CN105777196A - High-temperature-resistant high-colorability praseodymium yellow material preparation method - Google Patents

High-temperature-resistant high-colorability praseodymium yellow material preparation method Download PDF

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CN105777196A
CN105777196A CN201610167699.XA CN201610167699A CN105777196A CN 105777196 A CN105777196 A CN 105777196A CN 201610167699 A CN201610167699 A CN 201610167699A CN 105777196 A CN105777196 A CN 105777196A
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zirconia
melting
temperature
electric
yellow material
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CN105777196B (en
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程诗忠
包晓刚
陈美育
李有成
李小毅
陈清华
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SANXIANG ADVANCED MATERIALS CO Ltd
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SANXIANG ADVANCED MATERIALS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5042Zirconium oxides or zirconates; Hafnium oxides or hafnates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to a high-temperature-resistant high-colorability praseodymium yellow material preparation method. By grinding and homogenizing, grain composition of electrically fused zirconia is controlled in a reasonable range to increase the specific surface area of the electrically fused zirconia; appropriate active adhesives are added and fixed to the electrically fused zirconia to improve reaction activity of the electrically fused zirconia, so that modified electrically fused zirconia approximate to chemical zirconium in specific surface area and reaction activity is obtained. Temperature resistance of ceramic pigments prepared from the high-temperature-resistant modified electrically fused zirconia is approximate to that of high-temperature-resistant ceramic pigments prepared from chemical zirconium, so that the high-temperature-resistant modified electrically fused zirconia can completely substitute for chemical zirconium in production of the high-temperature-resistant ceramic pigments. An application bottleneck of the electrically fused zirconia in the field of high-end ceramic pigments is overcome, and production cost of the high-temperature-resistant ceramic pigments is reduced.

