CN105753510B - A kind of preparation method of heat resist modification electric-melting zirconia and pr-yellow material - Google Patents
A kind of preparation method of heat resist modification electric-melting zirconia and pr-yellow material Download PDFInfo
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- CN105753510B CN105753510B CN201610167886.8A CN201610167886A CN105753510B CN 105753510 B CN105753510 B CN 105753510B CN 201610167886 A CN201610167886 A CN 201610167886A CN 105753510 B CN105753510 B CN 105753510B
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B41/85—Coating or impregnation with inorganic materials
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating 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
- C04B41/5025—Coating 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
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Abstract
The present invention relates to the preparation method of a kind of heat resist modification electric-melting zirconia and pr-yellow material, first pass 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, so as 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, overcome electric-melting zirconia and apply bottleneck in high-end ceramic pigment field, reduce the production cost of refractory ceramics colorant.
Description
This case is the Application No. 201410738251.X using the applying date as 2014-12-05, 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, is specifically a kind of heat resist modification electric-melting zirconia and pr-yellow material
Preparation method.
Background technology
China is the big producer of ceramics, is used in the common glaze of ceramics with body stain, 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
It is preceding using electric-melting zirconia come the ceramic pigment such as pr-yellow material that produces, fade width when being used under 1200 DEG C of temperatures above environment
Degree is big, tinting strength, tinting power is weak, does not reach the using effect of the ceramic pigment produced with chemical zirconium, i.e., the performance ratio chemistry in terms of temperature tolerance
Zirconium is poor, it is impossible to used in high-end ceramic pigment field.
The content of the invention
It has been investigated that why temperature tolerance is poor for the current ceramic pigment such as pr-yellow material using electric-melting zirconia production,
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
Full packing makes the tinting strength, tinting power of ceramic pigment die down into lattice, easily fades in applied at elevated temperature, and heat resistance is deteriorated.
Analyze for these reasons, the defects of in order to overcome the prior art, the technical problems to be solved by the invention are to carry
For a kind of preparation method of specific surface area is big, reactivity is high heat resist modification electric-melting zirconia, and and then provide a kind of resistance to
The preparation method of the good pr-yellow material of warm nature.
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 heat resist modification electric-melting zirconia, including：
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Pass through high temperature melting after alkali metal is mixed with alkaline-earth metal according to the weight ratio of 6~7 ︰ 4~5 successively, enter water urgency
It is cold, be washed to neutral, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is
1200-1400 DEG C, the alkali metal is lithium, sodium or lithium sodium mixture, and the alkaline-earth metal is beryllium, magnesium or magnesium calcium compound；
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive for amount of the mixture 0.05~
0.3wt%, then handles 10-20h under 150-300 DEG C, 1-3MPa, obtains heat resist modification electric-melting zirconia.
The preparation method of heat resist modification electric-melting zirconia provided by the present invention, has the advantages that：Using this
The heat resist modification electric-melting zirconia that inventive method is prepared, its specific surface area and the close chemical zirconium of reactivity, it is alternative
Chemical zirconium produces refractory ceramics colorant, meets the requirement of high-end ceramic pigment, reduces the production of refractory ceramics colorant
Cost.
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：
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Pass through high temperature melting after alkali metal is mixed with alkaline-earth metal according to the weight ratio of 6~7 ︰ 4~5 successively, enter water urgency
It is cold, be washed to neutral, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is
1200-1400 DEG C, the alkali metal is lithium, sodium or lithium sodium mixture, and the alkaline-earth metal is beryllium, magnesium or magnesium calcium compound；
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive for amount of the mixture 0.05~
0.3wt%, then handles 10-20h under 150-300 DEG C, 1-3MPa, obtains heat resist modification electric-melting zirconia.
Heat resist modification electric-melting zirconia is uniformly mixed with other auxiliary materials of pr-yellow material, under oxidizing atmosphere with
The heating rate calcining 6-10h of 150-180 DEG C/h, 1-3h is kept the temperature when calcining heat reaches 950-1050 DEG C, is then cooled down cold
But, grind, wash, drying, obtaining pr-yellow material.
The preparation method of pr-yellow material provided by the present invention, has the advantages that：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, reduce high temperature resistant
The production cost of ceramic pigment.
Brief description of the drawings
Fig. 1 show the preparation technology flow chart of the heat resist 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.
Embodiment
For the technology contents that the present invention will be described in detail, the objects and the effects, below in conjunction with embodiment and coordinate attached
Figure is explained.
The design of most critical of the present invention is：First pass 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, aoxidizes so as to obtain specific surface area with reactivity close to the heat resist modification electric smelting of chemical zirconium
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 completely, overcome electric-melting zirconia answering in high-end ceramic pigment field
With bottleneck, the production cost of refractory ceramics colorant is reduced.
