CN114455594A - Cristobalite prepared by electric melting method - Google Patents
Cristobalite prepared by electric melting method Download PDFInfo
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- CN114455594A CN114455594A CN202210131126.7A CN202210131126A CN114455594A CN 114455594 A CN114455594 A CN 114455594A CN 202210131126 A CN202210131126 A CN 202210131126A CN 114455594 A CN114455594 A CN 114455594A
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- cristobalite
- quartz
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 229910052906 cristobalite Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000002844 melting Methods 0.000 title claims description 5
- 230000008018 melting Effects 0.000 title claims description 5
- 239000010453 quartz Substances 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 239000004575 stone Substances 0.000 claims abstract description 15
- 239000005350 fused silica glass Substances 0.000 claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910001415 sodium ion Inorganic materials 0.000 claims description 2
- 230000009466 transformation Effects 0.000 abstract description 9
- 229910021493 α-cristobalite Inorganic materials 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005495 investment casting Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000003822 epoxy resin Substances 0.000 abstract 1
- 229920000647 polyepoxide Polymers 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 4
- 239000006004 Quartz sand Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000029052 metamorphosis Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011044 quartzite Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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 invention discloses a preparation method of cristobalite. The natural quartz stone and the crystallization inhibitor are mixed according to a certain proportion, the mixed raw materials are put into a fused quartz furnace and heated under certain conditions, and the square quartz blocks obtained after heating are reserved or the outer skins of the square quartz blocks are removed according to the requirements of customers, and are crushed and ground into the corresponding sizes. The method for preparing the cristobalite comprises the following steps of filling the quartz stone and the crystallization inhibitor, converting the quartz stone into the cristobalite, and crushing and grinding according to requirements. The finished product rate of the prepared cristobalite is more than 90 percent, the transformation rate of alpha-cristobalite is more than or equal to 97 percent, and the method is particularly suitable for the epoxy resin pouring and precision casting industries. The method for preparing the cristobalite has simple process, and has the characteristics of low energy consumption, low requirement on equipment, easily obtained raw materials, low cost, excellent product quality and the like compared with the existing industrial process.
Description
Technical Field
The invention relates to the technical field of inorganic material preparation in the non-ferrous metal smelting industry, in particular to cristobalite prepared by an electric melting method.
Background
Cristobalite is one of quartz, the main component of which is silicon dioxide, the crystal phase of which is tetragonal, the hardness of which is about 6.5, and the density of which is 2.45. The cristobalite has the characteristics of high whiteness, high porosity, corrosion resistance, high temperature resistance, excellent thermal shock resistance, high temperature expansion and the like, so that the cristobalite is widely applied to the industries of paint, epoxy casting materials, gypsum jewelry casting powder, precision casting and the like.
With the social development and the continuous and deep understanding of cristobalite in the related industries, the demand for cristobalite is increasing. However, the natural cristobalite only exists in the acid volcanic rock, the stock is very small, and the cristobalite raw material on the market mainly comes from a byproduct quartz crucible for calcining and smelting polycrystalline silicon in a kiln. At present, the common industrial production method is to use an oil gas kiln to calcine quartz sand at high temperature or screen and crush byproducts produced in polysilicon production. The cristobalite transformation rate of the quartz product obtained by the high-temperature calcination method is about 95 percent. The disadvantages of this method are: 1. the quartz sand grains are required to be high in diameter and are in blocks of 50-150 mm, and in order to ensure sufficient heating, the quartz sand grains need to be stacked in order before entering a furnace, so that the cost is high; 2. the oil gas kiln needs longer time for heating to a specified temperature, and has higher energy consumption; 3. the produced product often contains impurities such as quartz phosphate and the like, and the high transformation rate product meeting the market demand needs manual separation. For the second production method described above, the greatest problem arises from the absence of raw materials. With the elimination of polysilicon products in the market, quartz crucibles, which are byproducts of polysilicon production, are also exhausted, and the market supply of cristobalite is further unable to meet the demands of buyers.
