed with de-ionized water 3 times, dries, obtains the yellow ceramic pigment of required praseodymium zirconium.
Colorant in colour strength decision method: the praseodymium zirconium of preparation yellow material is added in transparent base glaze with 6% and makes color glaze, then glazing makes test piece on base, burn till rear use color difference meter test brightness value L
*with yellow value degree b
*.
The formula of praseodymium zirconium yellow material is as shown in the table, and formula consists of mass percentage content.
From embodiment, the colorant in the present invention is high in yellow intensity in transparent, transparency good.
Comparative example 1
Formula consists of mass percentage content, and Praseodymium trioxide, mineralizer use consistent with embodiment, and zirconium white uses ordinary city sale of electricity to melt zirconium, and silicon-dioxide uses silica powder.
Can be found out by above-mentioned comparative example, in embodiment, colorant of the present invention is better than the colorant colouring effect of the common prescription of prior art.
Comparative example 2
Formula consists of mass percentage content, and mineralizer uses the mineralizer the same with embodiment to form.
Can be found out by above-mentioned comparative example, add cerium oxide and make to increase in colour strength.
Comparative example 3
Formula consists of mass percentage content:
Can be found out by above-mentioned comparative example, add yttrium oxide and make to increase in colour strength.
Yellow for the praseodymium zirconium obtained in above-described embodiment ceramic pigment is added in the solvent of ceramic ink with weight percent 20-40%, after mixing, this ink is ground to colorant particle diameter and is less than 1 μm and namely obtains the yellow ink of the good praseodymium zirconium of colour generation.
More preferably, can yellow for praseodymium zirconium in above-described embodiment ceramic pigment be added in the solvent of ceramic ink with weight percent 35-40%, be ground to colorant particle diameter after mixing and be less than 1 μm and namely obtain the yellow ink of required praseodymium zirconium.
Finally it should be noted that, above embodiment is only in order to illustrate the technical scheme of the embodiment of the present invention but not to be limited, although be described in detail the embodiment of the present invention with reference to preferred embodiment, those of ordinary skill in the art is to be understood that and still can modifies to the technical scheme of the embodiment of the present invention or equivalent replacement, and these are revised or be equal to the scope that replacement also can not make amended technical scheme disengaging embodiment of the present invention technical scheme.
Claims (9)
1. the yellow ceramic pigment of small particle size praseodymium zirconium, is characterized in that: the component of the yellow ceramic pigment of described praseodymium zirconium and weight percent corresponding to component are Praseodymium trioxide 3-6%, zirconium white 48-62%, silicon-dioxide 30-38%, mineralizer 3-8%;
Wherein zirconium white selects the product not removing hafnium element in zirconium white production process, and wherein zirconium white is greater than 40:1 with the atomic molar ratio of hafnium element;
Silicon-dioxide selects aerosil, and its BET specific surface area is 500-800m
2/ g, median size is 3-8 μm, and volume of voids is 3-5.
2. the yellow ceramic pigment of praseodymium zirconium according to claim 1, is characterized in that: silicon-dioxide selects median size to be the ultra-fine quartz of 1-5 μm.
3. the yellow ceramic pigment of praseodymium zirconium according to claim 1, is characterized in that: the component of the yellow ceramic pigment of described praseodymium zirconium and weight percent corresponding to component are Praseodymium trioxide 3.5-4%, zirconium white 58-62%, aerosil 30-35%, mineralizer 3-6%.
4. the yellow ceramic pigment of praseodymium zirconium according to claim 1-3, it is characterized in that: described mineralizer is the mixture of ammonium chloride, barium fluoride and potassium silicofluoride, its weight ratio is ammonium chloride 1: barium fluoride 2: potassium silicofluoride 1.5.
5. the yellow ceramic pigment of praseodymium zirconium according to claim 3, it is characterized in that: described mineralizer is the mixture of ammonium chloride, Sodium Fluoride and Sodium Silicofluoride, its weight ratio is ammonium chloride 1: Sodium Fluoride 2: Sodium Silicofluoride 1.5.
6. the yellow ceramic pigment of praseodymium zirconium according to claim 1, is characterized in that: also can add the cerium oxide or yttrium oxide that mass percent is 0.5-1% in the yellow ceramic pigment of described praseodymium zirconium.
7. prepare a method for the yellow ceramic pigment of praseodymium zirconium as claimed in claim 1, it is characterized in that:
Step one, by Praseodymium trioxide, zirconium white, aerosil and mineralizer raw material pulverizing, to be ground to particle diameter be 1-3 μm, mixes after oven dry;
Step 2, is positioned over the raw material mixed in saggar and calcines, and calcining temperature is 1000-1200 DEG C, and the time controling of temperature-rise period is 2-3h, and temperature is incubated 2-3h after rising to calcining temperature, and that takes out that namely saggar obtain the yellow ceramic pigment of praseodymium zirconium burns till product;
Step 3, will burn till product grinding evenly in step 2, by washed with de-ionized water 3-4 time, dries, obtains required praseodymium zirconium Huang ceramic pigment.
8. the method utilizing the yellow ceramic pigment of praseodymium zirconium as claimed in claim 7 to prepare ceramic ink, it is characterized in that: yellow for praseodymium zirconium ceramic pigment is added in the solvent of ceramic ink with weight percent 20-40%, after mixing, this ink is ground to colorant particle diameter and is less than 1 μm and namely obtains required ink.
9. the preparation method of ceramic ink according to claim 8, is characterized in that: the yellow ceramic pigment of praseodymium zirconium is added in the solvent of ceramic ink with weight percent 35-40%.
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| CN105753324A (en) * | 2016-01-23 | 2016-07-13 | 景德镇陶瓷学院 | Method for preparing high-alkali-resistance ceramic overglaze color fluxing agent by milling addition of silica sol |
| CN105753325A (en) * | 2016-01-23 | 2016-07-13 | 景德镇陶瓷学院 | Decoration method for ceramic over-glaze pigment with high alkali resistance |
| CN107298896A (en) * | 2017-06-22 | 2017-10-27 | 安徽省德邦瓷业有限公司 | A kind of preparation method of domestic ceramics Yellow ceramic ink |
| CN108892381A (en) * | 2018-07-26 | 2018-11-27 | 湖南省醴陵市楚华陶瓷实业有限公司 | A kind of preparation method of seven color pearl glaze and seven color pearl glazes |
| CN110025101A (en) * | 2019-03-29 | 2019-07-19 | 何胜利 | A kind of mineral element solution and its application in tcrude ore processing |
| CN111548650A (en) * | 2020-05-11 | 2020-08-18 | 佛山市利德嘉陶瓷制釉有限公司 | Ceramic pigment formula with good colorability and preparation method thereof |
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| CN105753324A (en) * | 2016-01-23 | 2016-07-13 | 景德镇陶瓷学院 | Method for preparing high-alkali-resistance ceramic overglaze color fluxing agent by milling addition of silica sol |
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| CN108892381A (en) * | 2018-07-26 | 2018-11-27 | 湖南省醴陵市楚华陶瓷实业有限公司 | A kind of preparation method of seven color pearl glaze and seven color pearl glazes |
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