CN105777196B - A kind of preparation method of high temperature resistant and the good pr-yellow material of coloring - Google Patents

A kind of preparation method of high temperature resistant and the good pr-yellow material of coloring Download PDF

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CN105777196B
CN105777196B CN201610167699.XA CN201610167699A CN105777196B CN 105777196 B CN105777196 B CN 105777196B CN 201610167699 A CN201610167699 A CN 201610167699A CN 105777196 B CN105777196 B CN 105777196B
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electric
melting
zirconia
melting zirconia
yellow material
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CN105777196A (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 present invention relates to a kind of high temperature resistant and the preparation methods of the good pr-yellow material of coloring, it first passes through grinding and homogenizing processing controls the grain composition of electric-melting zirconia in the reasonable scope, improve the specific surface area of electric-melting zirconia, suitable reactive adhesive is added again to close admittedly therewith, improve the reactivity of electric-melting zirconia, to obtain specific surface area with reactivity close to the modification electric-melting zirconia of chemical zirconium, the ceramic pigment produced using the heat resist modification electric-melting zirconia, the refractory ceramics colorant that temperature tolerance is prepared close to chemical zirconium, chemical zirconium production refractory ceramics colorant can be substituted completely, it overcomes electric-melting zirconia and applies bottleneck in high-end ceramic pigment field, reduce the production cost of refractory ceramics colorant.

