CN106830075B - A kind of high-purity zirconic acid calcium material and preparation method thereof - Google Patents
A kind of high-purity zirconic acid calcium material and preparation method thereof Download PDFInfo
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- CN106830075B CN106830075B CN201710100709.2A CN201710100709A CN106830075B CN 106830075 B CN106830075 B CN 106830075B CN 201710100709 A CN201710100709 A CN 201710100709A CN 106830075 B CN106830075 B CN 106830075B
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- acid calcium
- zirconic acid
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- lime stone
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of high-purity zirconic acid calcium materials and preparation method thereof.Its technical solution is：By natural zircon: the mass ratio of silicon powder is (3.15 ~ 3.20): 1 dispensing, and the zircon and the silicon powder are added in blender, stirs 0.2 ~ 0.3 hour, obtains mixture；The mixture is added in electric arc furnaces again, is warming up to 1535 ~ 1670 DEG C, keeps the temperature 20 ~ 30 minutes；Then lime stone is added in into the electric arc furnaces, is warming up to 1960 ~ 2010 DEG C, keep the temperature 20 ~ 30 minutes；Upper strata scum silica frost is removed, cools to room temperature with the furnace to get high-purity zirconic acid calcium material.The mass ratio of the lime stone and the mixture is (1.8 ~ 2.0): 1.The present invention has the characteristics that simple for process and of low cost；Advantages of good crystallization, purity height and the calcium zirconate high conversion rate of prepared high-purity zirconic acid calcium material.
Description
Technical field
The invention belongs to calcium zirconate field of material technology.More particularly to a kind of high-purity zirconic acid calcium material and preparation method thereof.
Background technology
Calcium zirconate（CaZrO3）It is CaO and ZrO2A kind of solid solution that chemical combination is formed under the high temperature conditions, have fusing point it is high,
Corrosion-resistant and mechanical strength it is big etc. it is a series of a little, be widely used in the fields such as structural ceramics, functional material and refractory material.
At present, the preparation method of calcium zirconate mainly includes sintering process and electric smelting method（Summer Wei, the synthesis of zirconic acid calcium material are ground
Study carefully, Liaoning Technology University's master thesis, 2014）.
Calcium zirconate is prepared using sintering process, generally with ZrO2With Ca (OH)2Or CaCO3Deng for raw material（You Jiegang waits " two
Influence of the silica to calcium zirconate material structure and performance ",《Artificial lens journal》, 2014,43 (5)：pp1280~1285）, it is auxiliary
With appropriate SiO2、Al2O3Deng for additive（You Jiegang waits " influence of the aluminium oxide to zirconic acid calcium material the Nomenclature Composition and Structure of Complexes ",《Material
Material heat treatment journal》, 2014,35 (5)：pp39~43）, calcium zirconate is prepared using solid phase reaction.Calcium zirconate is prepared using sintering process
Material, the temperature of solid phase reaction is relatively low, easily leads to that Grain growth is incomplete, and defect is more, the especially introducing of additive
The purity of zirconic acid calcium material is greatly reduced, and then influences the high-temperature behavior of zirconic acid calcium material.
Zirconic acid calcium material is prepared using electric smelting method, generally with natural zircon or baddeleyite etc. for main zirconium source, with reference to stone
Lime stone, white lime or dolomite etc. are calcium source, are aided with fluxing agent and stabilizer etc., in high-temperature electric resistance furnace melting prepare big crystallization and
The zirconic acid calcium material of high-purity.Zirconic acid calcium material, complex technical process, especially fluxing agent, stabilizer are prepared using electric smelting method
The manufacturing cost of zirconic acid calcium material is increased, while also reduce the purity of zirconic acid calcium material with inhibitor etc..
Invention content
The present invention is directed to overcome prior art defect, it is therefore an objective to provide a kind of high-purity zirconic acid simple for process and low-cost
The preparation method of calcium material, with the advantages of good crystallization of high-purity zirconic acid calcium material prepared by this method, purity height and zirconic acid calcium transformation ratio
It is high.
To achieve the above object, the technical solution adopted by the present invention is：By natural zircon: the mass ratio of silicon powder is
(3.15 ~ 3.20): 1 dispensing adds in the zircon and the silicon powder in blender, stirs 0.2 ~ 0.3 hour, is mixed
Close material.The mixture is added in electric arc furnaces again, is warming up to 1535 ~ 1670 DEG C, keeps the temperature 20 ~ 30 minutes；Then to the electricity
Lime stone is added in arc stove, is warming up to 1960 ~ 2010 DEG C, keeps the temperature 20 ~ 30 minutes.Upper strata scum silica frost is finally removed, is cooled to the furnace
Room temperature is to get high-purity zirconic acid calcium material.
The mass ratio of the lime stone and the mixture is (1.8 ~ 2.0): 1.