Specifically, refer to shown in Fig. 1, the preparation method of the heat resist modification electric-melting zirconia of the embodiment of the present invention, wrap
Include：
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Pass through high temperature melting after alkali metal is mixed with alkaline-earth metal according to the weight ratio of 6~7 ︰ 4~5 successively, enter water urgency
It is cold, be washed to neutral, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is
1200-1400 DEG C, the alkali metal is lithium, sodium or lithium sodium mixture, and the alkaline-earth metal is beryllium, magnesium or magnesium calcium compound；
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive for amount of the mixture 0.05~
0.3wt%, then handles 10-20h under 150-300 DEG C, 1-3MPa, obtains heat resist modification 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 electric-melting zirconia provided by the invention, its advantage are：Using this
The heat resist modification electric-melting zirconia that inventive method is prepared, its specific surface area and the close chemical zirconium of reactivity, it is alternative
Chemical zirconium produces refractory ceramics colorant, meets the requirement of high-end ceramic pigment, reduces the production of refractory ceramics colorant
Cost.
Further, electric-melting zirconia particle is also handled by homogenizing after grinding, makes the powder granularity of electric-melting zirconia
Tend to concentrate, be uniformly distributed, improve its specific surface area.
Further, the weight ratio of the alkali metal and alkaline-earth metal is 3 ︰ 2.
Specifically, refer to shown in Fig. 2, the preparation method of the pr-yellow material of the embodiment of the present invention, including：
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Pass through high temperature melting after alkali metal is mixed with alkaline-earth metal according to the weight ratio of 6~7 ︰ 4~5 successively, enter water urgency
It is cold, be washed to neutral, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is
1200-1400 DEG C, the alkali metal is lithium, sodium or lithium sodium mixture, and the alkaline-earth metal is beryllium, magnesium or magnesium calcium compound；
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive for amount of the mixture 0.05~
0.3wt%, then handles 10-20h under 150-300 DEG C, 1-3MPa, obtains heat resist modification electric-melting zirconia.
Modified electric-melting zirconia is uniformly mixed with other auxiliary materials of pr-yellow material, with 150- under oxidizing atmosphere
180 DEG C/h heating rate calcining 6-10h, 1-3h is kept the temperature when calcining heat reaches 950-1050 DEG C, then cooling down, grind
Mill, 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 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, its 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 bottleneck of applying of the electric-melting zirconia in high-end ceramic pigment field, drop
The low production cost of refractory ceramics colorant.
Further, electric-melting zirconia particle is also handled by homogenizing after grinding, makes the powder granularity of electric-melting zirconia
Tend to concentrate, be uniformly distributed, improve its specific surface area.
Further, the weight ratio of the alkali metal and alkaline-earth metal is 3 ︰ 2.
Further, holding temperature is 1000 DEG C, keeps the temperature 1-3 hour at such a temperature, i.e., when calcining heat reaches
1-3h is kept the temperature at 1000 DEG C, makes preparation process material reaction complete.
Embodiment 1
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Pass through high temperature melting after lithium is mixed with magnesium according to the weight ratio of 3 ︰ 2 successively, enter water quick cooling, be 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 1200 DEG C；
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture
0.3wt%, then handles 10h under 150 DEG C, 1MPa, makes zirconia powder and reactive adhesive be fully bonded to together, improve electricity
The reactivity of molten zirconium oxide, 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
Calcined under atmosphere with the heating rate of 150 DEG C/h, 1h is kept the temperature when calcining heat reaches 950 DEG C, then takes out, grinds after cooling down
Mill, washing, drying, obtain pr-yellow material.
Embodiment 2
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Pass through high temperature melting after sodium is mixed with beryllium according to the weight ratio of 6 ︰ 5 successively, enter water quick cooling, be 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%, 20h is handled under 300 DEG C, 3MPa, makes zirconia powder and reactive adhesive be fully bonded to together, improve electric smelting oxygen
Change the reactivity of zirconium, 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
Calcined under atmosphere with the heating rate of 180 DEG C/h, 3h is kept the temperature when calcining heat reaches 1050 DEG C, then cooling down, grinding, water
Wash, dry, obtain pr-yellow material.
Embodiment 3
By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；
Successively by high temperature melting, Shui temper after lithium sodium mixture is mixed with magnesium calcium compound according to the weight ratio of 7 ︰ 4
Manage, be washed to neutral, drying, grinding, obtain the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is
1300℃；
The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive is amount of the mixture
0.05wt%, 10h is handled under 200 DEG C, 2MPa, makes zirconia powder and reactive adhesive be fully bonded to together, improve electric smelting
The reactivity of zirconium oxide, 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
Calcined under atmosphere with the heating rate of 160 DEG C/h, 2h is kept the temperature when calcining heat reaches 1000 DEG C, then cooling down, grinding, water
Wash, dry, obtain pr-yellow material.
Modification electric-melting zirconia (2#) that above-described embodiment 1~3 is prepared, before processing electric-melting zirconia (1#) and
Chemical zirconium (3#, 4#) carries out multiple spot BET method measurement 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 |
It was found from shown in table 1, the modification electric-melting zirconia of the invention being prepared, specific surface area compares before processing electric smelting oxygen
Change zirconium to significantly increase, close to the specific surface area of chemistry zirconium.