Description

A kind of preparation method of high temperature resistant and the good pr-yellow material of coloring
This case is with the applying date for 2014-12-05, application No. is 201410738251.X, a kind of entitled " modified electric smelting The divisional application that the patent of invention of the preparation method of zirconium oxide and pr-yellow material " carries out for female case.
Technical field
The present invention relates to technical field of inorganic material, the system of specifically a kind of high temperature resistant and the good pr-yellow material of coloring Preparation Method.
Background technology
China is the big producer of ceramics, is used in body stain in ceramic common glaze, zirconium system colorant occupies importantly Position, 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 electricity The high-temperature stability of the quality especially colorant of molten zirconium oxide directly influences the quality of the zirconium vanadium blue produced and zirconium praseodymium yellow.Mesh The preceding ceramic pigment produced using electric-melting zirconia such as pr-yellow material, fade width when being used under 1200 DEG C of temperatures above environment Degree is big, tinting strength, tinting power is weak, and the using effect of the ceramic pigment with chemical zirconium production is not achieved, i.e., the performance ratio chemistry in terms of temperature tolerance Zirconium is poor, cannot be used in high-end ceramic pigment field.
Invention content
It has been investigated that using the ceramic pigment such as pr-yellow material of electric-melting zirconia production, why temperature tolerance is poor at present, Reason is that the specific surface area of electric-melting zirconia powder is small, reactivity is small, causes coloring element in colorant building-up process cannot be complete In full packing to lattice, the tinting strength, tinting power of ceramic pigment is made to die down, is easy to fade in applied at elevated temperature, heat resistance is deteriorated.
It analyzes for these reasons, in order to overcome the deficiencies of existing technologies, the technical problem to be solved by the present invention is to carry For a kind of preparation method producing temperature tolerance and the good pr-yellow material of coloring using electric-melting zirconia.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention one is:
A kind of preparation method of modified electric-melting zirconia, including:
The zirconia powder for being 3~5 μm at granularity by electric-melting zirconia particulate abrasive;
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enters water quick cooling, is washed to neutral, baking Dry, grinding, obtains the reactive adhesive that particle diameter is 1-1.5 μm, and the high temperature melting temperature is 1400 DEG C;
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture Then 0.2wt% handles 20h under 300 DEG C, 3MPa, obtain modified electric-melting zirconia.
The preparation method of modified electric-melting zirconia provided by the present invention, has the advantages that:Using present invention side The modification electric-melting zirconia that method is prepared, for specific surface area with reactivity close to chemical zirconium, alternative chemistry zirconium production is resistance to High temperature pigment of ceramic meets the requirement of high-end ceramic pigment, reduces the production cost of refractory ceramics colorant.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention two is:
A kind of preparation method of pr-yellow material, including:
The zirconia powder for being 3~5 μm at granularity by electric-melting zirconia particulate abrasive;
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enters water quick cooling, is washed to neutral, baking Dry, grinding, obtains the reactive adhesive that particle diameter is 1-1.5 μm, and the high temperature melting temperature is 1400 DEG C;
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture Then 0.2wt% handles 20h under 300 DEG C, 3MPa, obtain modified electric-melting zirconia;
Other auxiliary materials of modified electric-melting zirconia and pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies oxic gas It is calcined with the heating rate of 180 DEG C/h under atmosphere, 3h is kept the temperature when calcination temperature reaches 1050 DEG C, then cooling down, grinding, water It washes, dry, obtain pr-yellow material.
The preparation method of pr-yellow material provided by the present invention, has the advantages that:It is prepared using the method for the present invention Obtained pr-yellow material, good using not fugitive color, tinting strength, tinting power under 1200 DEG C of temperatures above environment, the close chemical zirconium system of temperature tolerance Standby high temperature resistant pr-yellow material overcomes electric-melting zirconia and applies bottleneck in high-end ceramic pigment field, reduces high temperature resistant The production cost of ceramic pigment.
Description of the drawings
Fig. 1 show the preparation technology flow chart of the modification 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.
Specific implementation mode
To explain the technical content, the achieved purpose and the effect of the present invention in detail, below in conjunction with embodiment and coordinate attached Figure is explained.
The design of most critical of the present invention is:It first passes through grinding and homogenizing processing controls the grain composition of electric-melting zirconia In the reasonable scope, the specific surface area of electric-melting zirconia is improved, then adds suitable reactive adhesive and closes admittedly therewith, improves electric smelting The reactivity of zirconium oxide is aoxidized close to the heat resist modification electric smelting of chemical zirconium to obtain specific surface area with reactivity Zirconium, the ceramic pigment produced using the modification electric-melting zirconia, the refractory ceramics color that temperature tolerance is prepared close to chemical zirconium Material can substitute chemical zirconium production refractory ceramics colorant, overcome electric-melting zirconia answering in high-end ceramic pigment field completely With bottleneck, the production cost of refractory ceramics colorant is reduced.
Specifically, please refer to shown in Fig. 1, the preparation method of the modification electric-melting zirconia of the embodiment of the present invention, including:
The zirconia powder for being 3~5 μm at granularity by electric-melting zirconia particulate abrasive;
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enters water quick cooling, is washed to neutral, baking Dry, grinding, obtains the reactive adhesive that particle diameter is 1-1.5 μm, and the high temperature melting temperature is 1400 DEG C;
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture Then 0.2wt% handles 20h under 300 DEG C, 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 by laser Particle size analyzer carries out observation control.