Description

A kind of preparation method of high temperature resistant and pr-yellow material that coloring is good
This case is with the applying date for 2014-12-05, and application number is 201410738251.X, and name is called that the patent of invention of " preparation method of a kind of modified electric-melting zirconia and pr-yellow material " is the divisional application that female case carries out.
Technical field
The present invention relates to technical field of inorganic material, the preparation method of specifically a kind of high temperature resistant and pr-yellow material that coloring is good.
Background technology
China is the big producing country of pottery, uses with in body stain at the glaze that pottery is conventional, and zirconium system colorant occupies critical role, such as zirconium system three primary colors colorant zirconium vanadium blue (Zr, V) SiO4, zirconium praseodymium yellow (Zr, Pr) SiO4, zirconium iron pink (Zr, Fe) SiO4, therefore the high-temperature stability of the quality of electric-melting zirconia especially colorant directly influences the zirconium vanadium blue produced and the quality of zirconium praseodymium yellow.Adopt the ceramic pigment such as pr-yellow material that electric-melting zirconia produces at present, fading when using under 1200 DEG C of temperatures above environment, amplitude is big, tinting strength, tinting power is weak, do not reach the result of use of the ceramic pigment produced with chemistry zirconium, namely the performance of temperature tolerance aspect is poorer than chemical zirconium, it is impossible to be used in high-end ceramic pigment field.
Summary of the invention
It has been investigated that, why temperature tolerance is poor for the ceramic pigment such as pr-yellow material that employing electric-melting zirconia produces at present, reason is in that the specific surface area of electric-melting zirconia powder is little, reactivity is little, cause coloring element in colorant building-up process can not be filled up completely with in lattice, the tinting strength, tinting power making ceramic pigment dies down, easily fading when applied at elevated temperature, heat resistance is deteriorated.
Analyzing for these reasons, in order to overcome the defect of prior art, the technical problem to be solved is to provide and a kind of adopts electric-melting zirconia to produce temperature tolerance and the preparation method of the good pr-yellow material of coloring.
In order to solve above-mentioned technical problem, the technical solution used in the present invention one is:
A kind of preparation method of modified electric-melting zirconia, including:
The zirconia powder becoming granularity to be 3~5 μm electric-melting zirconia particulate abrasive;
Sequentially pass through high temperature melting after being mixed according to the weight ratio of 65 with beryllium by sodium, enter water quick cooling, be washed to neutrality, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, described high temperature melting temperature is 1400 DEG C;
Described zirconia powder and reactive adhesive being mixed, the amount of allocating into of reactive adhesive is the 0.2wt% of amount of the mixture, then in 300 DEG C, process 20h under 3MPa, obtain modified electric-melting zirconia.
The preparation method of modified electric-melting zirconia provided by the present invention, have the advantages that the modified electric-melting zirconia adopting the inventive method to prepare, its specific surface area and reactivity close chemistry zirconium, alternative chemistry zirconium produces refractory ceramics colorant, meet the instructions for use of high-end ceramic pigment, reduce the production cost of refractory ceramics colorant.
In order to solve above-mentioned technical problem, the technical solution used in the present invention two is:
A kind of preparation method of pr-yellow material, including:
The zirconia powder becoming granularity to be 3~5 μm electric-melting zirconia particulate abrasive;
Sequentially pass through high temperature melting after being mixed according to the weight ratio of 65 with beryllium by sodium, enter water quick cooling, be washed to neutrality, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, described high temperature melting temperature is 1400 DEG C;
Described zirconia powder and reactive adhesive being mixed, the amount of allocating into of reactive adhesive is the 0.2wt% of amount of the mixture, then in 300 DEG C, process 20h under 3MPa, obtain modified electric-melting zirconia;
Other auxiliary materials of modified electric-melting zirconia Yu pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies to be calcined with the heating rate of 180 DEG C/h under oxidizing atmosphere, the insulation 3h when calcining heat reaches 1050 DEG C, then cooling down, grinding, washing, drying, obtain pr-yellow material.
The preparation method of pr-yellow material provided by the present invention, have the advantages that the pr-yellow material adopting the inventive method to prepare, use not fugitive color, tinting strength, tinting power good under 1200 DEG C of temperatures above environment, the high temperature resistant pr-yellow material that temperature tolerance is prepared close to chemistry zirconium, overcome the electric-melting zirconia application bottleneck in high-end ceramic pigment field, reduce the production cost of refractory ceramics colorant.
Accompanying drawing explanation
Fig. 1 show the preparation technology flow chart of the modified electric-melting zirconia of the embodiment of the present invention.
Fig. 2 show the preparation technology flow chart of the pr-yellow material of the embodiment of the present invention.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, below in conjunction with embodiment and coordinate accompanying drawing to be explained.
The design of most critical of the present invention is in that: first pass through grinding and homogenizing processes and the grain composition of electric-melting zirconia controlled in the reasonable scope, improve the specific surface area of electric-melting zirconia, add suitable reactive adhesive more admittedly to close with it, improve the reactivity of electric-melting zirconia, thus obtaining specific surface area with reactivity all close to the heat resist modification electric-melting zirconia of chemistry zirconium, this modified electric-melting zirconia is utilized to produce the ceramic pigment obtained, the refractory ceramics color material that temperature tolerance is prepared close to chemistry zirconium, chemistry zirconium can be substituted completely and produce refractory ceramics color material, overcome the electric-melting zirconia application bottleneck in high-end ceramic pigment field, reduce the production cost of refractory ceramics colorant.
Concrete, refer to shown in Fig. 1, the preparation method of the modified electric-melting zirconia of the embodiment of the present invention, including:
The zirconia powder becoming granularity to be 3~5 μm electric-melting zirconia particulate abrasive;
Sequentially pass through high temperature melting after being mixed according to the weight ratio of 65 with beryllium by sodium, enter water quick cooling, be washed to neutrality, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, described high temperature melting temperature is 1400 DEG C;
Described zirconia powder and reactive adhesive being mixed, the amount of allocating into of reactive adhesive is the 0.2wt% of amount of the mixture, then in 300 DEG C, process 20h under 3MPa, obtain modified electric-melting zirconia.
In the above-described embodiments, the specific surface area of zirconia powder can be measured by multiple spot BET method, and granularity can be undertaken observing control by laser particle analyzer.
Known from the above, the preparation method of modified electric-melting zirconia provided by the invention, it has the beneficial effects that: adopt the modified electric-melting zirconia that the inventive method prepares, its specific surface area and reactivity close chemistry zirconium, alternative chemistry zirconium produces refractory ceramics colorant, meet the instructions for use of high-end ceramic pigment, reduce the production cost of refractory ceramics colorant.
Further, electric-melting zirconia granule also processes through homogenizing after grinding, makes the powder granularity of electric-melting zirconia tend to concentrating, being uniformly distributed, improves its specific surface area.
Concrete, refer to shown in Fig. 2, the preparation method of the pr-yellow material that the high temperature resistant and coloring of the embodiment of the present invention is good, including:
The zirconia powder becoming granularity to be 3~5 μm electric-melting zirconia particulate abrasive;
Sequentially pass through high temperature melting after being mixed according to the weight ratio of 65 with beryllium by sodium, enter water quick cooling, be washed to neutrality, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, described high temperature melting temperature is 1400 DEG C;
Described zirconia powder and reactive adhesive being mixed, the amount of allocating into of reactive adhesive is the 0.2wt% of amount of the mixture, then in 300 DEG C, process 20h under 3MPa, obtain modified electric-melting zirconia.
Other auxiliary materials of modified electric-melting zirconia Yu pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies to be calcined with the heating rate of 180 DEG C/h under oxidizing atmosphere, the insulation 3h when calcining heat reaches 1050 DEG C, then cooling down, grinding, washing, drying, obtain pr-yellow material.
In the above-described embodiments, the specific surface area of zirconia powder can be measured by multiple spot BET method, and granularity can be undertaken observing control by laser particle analyzer.
Seen from the above description, the preparation method of pr-yellow material provided by the invention, it has the beneficial effects that: adopt the pr-yellow material that the inventive method prepares, use not fugitive color, tinting strength, tinting power good under 1200 DEG C of temperatures above environment, the high temperature resistant pr-yellow material that temperature tolerance is prepared close to chemistry zirconium, overcome the electric-melting zirconia application bottleneck in high-end ceramic pigment field, reduce the production cost of refractory ceramics colorant.
Further, electric-melting zirconia granule also processes through homogenizing after grinding, makes the powder granularity of electric-melting zirconia tend to concentrating, being uniformly distributed, improves its specific surface area.
Specific embodiment
The zirconia powder becoming granularity to be 3~5 μm electric-melting zirconia particulate abrasive;
Sequentially pass through high temperature melting after being mixed according to the weight ratio of 65 with beryllium by sodium, enter water quick cooling, be washed to neutrality, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, described high temperature melting temperature is 1400 DEG C;
Described zirconia powder and reactive adhesive are mixed, the amount of allocating into of reactive adhesive is the 0.2wt% of amount of the mixture, in 300 DEG C, process 20h under 3MPa, make together with zirconia powder is fully bonded to reactive adhesive, improve the reactivity of electric-melting zirconia, obtain modified electric-melting zirconia;
Other auxiliary materials of modified electric-melting zirconia Yu pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies to be calcined with the heating rate of 180 DEG C/h under oxidizing atmosphere, the insulation 3h when calcining heat reaches 1050 DEG C, then cooling down, grinding, washing, drying, obtain pr-yellow material.
The modified electric-melting zirconia (2#), the front electric-melting zirconia (1#) of process and chemistry zirconium (3#, 4#) that are prepared by above-described embodiment carry out multiple spot BET method respectively and measure specific surface area, and measurement result is as shown in table 1 below.
Table 1
Sample ID BET specific surface area (m2/g)
1# 2.03
2# 2.38
3# 2.41
4# 2.43
From shown in table 1 it can be seen that the modified electric-melting zirconia for preparing of the present invention, before specific surface area compares process, electric-melting zirconia significantly increases, close to the specific surface area of chemistry zirconium.
The pr-yellow material (1#), the front electric-melting zirconia of employing process that are prepared by above-described embodiment produce the pr-yellow material (2#) obtained and adopt the pr-yellow material (3#, 4#) that chemistry zirconium production obtains to carry out color development experiment respectively, and color development experimental result is as shown in table 2 below.
Table 2
From shown in table 2 it can be seen that the pr-yellow material for preparing of the present invention, color development experimental result is compared electric-melting zirconia before employing processes and is produced the pr-yellow material obtained and be significantly improved effect, and its color development aberration produces the pr-yellow material obtained close to adopting chemistry zirconium.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalents utilizing description of the present invention and accompanying drawing content to make, or directly or indirectly it is used in relevant technical field, all in like manner include in the scope of patent protection of the present invention.

