CN104710192A - Zirconium phosphate high-temperature nickel red ceramic pigment and preparation method thereof - Google Patents

Zirconium phosphate high-temperature nickel red ceramic pigment and preparation method thereof Download PDF

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Publication number
CN104710192A
CN104710192A CN201510115422.8A CN201510115422A CN104710192A CN 104710192 A CN104710192 A CN 104710192A CN 201510115422 A CN201510115422 A CN 201510115422A CN 104710192 A CN104710192 A CN 104710192A
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pigment
high temperature
colorant
red ceramic
drying
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CN104710192B (en
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顾幸勇
范薇
罗婷
董伟霞
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Jingdezhen Ceramic Institute
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Jingdezhen Ceramic Institute
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Abstract

The invention relates to a zirconium phosphate high-temperature nickel red ceramic pigment and a preparation method of the pigment. The pigment employs industrial chemical materials, takes 55-60.8wt% of diammonium phosphate ((NH4)2HPO4) and 39.2-45wt% of zirconium oxide (ZrO2) as major raw materials and 2-7wt% of black nickel oxide (Ni2O3) as a colorant. The high-temperature nickel red ceramic pigment is prepared via burdening, water adding for stirring and mixing, drying, grinding, sieving, roasting, crushing, washing, baking, crushing and drying. The chemical materials adopted by the pigment are low in cost; the obtained nickel red pigment is bright in color and stable in color generation, can be widely used in various high-temperature ceramic products; and at the same time, since zirconium phosphate has small thermal expansivity, belongs to a low-expansion material and is very beneficial for thermal stability of a material applying zirconium phosphate, the pigment has wide application prospects.