Disclosure of Invention
The invention aims to solve the technical problem of providing a stable alpha-cristobalite production method with high transformation ratio, which takes natural quartz stone as a raw material, has low energy consumption and simple process, is easy for industrial large-scale production, meets the market demand.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of cristobalite comprises the steps of mixing natural quartzite and a crystallization inhibitor according to a certain proportion, putting the mixed raw materials into a fused quartz furnace, heating under a certain condition, retaining or removing a sheath (the sheath contains 30-40% of cristobalite, the total purity of the product of the retained sheath is still higher than 97%) of 3-5 cm of the obtained cristobalite block according to the requirements of customers, and crushing and grinding the cristobalite block into corresponding specifications. The rate of finished products of the cristobalite prepared by the method is more than 90%, and the transformation rate of alpha-cristobalite is more than or equal to 97%.
The crystallization retardant is a high carbon and sodium ion complex.
The addition amount of the crystallization retardant is 3-5 per mill of the mass of the natural quartz stone.
The content of silicon dioxide in the natural quartz stone is more than or equal to 99.8 percent.
The particle size of the natural quartz stone is 0-200 mm.
The fused quartz furnace is an electric furnace which uses one or more graphite carbon rods as a heating body.
The heating voltage of the melting quartz furnace is 36-380V, and direct current or alternating current can be used.
The heating condition is that the heating temperature is more than or equal to 1580 ℃, and the heating time is more than or equal to 8 hours.
The working principle of the invention is as follows:
the quartz is divided into four kinds of metamorphosis variants, namely quartz, tridymite, cristobalite and fused quartz, according to different crystal structures. In natural quartz, silica is generally present in the state of quartz. When the natural quartz is heated, it is changed into tridymite and cristobalite, which are in turn changed into fused quartz. According to the invention, by adding the crystallization inhibitor, the quartz can still maintain the crystal structure of the cristobalite at a high temperature of 1680 ℃ and is not converted into fused quartz any more, and the cristobalite with high purity and high conversion rate is obtained through sufficient reaction.
Compared with the existing production method, the invention has the following advantages:
1. the raw material requirement is low, and stacking and stirring are not needed in production, so that the production cost is reduced;
2. the energy consumption of the fused quartz furnace is lower than that of an oil gas combustion furnace, and the used energy is cleaner;
3. the process is simple, the crystallization inhibitor is low in price and easy to obtain, the requirement on equipment is low, and the industrial production is facilitated;
4. the yield of the cristobalite prepared by the method is more than 90%, the transformation rate of alpha-cristobalite is more than or equal to 97%, the cristobalite has better quality than the products circulating in the market, and the cristobalite can particularly better meet the requirements of the precision casting industry.
Drawings
FIG. 1 is an XRD pattern of the material obtained in example 1.
Figure 2 is an XRD pattern of the material obtained in example 2.
Figure 3 is an XRD pattern of the material obtained in example 3.
FIG. 4 is a graph comparing the material obtained in the comparative example with cristobalite.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easy to understand, the invention is further explained by combining the specific embodiments and the drawings.
Example 1
1t of natural quartz stone with the particle size of 0-200mm and 5kg of crystallization inhibitor are placed in a fused quartz furnace after being stirred and mixed commonly, the mixture is heated for 10 hours, and the obtained product is kept with the outer skin and is crushed to obtain the cristobalite. The XRD pattern of the resulting material is shown in FIG. 1.
Example 2
1t of natural quartz stone with the particle size of 0-200mm and 5kg of crystallization inhibitor are placed in a fused quartz furnace after being stirred and mixed commonly, the mixture is heated for 12 hours, and the obtained product is kept with the outer skin and is crushed to obtain the cristobalite. The XRD pattern of the resulting material is shown in FIG. 1.
Example 3
1t of natural quartz stone with the particle size of 0-200mm and 5kg of crystallization inhibitor are placed in a fused quartz furnace after being stirred and mixed commonly, the mixture is heated for 10 hours, and the obtained product is subjected to crust removal and crushing to obtain cristobalite. The XRD pattern of the resulting material is shown in FIG. 1.
As is clear from FIG. 1, the material obtained in example 1 was cristobalite phase, and the α -cristobalite transformation ratio was 97.1%.
As is clear from FIG. 2, the material obtained in example 2 was cristobalite phase, and the α -cristobalite transformation ratio was 97.6%.
As can be seen from FIG. 3, the material obtained in example 2 was cristobalite phase, and the α -cristobalite transformation ratio was 99.5%.
