CN100582035C - Method for preparing cristobalite by calcining quartz - Google Patents
Method for preparing cristobalite by calcining quartz Download PDFInfo
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- CN100582035C CN100582035C CN200710051620A CN200710051620A CN100582035C CN 100582035 C CN100582035 C CN 100582035C CN 200710051620 A CN200710051620 A CN 200710051620A CN 200710051620 A CN200710051620 A CN 200710051620A CN 100582035 C CN100582035 C CN 100582035C
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Abstract
The invention disclose a preparing method of cristobalite through calcining quartz, which comprises the following steps: 1) mixing quartz power and phase-change activator; getting batches; compositing Y2O3,Na2CO and BaF2 as phase-change activator; making the adding quantity of Y2O3, Na2CO3 and BaF2 separately at 1 per mill -5 per mill , 5 per mill -10 per mill and 1 per mill -5 per mill against the weight of quartz power; 2) heating the batches up to 1300 deg.c with speed of 2-10 deg.c per minuet; keeping temperature at 1300 deg.c at 6 h; getting product with quartz phase bigger-than 94%.
Description
Technical field
The present invention relates to a kind of method of preparing cristobalite by calcining quartz.
Background technology
Cristobalite is a kind of mineral species of quartzy family mineral, has high temperature cristobalite (α-Fang Shiying) and low temperature cristobalite (β-cristobalite) not.Transformation temperature is at 200～270 ℃ between them, and is attended by bigger volume change.Natural cristobalite generally originates in the bubble of volcanics formation, does not have natural ore deposit.And there is phase transition process in quartzy family mineral under different temperature, pressure, and when temperature arrives 1470 ℃, quartz will be transformed into α-Fang Shiying.Usually be exactly this character of utilizing it, carry out the suitability for industrialized production of cristobalite.Cristobalite powder is because its distinctive performance, be widely used in the industries such as precision casting, high-grade electroceramics, dental material, electronic wafer, polishing material, special ceramic material, special refractories, high-grade papermaking, high-grade paint, shielding material, daily-use chemical industry, tamanori, plastics, silicon rubber, and its import price is very high.Along with the increase year by year of consumption, it is urgent day by day that the production domesticization of cristobalite powder has seemed.
The method of producer quartz has two kinds: a kind of is in 1500 ℃ of calcinings (quartzy invert point to the cristobalite phase transformation is 1470 ℃, considers temperature imbalance in the stove, and is thorough to guarantee incinerating), insulation 3-6 hour with quartz powder materials.Another kind method is directly to calcine blout to prepare cristobalite (as China Patent No.: ZL00107107.6), its technical process is: piece material → cleaning → removal of impurities → loading of kiln → calcining → insulation → kiln discharge → impurity elimination → ball milling processing → pack warehouse-in.
The domestic literature report, the method that reduces the cristobalite calcining temperature has following several: a kind of is to add metal oxide, see (Wang Jinshu, Deng. quartzy to α cristobalite transformation efficiency research [J]. Chinese pottery, 1992 (6): 1-5), report in the literary composition that aluminum oxide is an ideal phase-change catalyst comparatively, when add-on is 4%, be up to 42.2% at 1320 ℃ of transformation efficiencys; Second kind is lime-irony (CaO+FeO) or iron-calcium carbonate (FeO+CaO) mineralizer that extensively adopts in producing at present, and more extensive with the former application, add-on is, and: CaO is about 2.5%, FeO (Fe
2O
3) 0.5-1.0%, add-on is 3-4% usually; The third for fluorine-containing compound as mineralizer, can quicken greatly the quartz conversion, transformation efficiency can reach 85% during to 1400 ℃.The major defect of above method is that the additive add-on is excessive, influence the purity of cristobalite, and transformation efficiency is lower.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing cristobalite by calcining quartz, this method energy consumption is low, production cost is low, and the transformation efficiency height.
To achieve these goals, technical scheme of the present invention is: a kind of method of preparing cristobalite by calcining quartz is characterized in that it comprises the steps:
1), quartz powder materials and phase-change catalyst are mixed, admixtion; Described phase-change catalyst is Y
2O
3, Na
2CO
3And BaF
2The composite catalyst of being formed, Y
2O
3Add-on be 1 ‰ of quartz powder materials weight-5 ‰, Na
2CO
3Add-on be 5 ‰ of quartz powder materials weight-10 ‰, BaF
2Add-on be 1 ‰ of quartz powder materials weight-5 ‰;
2), admixtion is warming up to 1300 ℃ with the speed of 2 ℃-10 ℃ of per minutes, 1300 ℃ of insulations 6 hours, cristobalite greater than 94% product.