The ZrSiO of the natural zircon4Content >=92wt%；The granularity of the zircon is 0.1 ~ 1mm.
The SiO of the silicon powder2Content >=95wt%；The granularity of the silicon powder is 0.064 ~ 0.088mm.
The CaCO of the lime stone3Content >=95wt%；The granularity of the lime stone is 0.12 ~ 0.15mm.
Due to the adoption of the above technical scheme, the present invention has the positive effect that compared with prior art：
1st, the present invention uses natural zircon, silicon powder and lime stone as raw material, and do not introduce the fluxing agent of other components
Deng raw material sources enrich, and technical process is simple, reduce the production cost of high-purity zirconic acid calcium material.
2nd, the present invention using raw material components directly in conjunction with solid solution reaction, improve the purity and crystal grain of zirconic acid calcium material
Degree increases the conversion ratio of calcium zirconate.
High-purity zirconic acid calcium material prepared by the present invention is after testing：Zirconic acid calcium transformation ratio is 95 ~ 98%；Grain size is 4 ~ 7 μ
m。
Therefore, the present invention has the characteristics that simple for process and of low cost；The crystallization of prepared high-purity zirconic acid calcium material
Good, purity height and calcium zirconate high conversion rate.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limit of the scope of the present invention
System：
It is first that the material Unify legislation involved by present embodiment is as follows to avoid repeating, it is no longer superfluous in embodiment
It states：
The ZrSiO of the natural zircon4Content >=92wt%；The granularity of the zircon is 0.1 ~ 1mm.
The SiO of the silicon powder2Content >=95wt%；The granularity of the silicon powder is 0.064 ~ 0.088mm.
The CaCO of the lime stone3Content >=95wt%；The granularity of the lime stone is 0.12 ~ 0.15mm.
Embodiment 1
A kind of high-purity zirconic acid calcium material and preparation method thereof.Preparation method is described in the present embodiment：By natural zircon: silicon
The mass ratio of micro mist is (3.15 ~ 3.17): 1 dispensing, and the zircon and the silicon powder are added in blender, stirring 0.2 ~
0.3 hour, obtain mixture.The mixture is added in electric arc furnaces again, is warming up to 1535 ~ 1589 DEG C, keeps the temperature 20 ~ 30 points
Clock；Then lime stone is added in into the electric arc furnaces, is warming up to 1960 ~ 1980 DEG C, keep the temperature 20 ~ 30 minutes.Finally remove upper strata
Scum silica frost cools to room temperature with the furnace to get high-purity zirconic acid calcium material.
The mass ratio of the lime stone and the mixture is (1.8 ~ 1.88): 1.
High-purity zirconic acid calcium material manufactured in the present embodiment is after testing：Zirconic acid calcium transformation ratio is 95 ~ 97%；Grain size is 4 ~ 6 μ
m。
Embodiment 2
A kind of high-purity zirconic acid calcium material and preparation method thereof.Preparation method is described in the present embodiment：By natural zircon: silicon
The mass ratio of micro mist is (3.16 ~ 3.18): 1 dispensing, and the zircon and the silicon powder are added in blender, stirring 0.2 ~
0.3 hour, obtain mixture.The mixture is added in electric arc furnaces again, is warming up to 1562 ~ 1616 DEG C, keeps the temperature 20 ~ 30 points
Clock；Then lime stone is added in into the electric arc furnaces, is warming up to 1970 ~ 1990 DEG C, keep the temperature 20 ~ 30 minutes.Finally remove upper strata
Scum silica frost cools to room temperature with the furnace to get high-purity zirconic acid calcium material.
The mass ratio of the lime stone and the mixture is (1.84 ~ 1.92): 1.
High-purity zirconic acid calcium material manufactured in the present embodiment is after testing：Zirconic acid calcium transformation ratio is 95 ~ 97%；Grain size is 4 ~ 6 μ
m。
Embodiment 3
A kind of high-purity zirconic acid calcium material and preparation method thereof.Preparation method is described in the present embodiment：By natural zircon: silicon
The mass ratio of micro mist is (3.17 ~ 3.19): 1 dispensing, and the zircon and the silicon powder are added in blender, stirring 0.2 ~
0.3 hour, obtain mixture.The mixture is added in electric arc furnaces again, is warming up to 1589 ~ 1643 DEG C, keeps the temperature 20 ~ 30 points
Clock；Then lime stone is added in into the electric arc furnaces, is warming up to 1980 ~ 2000 DEG C, keep the temperature 20 ~ 30 minutes.Finally remove upper strata
Scum silica frost cools to room temperature with the furnace to get high-purity zirconic acid calcium material.
The mass ratio of the lime stone and the mixture is (1.88 ~ 1.96): 1.