Pr-yellow material (1#) that above-described embodiment 1~3 is prepared, produced using before processing electric-melting zirconia
Pr-yellow material (2#) and the pr-yellow material (3#, 4#) for using chemical zirconium to produce carry out color development experiment, color development experiment respectively
As a result it is as shown in table 2 below.
Table 2
It was found from shown in table 2, the pr-yellow material of the invention being prepared, color development experimental result is compared and uses before processing electric smelting
The pr-yellow material that zirconium oxide produces is significantly improved effect, its color development aberration is close to the praseodymium produced using chemical zirconium
Yellow material.
The foregoing is merely the embodiment of the present invention, is not intended to limit the scope of the invention, every to utilize this hair
The equivalents that bright specification and accompanying drawing content are made, are directly or indirectly used in relevant technical field, similarly include
In the scope of patent protection of the present invention.
Claims (5)
- A kind of 1. preparation method of heat resist modification electric-melting zirconia, it is characterised in that including：By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；Pass through high temperature melting after alkali metal is mixed with alkaline-earth metal according to the weight ratio of 6~7 ︰ 4~5 successively, enter water quick cooling, water Neutral, drying, grinding are washed till, obtains the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is 1200- 1400 DEG C, the alkali metal is lithium, sodium or lithium sodium mixture, and the alkaline-earth metal is beryllium, magnesium or magnesium calcium compound；The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive for amount of the mixture 0.05~ 0.3wt%, then handles 10-20h under 150-300 DEG C, 1-3MPa, obtains heat resist modification electric-melting zirconia；Wherein, it is described Electric-melting zirconia particle is also handled by homogenizing after grinding.
- 2. the preparation method of heat resist modification electric-melting zirconia according to claim 1, it is characterised in that：The alkali metal Weight ratio with alkaline-earth metal is 3 ︰ 2.
- A kind of 3. preparation method of pr-yellow material, it is characterised in that including：By electric-melting zirconia particulate abrasive into granularity be 3~5 μm of zirconia powder；Pass through high temperature melting after alkali metal is mixed with alkaline-earth metal according to the weight ratio of 6~7 ︰ 4~5 successively, enter water quick cooling, water Neutral, drying, grinding are washed till, obtains the reactive adhesive that particle diameter is 1-1.5 μm, the high temperature melting temperature is 1200- 1400 DEG C, the alkali metal is lithium, sodium or lithium sodium mixture, and the alkaline-earth metal is beryllium, magnesium or magnesium calcium compound；The zirconia powder and reactive adhesive are mixed, the amount of allocating of reactive adhesive for amount of the mixture 0.05~ 0.3wt%, then handles 10-20h under 150-300 DEG C, 1-3MPa, obtains heat resist modification electric-melting zirconia；Heat resist modification electric-melting zirconia is mixed with other auxiliary materials of pr-yellow material, with 150-180 under oxidizing atmosphere DEG C/heating rate of h calcining 6-10h, 1-3h is kept the temperature when calcining heat reaches 950-1050 DEG C, then cooling down, grinding, Washing, drying, obtain pr-yellow material；Wherein, the electric-melting zirconia particle is also handled by homogenizing after grinding.
- 4. the preparation method of pr-yellow material according to claim 3, it is characterised in that：The alkali metal and alkaline-earth metal Weight ratio is 3 ︰ 2.
- 5. the preparation method of pr-yellow material according to claim 3, it is characterised in that：When calcining heat reaches 1000 DEG C Keep the temperature 1-3h.
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| CN201610167886.8A CN105753510B (en) | 2014-12-05 | 2014-12-05 | A kind of preparation method of heat resist modification electric-melting zirconia and pr-yellow material |
| 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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|---|---|---|---|---|
| CN1126463A (en) * | 1993-06-30 | 1996-07-10 | 技术资源有限公司 | Zirconia based opacifiers |
| CN101792179A (en) * | 2010-02-11 | 2010-08-04 | 王必庆 | Production method of electrically melt yttrium oxide stabilized zirconia granulation powder |
| WO2010135278A1 (en) * | 2009-05-21 | 2010-11-25 | Robert Barry | Solvent-based surface coating |
| CN102173867A (en) * | 2011-01-28 | 2011-09-07 | 福建三祥工业新材料有限公司 | Method for preparing zirconium iron pink pigment from electrically-melted zirconium oxide |
-
2014
- 2014-12-05 CN CN201610167886.8A patent/CN105753510B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1126463A (en) * | 1993-06-30 | 1996-07-10 | 技术资源有限公司 | Zirconia based opacifiers |
| WO2010135278A1 (en) * | 2009-05-21 | 2010-11-25 | Robert Barry | Solvent-based surface coating |
| CN101792179A (en) * | 2010-02-11 | 2010-08-04 | 王必庆 | Production method of electrically melt yttrium oxide stabilized zirconia granulation powder |
| CN102173867A (en) * | 2011-01-28 | 2011-09-07 | 福建三祥工业新材料有限公司 | Method for preparing zirconium iron pink pigment from electrically-melted zirconium oxide |
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