The particle diameter of described quartz powder materials is less than 100 orders (0.149mm), and SiO
2Content greater than 99.8%.
The present invention adopts quartz powder materials and Y
2O
3, Na
2CO
3And BaF
2The composite catalyst of being formed mixes, and can make the invert point that quartz changes cristobalite into reduce to 1300 ℃ by 1470 ℃, and transformation efficiency is greater than 94%.The outstanding advantage that the present invention compared with prior art has can reduce energy consumption exactly, reduce production costs, and transformation efficiency height (greater than 94%).
Characteristics of the present invention are mainly reflected in:
1. phase-change catalyst consumption few (less than 2%), the mineralizer addition of ordinary method is at 3-4%.
2. calcining temperature low (1300 ℃), the calcining temperature of ordinary method is more than 1500 ℃.
3. the transformation efficiency height (greater than 94%) of cristobalite.
Application Areas of the present invention is a fire resisting material field, particularly a kind of cristobalite material.The present invention can improve existing production technique, cuts down the consumption of energy, and save energy reduces and pollutes, and reduces production costs greatly, makes product have more the market competitiveness.
Description of drawings
Fig. 1 does not add phase-change catalyst for comparative example 1[silica powder, 1300 ℃ of calcining insulations 6 hours] the XRD figure spectrum of gained.
Fig. 2 adds 5 ‰ yttrium oxide for comparative example 2[silica powder, and 10 ‰ yellow soda ash, 5 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] the XRD figure spectrum of gained.
Fig. 3 is the XRD figure spectrum of the embodiment of the invention one [silica powder adds 2 ‰ yttrium oxide, 8 ‰ yellow soda ash, 5 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] gained.
Fig. 4 is the XRD figure spectrum of the embodiment of the invention two [silica powder adds 5 ‰ yttrium oxide, 9 ‰ yellow soda ash, 3 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] gained.
Fig. 5 is the XRD figure spectrum of the embodiment of the invention three [silica powder adds 4 ‰ yttrium oxide, 8 ‰ yellow soda ash, 5 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] gained.
Fig. 6 is the XRD figure spectrum of the embodiment of the invention four [silica powder adds 5 ‰ yttrium oxide, 8 ‰ yellow soda ash, 5 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] gained.
Fig. 7 is the XRD figure spectrum of the embodiment of the invention five [silica powder adds 3 ‰ yttrium oxide, 8 ‰ yellow soda ash, 4 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] gained.
Fig. 8 is the XRD figure spectrum of the embodiment of the invention six [silica powder adds 4 ‰ yttrium oxide, 8 ‰ yellow soda ash, 4 ‰ barium fluorides were 1300 ℃ of calcining insulations 6 hours] gained.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment one:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 2 ‰, add the yellow soda ash of quartz powder materials weight 8 ‰, add the barium fluoride of quartz powder materials weight 5 ‰, mix, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 3.As can be seen from Figure 3 the cristobalite transformation efficiency is 95.23%.
Embodiment two:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 5 ‰, add the yellow soda ash of quartz powder materials weight 9 ‰, add the barium fluoride of quartz powder materials weight 3 ‰, mix, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 4.As can be seen from Figure 4 the cristobalite transformation efficiency is 94.34%.
Embodiment three:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 4 ‰, add the yellow soda ash of quartz powder materials weight 8 ‰, add the barium fluoride of quartz powder materials weight 5 ‰, mix, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 5.As can be seen from Figure 5 the cristobalite transformation efficiency is 95.23%.
Embodiment four:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 5 ‰, the yellow soda ash of quartz powder materials weight 8 ‰, the barium fluoride of quartz powder materials weight 5 ‰ mixes, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 6.As can be seen from Figure 6 the cristobalite transformation efficiency is 94.34%.
Embodiment five:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 3 ‰, add the yellow soda ash of quartz powder materials weight 8 ‰, add the barium fluoride of quartz powder materials weight 4 ‰, mix, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 7.As can be seen from Figure 7 the cristobalite transformation efficiency is 94.34%.