High-purity zirconic acid calcium material manufactured in the present embodiment is after testing：Zirconic acid calcium transformation ratio is 96 ~ 98%；Grain size is 5 ~ 7 μ
m。
Embodiment 4
A kind of high-purity zirconic acid calcium material and preparation method thereof.Preparation method is described in the present embodiment：By natural zircon: silicon
The mass ratio of micro mist is (3.18 ~ 3.20): 1 dispensing, and the zircon and the silicon powder are added in blender, stirring 0.2 ~
0.3 hour, obtain mixture.The mixture is added in electric arc furnaces again, is warming up to 1616 ~ 1670 DEG C, keeps the temperature 20 ~ 30 points
Clock；Then lime stone is added in into the electric arc furnaces, is warming up to 1990 ~ 2010 DEG C, keep the temperature 20 ~ 30 minutes.Finally remove upper strata
Scum silica frost cools to room temperature with the furnace to get high-purity zirconic acid calcium material.
The mass ratio of the lime stone and the mixture is (1.92 ~ 2.0): 1.
High-purity zirconic acid calcium material manufactured in the present embodiment is after testing：Zirconic acid calcium transformation ratio is 96 ~ 98%；Grain size is 5 ~ 7 μ
m。
Present embodiment has the positive effect that compared with prior art：
1st, present embodiment uses natural zircon, silicon powder and lime stone as raw material, and does not introduce other components
Fluxing agent etc., raw material sources enrich, and technical process is simple, reduce the production cost of high-purity zirconic acid calcium material.
2nd, present embodiment using raw material components directly in conjunction with solid solution reaction, improve the pure of zirconic acid calcium material
Degree and grain size increase the conversion ratio of calcium zirconate.
High-purity zirconic acid calcium material prepared by present embodiment is after testing：Zirconic acid calcium transformation ratio is 95 ~ 98%；Crystal grain
Spend is 4 ~ 7 μm.
Therefore, present embodiment has the characteristics that simple for process and of low cost；Prepared high-purity calcium zirconate material
Advantages of good crystallization, purity height and the calcium zirconate high conversion rate of material.
Claims (1)
1. a kind of preparation method of high-purity zirconic acid calcium material, it is characterised in that the preparation method is：By natural zircon: silicon is micro-
The mass ratio of powder is (3.15 ~ 3.20): 1 dispensing, and the zircon and the silicon powder are added in blender, stirring 0.2 ~
0.3 hour, obtain mixture；The mixture is added in electric arc furnaces again, is warming up to 1535 ~ 1670 DEG C, keeps the temperature 20 ~ 30 points
Clock；Then lime stone is added in into the electric arc furnaces, is warming up to 1960 ~ 2010 DEG C, keep the temperature 20 ~ 30 minutes；Upper strata scum silica frost is removed,
Room temperature is cooled to the furnace to get high-purity zirconic acid calcium material；
The mass ratio of the lime stone and the mixture is (1.8 ~ 2.0): 1；
The ZrSiO of the natural zircon4Content >=92wt%；The granularity of the zircon is 0.1 ~ 1mm；
The SiO of the silicon powder2Content >=95wt%；The granularity of the silicon powder is 0.064 ~ 0.088mm；
The CaCO of the lime stone3Content >=95wt%；The granularity of the lime stone is 0.12 ~ 0.15mm.
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| CN108726566A (en) * | 2018-07-27 | 2018-11-02 | 孙志成 | A kind of high-purity zirconic acid calcium material and preparation method thereof of low cost |
| CN108546123A (en) * | 2018-07-27 | 2018-09-18 | 孙志成 | A kind of zirconic acid calcium material and preparation method thereof with high-purity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420103A (en) * | 2001-11-21 | 2003-05-28 | 郑州振中电熔锆业有限公司 | Method for producing electric smelting calcium zirconate |
| CN106431370A (en) * | 2016-09-09 | 2017-02-22 | 武汉科技大学 | Mullite raw material adopting alumina-chrome slag as main ingredient and preparation method thereof |
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2017
- 2017-02-23 CN CN201710100709.2A patent/CN106830075B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420103A (en) * | 2001-11-21 | 2003-05-28 | 郑州振中电熔锆业有限公司 | Method for producing electric smelting calcium zirconate |
| CN106431370A (en) * | 2016-09-09 | 2017-02-22 | 武汉科技大学 | Mullite raw material adopting alumina-chrome slag as main ingredient and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 二氧化硅对锆酸钙材料结构及性能的影响;游杰刚等;《人工晶体学报》;20140531;第43卷(第5期);第1280-1285页 * |
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Application publication date: 20170613 Assignee: Wuhan Chuanfu metal materials Co., Ltd Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000002 Denomination of invention: A high purity calcium zirconate material and its preparation method Granted publication date: 20180619 License type: Common License Record date: 20201021 |
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Assignee: Wuhan Chuanfu metal materials Co.,Ltd. Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000002 Date of cancellation: 20220117 |