Claims (2)

1. one kind high temperature resistant and the preparation method of pr-yellow material that coloring is good, it is characterised in that including:
The zirconia powder becoming granularity to be 3~5 μm electric-melting zirconia particulate abrasive;
Sequentially pass through high temperature melting after being mixed according to the weight ratio of 65 with beryllium by sodium, enter water quick cooling, be washed to neutrality, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, described high temperature melting temperature is 1400 DEG C;
Described zirconia powder and reactive adhesive being mixed, the amount of allocating into of reactive adhesive is the 0.2wt% of amount of the mixture, then in 300 DEG C, process 20h under 3MPa, obtain modified electric-melting zirconia;
Other auxiliary materials of modified electric-melting zirconia Yu pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies to be calcined with the heating rate of 180 DEG C/h under oxidizing atmosphere, the insulation 3h when calcining heat reaches 1050 DEG C, then cooling down, grinding, washing, drying, obtain pr-yellow material.
2. the preparation method of according to claim 1 high temperature resistant and pr-yellow material that coloring is good, it is characterised in that: described electric-melting zirconia granule also processes through homogenizing after grinding.
CN201610167699.XA 2014-12-05 2014-12-05 A kind of preparation method of high temperature resistant and the good pr-yellow material of coloring Active CN105777196B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111196898A (en) * 2020-01-08 2020-05-26 佛山市大千色釉料有限公司 Eutectic synthetic zirconium praseodymium yellow material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101381245A (en) * 2008-10-20 2009-03-11 福建三祥工业新材料有限公司 Method for improving electrofusion zirconia chromophoric redness value
CN103145453A (en) * 2013-03-29 2013-06-12 佛山市南海万兴材料科技有限公司 Praseodymium yellow material for ceramic ink and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101381245A (en) * 2008-10-20 2009-03-11 福建三祥工业新材料有限公司 Method for improving electrofusion zirconia chromophoric redness value
CN103145453A (en) * 2013-03-29 2013-06-12 佛山市南海万兴材料科技有限公司 Praseodymium yellow material for ceramic ink and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111196898A (en) * 2020-01-08 2020-05-26 佛山市大千色釉料有限公司 Eutectic synthetic zirconium praseodymium yellow material and preparation method thereof

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