Embodiment six:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 4 ‰, add the yellow soda ash of quartz powder materials weight 8 ‰, add the barium fluoride of quartz powder materials weight 4 ‰, mix, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 8.As can be seen from Figure 8 the cristobalite transformation efficiency is 96.15%.
Embodiment seven:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 1 ‰, add the yellow soda ash of quartz powder materials weight 5 ‰, add the barium fluoride of quartz powder materials weight 1 ‰, mix, put into, be warming up to 1300 ℃ with the speed of 10 ℃ of per minutes in the Si-Mo rod chamber type electric resistance furnace, 1300 ℃ of insulations 6 hours, obtain the cristobalite product.
Embodiment eight:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 5 ‰, add the yellow soda ash of quartz powder materials weight 10 ‰, add the barium fluoride of quartz powder materials weight 5 ‰, mix, put into, be warming up to 1300 ℃ with the speed of 2 ℃ of per minutes in the Si-Mo rod chamber type electric resistance furnace, 1300 ℃ of insulations 6 hours, obtain the cristobalite product.
The comparative example 1:
To put into corundum crucible less than 0.149mm silica powder 5.00g, under the situation of not adding phase-change catalyst, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtain the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 1.As can be seen from Figure 1 the cristobalite transformation efficiency is less than 10%.
The comparative example 2:
To put into corundum crucible less than 0.149mm silica powder 5.00g, add the yttrium oxide of quartz powder materials weight 5 ‰, add the yellow soda ash of quartz powder materials weight 10 ‰, add the barium fluoride of quartz powder materials weight 5 ‰, mix, put in the Si-Mo rod chamber type electric resistance furnace, speed with 4 ℃ of per minutes is warming up to 1300 ℃, 1300 ℃ of insulations 6 hours, obtains the cristobalite product, product is carried out X powder crystal diffraction analysis, obtain XRD figure spectrum 2.As can be seen from Figure 2 the cristobalite transformation efficiency is greater than 94%.
Claims (2)
1. the method for a preparing cristobalite by calcining quartz is characterized in that it comprises the steps:
1), quartz powder materials and phase-change catalyst are mixed, admixtion; Described phase-change catalyst is Y
2O
3, Na
2CO
3And BaF
2The composite catalyst of being formed, Y
2O
3Add-on be 1 ‰ of quartz powder materials weight-5 ‰, Na
2CO
3Add-on be 5 ‰ of quartz powder materials weight-10 ‰, BaF
2Add-on be 1 ‰ of quartz powder materials weight-5 ‰;
2), admixtion is warming up to 1300 ℃ with the speed of 2 ℃-10 ℃ of per minutes, 1300 ℃ of insulations 6 hours, cristobalite greater than 94% product.
2. the method for a kind of preparing cristobalite by calcining quartz according to claim 1, it is characterized in that: the particle diameter of described quartz powder materials is less than 100 orders, and SiO
2Content greater than 99.8%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282035A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工股份有限公司 | A kind of cristobalite and its preparation method and application |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531368B (en) * | 2009-04-10 | 2011-06-22 | 华南师范大学 | Method for preparing cristobalite material by taking quartz crucible as raw material |
| CN103286259B (en) * | 2013-07-03 | 2016-01-20 | 黄建荣 | A kind of cristobalite lost foam casting coating and preparation method |
| CN103771426B (en) * | 2014-01-16 | 2015-08-19 | 中国科学院广州地球化学研究所 | A kind of take diatomite as the method for raw material low-firing porous cristobalite |
| CN105174271B (en) * | 2015-08-24 | 2017-05-03 | 上海工程技术大学 | Method for crystallizing silicon oxide at low temperature in molten salt system |
| CN109052417B (en) * | 2018-09-11 | 2019-07-26 | 安徽科技学院 | A kind of synthetic method of high-purity low-temperature phase cristobalite |
| CN114455594A (en) * | 2022-02-13 | 2022-05-10 | 段晓文 | Cristobalite prepared by electric melting method |
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2007
- 2007-03-05 CN CN200710051620A patent/CN100582035C/en not_active Expired - Fee Related
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282035A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工股份有限公司 | A kind of cristobalite and its preparation method and application |
| CN107282035B (en) * | 2016-04-12 | 2019-12-24 | 中国石油化工股份有限公司 | Cristobalite and preparation method and application thereof |
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