CN111661874A - Method for reducing content of silicon oxide in fused zirconia powder - Google Patents
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 210
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000002844 melting Methods 0.000 claims abstract description 28
- 230000008018 melting Effects 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical group F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 11
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000007602 hot air drying Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 235000003270 potassium fluoride Nutrition 0.000 claims description 4
- 239000011698 potassium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000002912 waste gas Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 238000003723 Smelting Methods 0.000 abstract 2
- 239000007789 gas Substances 0.000 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- 229910004014 SiF4 Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000011819 refractory material Substances 0.000 description 3
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- -1 fluoride ions Chemical class 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a purification technology of electric smelting zirconia powder, in particular to a method for reducing the content of silicon oxide in the electric smelting zirconia powder, which comprises the following steps: step 1, grinding silicon oxide to obtain electric melting zirconia powder; step 2, fully reacting the obtained electric melting zirconia powder with a desilicication solution to obtain zirconia slurry; the silicon reduction acid solution comprises the following components in parts by mass: 100 parts of water, 5-10 parts of concentrated acid and 2-3 parts of fluoride; and 3, filtering, washing and drying the zirconia slurry obtained in the step 2 to obtain the low-silicon electrofusion zirconia powder. The invention has the beneficial effects that: different from the prior art, the method can purify the zirconia with the silicon oxide content of 0.1-0.5% to the silicon oxide content of less than or equal to 0.05%, so that the final zirconia powder has higher purity and more stable quality. And waste gas can be recovered in the production process, the desiliconization acid liquid can be recycled, and the environmental pollution is small.
Description
Technical Field
The invention relates to a purification technology of electric melting zirconia powder, in particular to a method for reducing the content of silicon oxide in the electric melting zirconia powder.
Background
The industrial production of zirconia is widely applied to the fields of refractory materials, ceramic color glaze materials, sponge zirconium and the like, and the main production methods comprise a chemical method and an electric melting method. The electric melting method is characterized in that a zircon sand raw material and a carbon reducing agent are subjected to desiliconization treatment at high temperature in an electric arc furnace, then a zirconium oxide solution is formed by compressed air blowing or casting to obtain an electric melting zirconium oxide product, and then particles or powder with proper granularity requirements are obtained by subsequent finish machining treatment and are applied to related fields.
In the process of producing zirconia by an electric melting method, whether desiliconization completely determines the content of silicon oxide in an electric melting zirconia product, and the lower the content of silicon oxide is, the higher the grade of zirconium oxide is according to different grades of zirconium oxide with different contents of silicon oxide. The content of silicon oxide in the zirconia powder by the electric melting method is usually between 0.1 and 0.5 percent, the difficulty of enabling the content of the silicon oxide to reach within 0.1 percent by only electric melting desiliconization is very large, and the production is extremely unstable.
The content of the silicon oxide in the electric melting zirconia influences the service performance of the refractory material, and also has certain influence on the color development performance of ceramic color glaze, and in the production of ceramic products, the existence of the silicon oxide is easy to generate a glass phase, thereby influencing the appearance and the service performance of products. In the production of commercial zirconium sponge, although the silica will eventually be SiCl4The amount of SiCl is greatly reduced if the silica content in the zirconia is low4The production is more energy-saving and environment-friendly in production.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problems to be solved by the invention are as follows: provides a method for reducing the content of silicon oxide in fused zirconia powder.
In order to solve the technical problems, the invention adopts the technical scheme that: the method for reducing the content of silicon oxide in the fused zirconia powder comprises the following steps:
step 1, processing the fused zirconia hollow spheres or particles with the silicon oxide content of 0.1-0.5% into the particle size of below 200 meshes by using crushing and grinding equipment to obtain fused zirconia powder;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: (1.5-3), mixing and stirring, and fully reacting to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 5-10 parts of concentrated acid and 2-3 parts of fluoride;
and 3, filtering, washing and drying the zirconia slurry obtained in the step 2 to obtain the low-silicon electrofusion zirconia powder.
Preferably, in the method for reducing the content of fused zirconia powder silica, the reaction time in step 2 is 0.5 to 2 hours.
Preferably, in the method for reducing the content of silicon oxide in the fused zirconia powder, the particle size D50 of the fused zirconia powder in the step 1 is controlled to be 5-30 μm.
Preferably, in the above method for reducing the content of fused zirconia powder silica, the concentrated acid is concentrated sulfuric acid, concentrated hydrochloric acid or concentrated nitric acid; the fluoride is hydrogen fluoride, sodium fluoride or potassium fluoride.
Preferably, in the above method for reducing the content of fused zirconia powder silica, the filtration in step 3 is plate-and-frame filter pressing or vacuum filtration.
Preferably, in the above method for reducing the content of fused zirconia powder silica, the drying in step 3 is flash drying, spray drying or hot air drying.