As can be seen from the above description, the preparation method of modified electric-melting zirconia provided by the invention, advantage are:It adopts The modification electric-melting zirconia being prepared with the method for the present invention, specific surface area and the close chemical zirconium of reactivity, alternativeization It learns zirconium and produces refractory ceramics colorant, meet the requirement of high-end ceramic pigment, reduce being produced into for refractory ceramics colorant This.
Further, electric-melting zirconia particle also passes through homogenizing and handles after grinding, makes the powder granularity of electric-melting zirconia Tend to concentrate, be uniformly distributed, improves its specific surface area.
Specifically, please referring to shown in Fig. 2, the preparation side of the good pr-yellow material of high temperature resistant and coloring of the embodiment of the present invention Method, including:
The zirconia powder for being 3~5 μm at granularity by electric-melting zirconia particulate abrasive;
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enters water quick cooling, is washed to neutral, baking Dry, grinding, obtains the reactive adhesive that particle diameter is 1-1.5 μm, and the high temperature melting temperature is 1400 DEG C;
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture Then 0.2wt% handles 20h under 300 DEG C, 3MPa, obtain modified electric-melting zirconia.
Other auxiliary materials of modified electric-melting zirconia and pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies oxic gas It is calcined with the heating rate of 180 DEG C/h under atmosphere, 3h is kept the temperature when calcination temperature reaches 1050 DEG C, then cooling down, grinding, water It washes, dry, 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 by laser Particle size analyzer carries out observation control.
Seen from the above description, the preparation method of pr-yellow material provided by the invention, advantage are:Using this hair The pr-yellow material that bright method is prepared, good using not fugitive color, tinting strength, tinting power under 1200 DEG C of temperatures above environment, temperature tolerance connects High temperature resistant pr-yellow material prepared by nearly chemistry zirconium overcomes electric-melting zirconia in the bottleneck of applying in high-end ceramic pigment field, drop The low production cost of refractory ceramics colorant.
Further, electric-melting zirconia particle also passes through homogenizing and handles after grinding, makes the powder granularity of electric-melting zirconia Tend to concentrate, be uniformly distributed, improves its specific surface area.
Specific embodiment
The zirconia powder for being 3~5 μm at granularity by electric-melting zirconia particulate abrasive;
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enters water quick cooling, is washed to neutral, baking Dry, grinding, obtains the reactive adhesive that particle diameter is 1-1.5 μm, and the high temperature melting temperature is 1400 DEG C;
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture 0.2wt% handles 20h under 300 DEG C, 3MPa, and zirconia powder and reactive adhesive is made to be fully bonded to together, improve electric smelting oxygen The reactivity for changing zirconium obtains modified electric-melting zirconia;
Other auxiliary materials of modified electric-melting zirconia and pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies oxic gas It is calcined with the heating rate of 180 DEG C/h under atmosphere, 3h is kept the temperature when calcination temperature reaches 1050 DEG C, then cooling down, grinding, water It washes, dry, obtain pr-yellow material.
Modification electric-melting zirconia (2#), the preceding electric-melting zirconia (1#) of processing and the chemistry that above-described embodiment is prepared Zirconium (3#, 4#) carries out multiple spot BET method and measures specific surface area respectively, 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 it is found that the modification electric-melting zirconia that the present invention is prepared, specific surface area is compared to electric smelting oxygen before processing shown in table 1 Change zirconium to significantly increase, close to the specific surface area of chemistry zirconium.
By the praseodymium yellow that above-described embodiment is prepared pr-yellow material (1#), is produced using electric-melting zirconia before processing Colorant (2#) and the pr-yellow material (3#, 4#) produced using chemical zirconium carry out color development experiment, color development experimental result respectively As shown in table 2 below.
Table 2
From it is found that the pr-yellow material that the present invention is prepared, color development experimental result is compared using electric smelting before processing shown in table 2 The pr-yellow material that zirconium oxide produces is significantly improved effect, and color development aberration is close to the praseodymium produced using chemical zirconium Yellow material.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair Equivalents made by bright specification and accompanying drawing content are applied directly or indirectly in relevant technical field, include similarly In the scope of patent protection of the present invention.

Claims (1)

1. the preparation method of a kind of high temperature resistant and the good pr-yellow material of coloring, which is characterized in that including:
The zirconia powder for being 3~5 μm at granularity by electric-melting zirconia particulate abrasive, the electric-melting zirconia particle are gone back after grinding It is handled by homogenizing;
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enters water quick cooling, be washed to neutrality, dry, grind Mill, obtains the reactive adhesive that particle diameter is 1-1.5 μm, and the high temperature melting temperature is 1400 DEG C;
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is the 0.2wt% of amount of the mixture, so 20h is handled under 300 DEG C, 3MPa afterwards, obtains modified electric-melting zirconia;
Other auxiliary materials of modified electric-melting zirconia and pr-yellow material are sufficiently mixed uniformly, dress alms bowl calorifies under oxidizing atmosphere Calcined with the heating rate of 180 DEG C/h, 3h kept the temperature when calcination temperature reaches 1050 DEG C, then cooling down, grinding, washing, Drying, obtains pr-yellow material.
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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CN201410738251.XA CN104529541B (en) 2014-12-05 2014-12-05 The preparation method of a kind of modification electric-melting zirconia and pr-yellow material

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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

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