Comparative example
1t of natural quartz stone with the particle size of 0-200mm is placed in a fused quartz furnace after being stirred and mixed normally, the mixture is heated for 10 hours, and the obtained product is crushed to obtain fused quartz. The resulting material is compared to cristobalite as shown in figure 4.
As can be seen from FIG. 4, the material obtained in the comparative example was a colorless transparent block on the right side, which was different from the cristobalite white and opaque on the left side.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (9)
1. A method for preparing cristobalite is characterized by comprising the following steps: mixing natural quartz stone and a crystallization inhibitor according to a certain proportion, putting the mixed raw materials into a fused quartz furnace, heating under a certain condition, retaining or removing the outer skin of a square quartz block obtained after heating according to the requirements of customers, and crushing and grinding the square quartz block into a corresponding size.
2. The method for producing cristobalite according to claim 1, characterized in that: the crystallization retardant is a high carbon and sodium ion complex.
3. The method for producing cristobalite according to claim 2, characterized in that: the addition amount of the crystallization retardant is 3-5 per mill of the mass of the natural quartz stone.
4. The method for producing cristobalite according to claim 1, characterized in that: the content of silicon dioxide in the natural quartz stone is more than or equal to 99.8 percent.
5. The method for producing cristobalite according to claim 4, characterized in that: the particle size of the natural quartz stone is 0-200 mm.
6. The method for producing cristobalite according to claim 1, characterized in that: the fused quartz furnace is an electric furnace which uses one or more graphite carbon rods as a heating body.
7. The method for producing cristobalite according to claim 6, characterized in that: the heating voltage of the melting quartz furnace is 36-380V, and direct current or alternating current can be used.
8. The method for producing cristobalite according to claim 1, characterized in that: the heating condition is that the heating temperature is more than or equal to 1580 ℃, and the heating time is more than or equal to 8 hours.
9. A cristobalite produced by the method according to any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210131126.7A CN114455594A (en) | 2022-02-13 | 2022-02-13 | Cristobalite prepared by electric melting method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210131126.7A CN114455594A (en) | 2022-02-13 | 2022-02-13 | Cristobalite prepared by electric melting method |
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| Publication Number | Publication Date |
|---|---|
| CN114455594A true CN114455594A (en) | 2022-05-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210131126.7A Pending CN114455594A (en) | 2022-02-13 | 2022-02-13 | Cristobalite prepared by electric melting method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041548A (en) * | 2007-03-05 | 2007-09-26 | 中国地质大学（武汉） | Method for preparing cristobalite by calcining quartz |
| CN104030295A (en) * | 2014-06-27 | 2014-09-10 | 贵州大学 | Method for improving conversion ratio of alpha-cristobalite crystal form through sodium hydroxide |
| US20170130793A1 (en) * | 2015-11-06 | 2017-05-11 | Schaeffler Technologies AG & Co. KG | Wet friction materials including cristobalite as filler material |
| CN207031321U (en) * | 2017-03-16 | 2018-02-23 | 湖南金马新材料科技有限公司 | A kind of konilite prepares the process units of active cristobalite |
| CN109665530A (en) * | 2019-01-23 | 2019-04-23 | 景德镇陶瓷大学 | A method of ultra-fine cristobalite powder is prepared with quartz sand |
-
2022
- 2022-02-13 CN CN202210131126.7A patent/CN114455594A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041548A (en) * | 2007-03-05 | 2007-09-26 | 中国地质大学（武汉） | Method for preparing cristobalite by calcining quartz |
| CN104030295A (en) * | 2014-06-27 | 2014-09-10 | 贵州大学 | Method for improving conversion ratio of alpha-cristobalite crystal form through sodium hydroxide |
| US20170130793A1 (en) * | 2015-11-06 | 2017-05-11 | Schaeffler Technologies AG & Co. KG | Wet friction materials including cristobalite as filler material |
| CN108350966A (en) * | 2015-11-06 | 2018-07-31 | 舍弗勒技术股份两合公司 | Include wet friction material of the cristobalite as filler material |
| CN207031321U (en) * | 2017-03-16 | 2018-02-23 | 湖南金马新材料科技有限公司 | A kind of konilite prepares the process units of active cristobalite |
| CN109665530A (en) * | 2019-01-23 | 2019-04-23 | 景德镇陶瓷大学 | A method of ultra-fine cristobalite powder is prepared with quartz sand |
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Application publication date: 20220510 |