Description

A kind of zirconium phosphate type high temperature nickel red ceramic colorant and preparation method thereof
Technical field
The invention belongs to ceramic (pottery) field, specifically a kind of zirconium phosphate type high temperature nickel red ceramic colorant and preparation method thereof.
Background technology
China is the big producing country of domestic ceramics (comprising porcelain) in the world.Also be the big producing country of architectural pottery and snitaryware in the world, according to according to a preliminary estimate, China's ceramic industry every year need glaze stain about 100,000 tons, body stain about 200,000 tons, frit output about 800,000 tons, becomes glaze output to be about 200,000 tons.Demand as can be seen here as the glaze materials of above-mentioned ceramic product finishing material is sizable.Have a lot with the ceramic pigment of redness name in current Production of Ceramics, red ceramic colorant is used widely in Production of Ceramics, red ceramic material is the research emphasis of ceramist always, in decorating ceramic products, have very consequence, its research application has had the history of 1,100; In recent ten years, novel red ceramic pigment constantly occurs, at present, high-temperature red ceramic pigment mainly contains the red and occlusion pigment of chrome alumina red, chrome tin pink, manganese red, cobalt magnesium.Shown by XRD test analysis, chrome alumina red is spinel structure, chrome tin pink is zinntitanite type structure, manganese red is corundum type structure, cobalt magnesium is red belongs to clinoenstatite type structure.Chrome alumina red and chrome tin pink are mainly used in glaze painted, and cobalt magnesium is red is colorant on glaze, and high temperature selenium ruby colorant and manganese red all can obtain good coloring effect in high/low temperature base substrate.Although the kind of red stain is a lot, but great majority are containing toxic element, or many colorants exceed all to decompose at certain temperature or colour generation unstable, a lot of crystal is structural instability unstable properties at high temperature, and the technique for packing being conducive to improving colorant high-temperature stability also needs to improve its encapsulation ratio further.Therefore the red colorant of a kind of new type high temperature is studied just very necessary.
Nickel is the element that a kind of tinting strength is very strong, adopts trace just can produce color.Ni to melt in silicate glaze normally unstable.Its valency variation with temperature and changing, the compound of nickel can generate brown, dark brown, green and blue usually.The compound that can generate red nickel is substantially seldom seen, but the compound mixing the zirconium phosphate synthesis of Ni presents redness, and the zirconium phosphate as carrier has good chemistry, thermostability and physical strength, and its thermal expansivity is minimum, belongs to low-expansion material.Therefore prepare zirconium phosphate type high temperature nickel red ceramic colorant and can solve long-term frustration ceramic industry technical barrier.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of with low cost, technique is simple and easy to control, the zirconium phosphate type high temperature nickel red ceramic colorant of environmental protection and preparation method thereof.
For solving above technical problem, technical scheme of the present invention is: a kind of zirconium phosphate type high temperature nickel red ceramic colorant, is characterized in that: adopt technical grade industrial chemicals, be made up of: Secondary ammonium phosphate ((NH following compositions in weight percentage 4) 2hPO 4) 55 ~ 60.8wt%, zirconium white (ZrO 2) 39.2 ~ 45wt%, additional black nickel oxide (Ni 2o 3) 2 ~ 7wt%.
The preparation method of described zirconium phosphate type high temperature nickel red ceramic colorant, is characterized in that comprising the following steps:
Step one: take raw material DAP, zirconium white by a certain percentage, and to add a certain amount of black nickel oxide be tinting material;
Step 2: add a certain amount of water in the mixture that step one obtains, dry after stirring;
Step 3: mixture grinding step 2 drying obtained is sieved, and is placed in resistance furnace and calcines, and calcining temperature is: 1370 ~ 1420 DEG C, insulation 45 ~ 75min;
Step 4: the colorant after step 3 being calcined is pulverized and ground and wash, after drying, pulverizing, drying, obtains high temperature nickel red ceramic colorant.
The use temperature scope of described obtained high temperature nickel red ceramic colorant is≤1420 DEG C.
The colourimetric number of described obtained high temperature nickel red ceramic colorant is L*=60 ~ 83, a*=16 ~ 24, b*=9 ~ 17.
Researched and analysed by means of testing such as XRD, differential thermal-thermogravimetric curve analyses (TG-DTA) and show: it is Ni when utilizing high temperature that zirconium phosphate type high temperature nickel red ceramic colorant presents red mechanism 2o 3can NiO be resolved into, and NiO, ZrO 2and P 2o 5can react and generate Ni 0.5zr 2(PO 4) 3, Ni again 0.5zr 2(PO 4) 3can caused by the wavelength of reflection Red.Meanwhile, the add-on of black nickel oxide to strictly be controlled, because Ni 0.5zr 2(PO 4) 3formation have sex-limited.
The present invention's advantage compared with the red ceramic pigment of tradition is:
(1) nickel element adopting toxicity little is first that coloring element prepares red ceramic colorant, and both environmental protections, have widened again the range of choice of ceramic pigment color development element;
(2) based on zirconium phosphate, there is phosphoric acid salt Heat stability is good, low expansion, structure intermediate ion replace flexibly, the feature of fast ion conduction and high dissolubility resistent, so be that high temperature decorating colour prepared by carrier has good thermostability with zirconium phosphate;
(3) raw material sources of the present invention are wide, are substantially all common industrial chemicals and cheap, and the colorant colour generation of acquisition is bright-coloured, stable, can be widely used in, in all kinds of pyroceramic product, therefore having wide market outlook.
Accompanying drawing explanation
Fig. 1 embodiment 2 prepares the XRD test result of high temperature nickel red ceramic colorant;
Fig. 2 embodiment 3 prepares the TG-DTA test curve of high temperature nickel red ceramic colorant.
Embodiment
Embodiment 1:
Take raw material 15g, by Secondary ammonium phosphate ((NH 4) 2hPO 4) 55.8%, zirconium white (ZrO 2) 44.2%, additional black nickel oxide (Ni 2o 3) 2% ratio, the then drying that stirs of adding water obtains mixture; The grinding of the mixture of acquisition sieved, and be placed in resistance furnace and calcine, calcining temperature is: 1370 DEG C, and soaking time is 75min; Colorant after calcining is pulverized and is ground and wash, pulverizing after drying, drying, obtains the high temperature nickel red ceramic colorant that use temperature scope is≤1370 DEG C.
Embodiment 2:
Take raw material 15g, by Secondary ammonium phosphate ((NH 4) 2hPO 4) 58.8%, zirconium white (ZrO 2) 41.2%, additional black nickel oxide (Ni 2o 3) 4% add water the then drying that stirs of ratio obtain mixture; The grinding of the mixture of acquisition sieved, and be placed in resistance furnace and calcine, calcining temperature is: 1400 DEG C, and soaking time is 60min; Colorant after calcining is pulverized and is ground and wash, pulverizing after drying, drying, and obtain the high temperature nickel red ceramic colorant that use temperature scope is≤1400 DEG C, its XRD test result as shown in Figure 1.
Embodiment 3:
Take raw material 15g, by Secondary ammonium phosphate ((NH 4) 2hPO 4) 58.8%, zirconium white (ZrO 2) 41.2%, additional black nickel oxide (Ni 2o 3) 6% add water the then drying that stirs of ratio obtain mixture; The grinding of the mixture of acquisition sieved, and be placed in resistance furnace and calcine, calcining temperature is: 1400 DEG C, and soaking time is 60min; Colorant after calcining is pulverized and is ground and wash, pulverizing after drying, drying, and obtain the high temperature nickel red ceramic colorant that use temperature scope is≤1400 DEG C, its TG-DTA test curve as shown in Figure 2.
Embodiment 4:
Take raw material 15g, by Secondary ammonium phosphate ((NH 4) 2hPO 4) 60.8%, zirconium white (ZrO 2) 39.2%, additional black nickel oxide (Ni 2o 3) 7% add water the then drying that stirs of ratio obtain mixture; The grinding of the mixture of acquisition sieved, and be placed in resistance furnace and calcine, calcining temperature is: 1420 DEG C, and soaking time is 45min; Colorant after calcining is pulverized and is ground and wash, pulverizing after drying, drying, obtains the high temperature nickel red ceramic colorant that use temperature scope is≤1420 DEG C.
Adopt the full-automatic whiteness instrument of WSD-3C that Beijing Kang Guang Instrument Ltd. produces, measure the chrominance data values obtained and see the following form:

Claims (4)

1. a zirconium phosphate type high temperature nickel red ceramic colorant, it is characterized in that: adopt technical grade industrial chemicals, be made up of following compositions in weight percentage: Secondary ammonium phosphate 55 ~ 60.8wt%, zirconium white 39.2 ~ 45wt%, additional black nickel oxide 2 ~ 7wt%.
2. the preparation method of zirconium phosphate type high temperature nickel red ceramic colorant according to claim 1, is characterized in that comprising the following steps:
Step one: take raw material DAP, zirconium white by a certain percentage, and to add a certain amount of black nickel oxide be tinting material;
Step 2: add a certain amount of water in the mixture that step one obtains, dry after stirring;
Step 3: mixture grinding step 2 drying obtained is sieved, and is placed in resistance furnace and calcines, and calcining temperature is: 1370 ~ 1420 DEG C, insulation 45 ~ 75min;
Step 4: the colorant after step 3 being calcined is pulverized and ground and wash, after drying, pulverizing, drying, obtains high temperature nickel red ceramic colorant.
3. preparation method according to claim 2, is characterized in that: the use temperature scope of described obtained high temperature nickel red ceramic colorant is≤1420 DEG C.
4. preparation method according to claim 2, is characterized in that: the colourimetric number of described obtained high temperature nickel red ceramic colorant is L*=60 ~ 83, a*=16 ~ 24, b*=9 ~ 17.
CN201510115422.8A 2015-03-17 2015-03-17 A kind of zirconium phosphate type high temperature nickel red ceramic colorant and preparation method thereof Expired - Fee Related CN104710192B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104710192B (en) * 2015-03-17 2016-06-29 景德镇陶瓷大学 A kind of zirconium phosphate type high temperature nickel red ceramic colorant and preparation method thereof
CN110937889A (en) * 2019-12-10 2020-03-31 武汉科技大学 Zirconium phosphate ceramic material and preparation method thereof
CN116462502A (en) * 2022-10-04 2023-07-21 汶川县神州锆业科技有限公司 High-temperature-resistant and electric corrosion-resistant method for special equipment

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1107490A (en) * 1993-10-29 1995-08-30 库克森马西瓷器及材料有限公司 Pigmentary material
CN1227278A (en) * 1997-11-11 1999-09-01 川崎制铁株式会社 Porcelain-enameled steel sheets and frits for enameling

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104710192B (en) * 2015-03-17 2016-06-29 景德镇陶瓷大学 A kind of zirconium phosphate type high temperature nickel red ceramic colorant and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1107490A (en) * 1993-10-29 1995-08-30 库克森马西瓷器及材料有限公司 Pigmentary material
CN1227278A (en) * 1997-11-11 1999-09-01 川崎制铁株式会社 Porcelain-enameled steel sheets and frits for enameling

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
K. KASTHURI RANGAN ETAL.: "AMVMⅢ(P04)3: New Mixed-Metal Phosphates Having NASICON and Related Structures", 《INORG. CHEM.》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104710192B (en) * 2015-03-17 2016-06-29 景德镇陶瓷大学 A kind of zirconium phosphate type high temperature nickel red ceramic colorant and preparation method thereof
CN110937889A (en) * 2019-12-10 2020-03-31 武汉科技大学 Zirconium phosphate ceramic material and preparation method thereof
CN110937889B (en) * 2019-12-10 2022-03-04 武汉科技大学 Zirconium phosphate ceramic material and preparation method thereof
CN116462502A (en) * 2022-10-04 2023-07-21 汶川县神州锆业科技有限公司 High-temperature-resistant and electric corrosion-resistant method for special equipment

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