Preferably, the method for reducing the content of the fused zirconia powder silicon oxide specifically comprises the following steps:
step 1, processing an electric melting zirconia hollow ball or particle with the silicon oxide content of 0.16% into a particle size of 1000 meshes by using crushing and grinding equipment to obtain electric melting zirconia powder;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: 2, mixing and stirring the mixture, and fully reacting for 1 hour to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 5 parts of concentrated hydrochloric acid and 2 parts of hydrofluoric acid;
step 3, filtering the zirconia slurry obtained in the step 2 by using a plate-and-frame filter press, and washing for 3 times; drying by a hot air drying box; obtaining the low-silicon electric melting zirconia.
The invention has the beneficial effects that: different from the prior art, the invention provides a method for removing silicon oxide in fused zirconia by a wet method, which can purify zirconia with the silicon oxide content of 0.1-0.5% until the silicon oxide content is less than or equal to 0.05%, so that the final zirconia powder has higher purity and more stable quality. In the method, when the electric melting zirconia powder and the desiliconization acid solution react, free silica reacts with fluoride ions to generate silicon tetrafluoride gas to be discharged, the gas is absorbed by liquid alkali, waste gas in the production process is recovered, and the desiliconization acid solution can be recycled and has little pollution to the environment.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The invention provides a method for reducing the content of silicon oxide in fused zirconia powder, which comprises the following steps:
1. the fused zirconia hollow spheres or particles with the silicon oxide content of 0.1-0.5 percent are processed into 200 meshes with fine granularity by crushing and grinding equipment.
The method for detecting the content of the silicon oxide comprises the following steps: GB T21114-2007 refractory material X-ray fluorescence spectrochemistry analysis fusion-cast glass flake method.
2. Preparing a silicic acid reducing solution, wherein the formula is as follows: 100 parts of water, 5-10 parts of concentrated acid and 2-3 parts of fluoride, and fully stirring the mixture to ensure that no insoluble substance exists for later use. The parts of the formula refer to parts by mass; the concentrated acid comprises concentrated sulfuric acid (mass fraction is more than or equal to 92%), concentrated hydrochloric acid, concentrated nitric acid and other strong acids; the fluoride comprises soluble fluorides such as hydrogen fluoride (mass fraction is more than or equal to 40%), sodium fluoride, potassium fluoride and the like;
3. mixing the fused zirconia powder and the desilicication solution according to the mass ratio of 1: (1.5-3), mixing and stirring, and fully reacting for 0.5-2 hours.
The reaction mechanism is that under the acidic condition, free silicon oxide reacts with fluorine ions to generate silicon tetrafluoride gas to be discharged, and the equation of the reaction ions is as follows: SiO 22+4F-+4H+—SiF4(q)+2H2O；SiF4The gas is absorbed by liquid alkali, and the reaction equation is as follows: SiF4+6NaOH—Na2SiO3+4NaF+3H2O。
4. Filtering, washing and drying the zirconia slurry treated by the silicic acid reducing solution to obtain SiO2Low silicon electric melting zirconia powder with the content less than or equal to 0.05 percent.
The filtering mode can select plate-and-frame filter pressing, vacuum filtering and the like;
the drying can be performed by flash drying, spray drying, hot air drying, etc.;
compared with the prior art, the method for reducing the content of the silicon oxide in the fused zirconia powder provides a method for removing the silicon oxide in the fused zirconia by a wet method, and the method can purify the zirconia with the silicon oxide content of 0.1-0.5% until the silicon oxide content is less than or equal to 0.05%, so that the final zirconia powder has higher purity and more stable quality. And waste gas can be recovered in the production process, the desiliconization acid liquid can be recycled, and the environmental pollution is small.
Example 1
A method for reducing the content of silicon oxide in fused zirconia powder comprises the following steps:
step 1, processing an electric melting zirconia hollow ball with the silicon oxide content of 0.35% into 325-mesh granularity by using crushing and grinding equipment to obtain electric melting zirconia powder; the particle size D50 of the fused zirconia powder is controlled to be 12.6 mu m;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: 2, mixing and stirring the mixture, and fully reacting for 1 hour to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 8 parts of concentrated sulfuric acid (the mass fraction of the embodiment is 92%) and 2 parts of hydrofluoric acid (the mass fraction of the embodiment is 43%);
step 3, filtering the zirconia slurry obtained in the step 2 by using a plate-and-frame filter press, and washing for 3 times; drying by a flash evaporation dryer; the obtained zirconia powder has the following silicon oxide content: 0.036%.
Example 2
A method for reducing the content of silicon oxide in fused zirconia powder comprises the following steps:
step 1, processing an electric melting zirconia hollow ball with the silicon oxide content of 0.42% into a particle size of 200 meshes by using crushing and grinding equipment to obtain electric melting zirconia powder; the particle size D50 of the fused zirconia powder is controlled to be 12.6 mu m;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: 1.6, fully reacting for 1.5 hours to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 10 parts of concentrated sulfuric acid (the mass fraction of the embodiment is 92.5%) and 2 parts of sodium fluoride (the mass fraction of the embodiment is 45%);
step 3, filtering the zirconia slurry obtained in the step 2 by using a plate-and-frame filter press, and washing for 3 times; drying by a spray dryer; the obtained zirconia powder has the following silicon oxide content: 0.047 percent.
Example 3
A method for reducing the content of silicon oxide in fused zirconia powder comprises the following steps:
step 1, processing an electric melting zirconia hollow ball with the silicon oxide content of 0.25% into a particle size of 200 meshes by using crushing and grinding equipment to obtain electric melting zirconia powder; the particle size D50 of the fused zirconia powder is controlled to be 17.3 mu m;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: 1.8, fully reacting for 1.5 hours to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 8 parts of concentrated sulfuric acid (the mass fraction of the embodiment is 93%) and 3 parts of potassium fluoride (the mass fraction of the embodiment is 53%);
step 3, filtering the zirconia slurry obtained in the step 2 by using a plate-and-frame filter press, and washing for 3 times; drying by a hot air drying box; the obtained zirconia powder has the following silicon oxide content: 0.031%.
Example 4
A method for reducing the content of silicon oxide in fused zirconia powder comprises the following steps:
step 1, processing an electric melting zirconia hollow ball with the silicon oxide content of 0.16% into a particle size of 1000 meshes by using crushing and grinding equipment to obtain electric melting zirconia powder; the particle size D50 of the fused zirconia powder is controlled to be 6.58 mu m;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: 2, mixing and stirring the mixture, and fully reacting for 1 hour to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 5 parts of concentrated hydrochloric acid and 2 parts of hydrofluoric acid;
step 3, filtering the zirconia slurry obtained in the step 2 by using a plate-and-frame filter press, and washing for 3 times; drying by a hot air drying box; the obtained zirconia powder has the following silicon oxide content: 0.026%.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (7)
1. A method for reducing the content of silicon oxide in fused zirconia powder is characterized by comprising the following steps:
step 1, processing the fused zirconia hollow spheres or particles with the silicon oxide content of 0.1-0.5% into the particle size of below 200 meshes by using crushing and grinding equipment to obtain fused zirconia powder;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: (1.5-3), mixing and stirring, and fully reacting to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by mass: 100 parts of water, 5-10 parts of concentrated acid and 2-3 parts of fluoride;
and 3, filtering, washing and drying the zirconia slurry obtained in the step 2 to obtain the low-silicon electrofusion zirconia powder.
2. A method for reducing the silica content of electrofused zirconia powder according to claim 1, characterized in that the reaction time of step 2 is 0.5-2 hours.
3. The method for reducing the content of silicon oxide in the electrofused zirconia powder according to claim 1, wherein the particle size D50 of the electrofused zirconia powder in the step 1 is controlled to be 5 to 30 μm.
4. The method for reducing the content of fused zirconia powder silica according to claim 1, wherein the concentrated acid is concentrated sulfuric acid, concentrated hydrochloric acid or concentrated nitric acid; the fluoride is hydrogen fluoride, sodium fluoride or potassium fluoride.
5. The method for reducing the content of fused zirconia powder silica according to claim 1, wherein the filtration in step 3 is plate and frame filter pressing or vacuum filtration.
6. The method for reducing the content of silicon oxide in the electrofused zirconia powder according to claim 1, wherein the drying in step 3 is flash drying, spray drying or hot air drying.
7. The method for reducing the content of fused zirconia powder silica according to claim 1, comprising the steps of:
step 1, processing an electric melting zirconia hollow ball or particle with the silicon oxide content of 0.16% into a particle size of 1000 meshes by using crushing and grinding equipment to obtain electric melting zirconia powder;
step 2, mixing the fused zirconia powder obtained in the step 1 and the desilicication solution according to a mass ratio of 1: 2, mixing and stirring the mixture, and fully reacting for 1 hour to obtain zirconia slurry;
the silicon reduction acid solution comprises the following components in parts by weight: 100 parts of water, 5 parts of concentrated hydrochloric acid and 2 parts of hydrofluoric acid;
step 3, filtering the zirconia slurry obtained in the step 2 by using a plate-and-frame filter press, and washing for 3 times; drying by a hot air drying box; obtaining the low-silicon electric melting zirconia powder.
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| CN101863478A (en) * | 2010-06-22 | 2010-10-20 | 石平湘 | Preparation method of high-purity silicon tetrafluoride |
| CN102134078A (en) * | 2011-01-14 | 2011-07-27 | 浙江中宁硅业有限公司 | Method for closed-loop production of silicon tetrafluoride by utilizing sulfuric acid and quartz sand |
| CN103708472A (en) * | 2013-12-20 | 2014-04-09 | 贵州万方铝化科技开发有限公司 | Method for preparing SiO2 powder by using zircon sand |
| CN104692440A (en) * | 2015-02-09 | 2015-06-10 | 东北大学 | De-silicication purifying method for fluorite for pre-melted slag |
| US20160068443A1 (en) * | 2014-09-04 | 2016-03-10 | Kaohsiung Medical University | Methods for producing a silicon-containing zirconia calcined body and a silicon-containing zirconia sintered body |
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Application publication date: 20200915 |