CN109665530B - A method of ultra-fine cristobalite powder is prepared with quartz sand - Google Patents
A method of ultra-fine cristobalite powder is prepared with quartz sand Download PDFInfo
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- CN109665530B CN109665530B CN201910060894.6A CN201910060894A CN109665530B CN 109665530 B CN109665530 B CN 109665530B CN 201910060894 A CN201910060894 A CN 201910060894A CN 109665530 B CN109665530 B CN 109665530B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a kind of methods for preparing ultra-fine cristobalite powder with quartz sand, its feature includes the following steps: step 1: using quartz sand as raw material, a certain amount of mineralizer is mixed into quartz sand by certain mode, 80 meshes are crossed after ball milling mixes, and form uniform quartz sand, mineralizer mixture；Step 2: mixture is calcined in certain temperature, and then quenching, obtains fluffy cristobalite powder；Step 3: cristobalite powder obtains ultra-fine cristobalite powder through certain way grinding treatment.This method is low in cost, environmentally protective, simple process, short preparation period and is suitable for large-scale production, and the feasibility of practical application is high, has broad application prospects.
Description
Technical field
The invention belongs to superfine powder preparation fields, and in particular to a kind of side that ultra-fine cristobalite powder is prepared with quartz sand
Method.
Background technique
Cristobalitkristall stable structure, physical and chemical properties are excellent, and have excellent dielectric properties.Cristobalite it is close
Spend that low, whiteness is high, thermal expansion coefficient is low, thermal coefficient is high, heat resistance is good, corrosion resistance is strong.With other silica material phases
Than cristobalite has more excellent optical property, higher stability and more excellent thermal shock resistance.These excellent characteristics
Cristobalite is set to be widely used in coating, glass, papermaking, plastic filler, functional material, high-performance ceramic, hot investment casting, biological material
The fields such as material, aerospace.However, it is considered that natural cristobalite is not present.SiO in nature2It is most common
Crystal habit isβQuartz, cristobalite need to be occurred from transformation of crystal at 1470 DEG C or more by quartz.Meanwhile cristobalite is answered
With often requiring to be directly added into the form of powder in main body formula or answered again after the device shape that reshaping needs, sintering
With.Cristobalite is prepared into superfine powder to be conducive to improve its activity, the sintering temperature of material is reduced, improves the comprehensive of product
Energy.
Currently, the demand of domestic high-quality, ultra-fine cristobalite powder relies primarily on import satisfaction.Develop large-scale industrial production
Cristobalite superfine powder technology of preparing has shown important and urgent day.Has the document report of some cristobalite preparations at present.Both at home and abroad
The process for preparing cristobalite powder mainly has synthesis chemical method and blout to be directly calcined method, and synthesis chemical method is using stone
Sand is first chemically treated, then is carried out high-temperature calcination and also prepared cristobalite powder originally, it needs huge chemical processing device,
Thus this preparation method investment is big, high production cost, and cristobalite powder synthesizes unstable quality.Blout is directly calcined method
To directly adopt blout to prepare cristobalite powder through high-temperature calcination, quartz inversion at the temperature of cristobalite be up to 1470 DEG C with
On, thus this preparation method high production cost.Also having at present reduces cristobalite by addition phase-change catalyst or mineralizer
The report of phase transition temperature.Takao Suzuki's et al. studies have shown that Al2O3It can promote the conversion of quartz.But conversion temperature
Height, the time is long and conversion ratio is low, less than 40%.Wang Jinshu etc. has studied the shadow that additive metal oxide converts cristobalite powder
It rings, sample preparation passes through first by silica flour raw material grinding to 0.0374 mm, and suitable quantity of water is added after then mineralizer weighs in mass ratio
It is added in raw material after dissolution, being then sufficiently stirred is uniformly mixed it.Obtained slurry, which is put into vitrified pot, to be burnt into.From
So sample is obtained after cooling.Mineralizer oxide is had studied, such as lanthana (La2O3), aluminium oxide (Al2O3), magnesia (MgO),
Calcium oxide (CaO), sodium oxide molybdena (Na2O), copper oxide (CuO) and lead oxide (PbO) etc., to the shadow of 1320 DEG C of cristobalite conversion ratios
It rings, although the transition temperature of cristobalite is reduced to 1320 DEG C by the research, which mainly passes through oxide and formed with silica
Eutectic compound, and then Si-O bonding is destroyed, promote the crystal transfer of silica, this method inevitably results in oxidation
Silicon caking phenomenon, is not easy to ultra fine.Yan Chunjie etc. discloses a kind of method of preparing cristobalite by calcining quartz, main logical
Crossing addition composite phase-change catalyst is Y2O3、Na2CO3And BaF2, 6 hours are kept the temperature in 1300 DEG C, cristobalite is made and is mutually greater than 94%
Product.The cost is relatively high there are phase-change catalyst for this method, and cristobalite is not deeply carried out ultra fine etc. and is asked
Topic.
In conclusion urgent need development cost is low, simple process, and the ashlar that cristobalite phase transition temperature is low, conversion is formed
English is fluffy, the simply ultra-fine cristobalite powder preparation of ultra fine.
Summary of the invention
It is an object of the invention to overcome disadvantage existing in the prior art, one kind low in cost is provided, simple process, is turned
The low method for preparing ultra-fine cristobalite powder with quartz sand of temperature.
In order to solve the above technical problems, the technical scheme is that a kind of prepare ultra-fine cristobalite powder with quartz sand
Method, feature include the following steps:
Step 1: using quartz sand as raw material, a certain amount of mineralizer is mixed into quartz sand by certain mode, through ball
Mill crosses 80 meshes after mixing, and forms uniform quartz sand, mineralizer mixture；
Step 2: mixture is calcined in certain temperature, and then quenching, obtains fluffy cristobalite powder；
Step 3: cristobalite powder obtains ultra-fine cristobalite powder through certain way grinding treatment.
In the step 1 mineralizer be sodium ethoxide, lithium ethoxide, magnesium ethylate, calcium ethoxide, sodium acetate, lithium acetate, magnesium acetate,
One of calcium acetate.
The additive amount of the mineralizer is the 0.1~5% of quartz sand weight.
The mode that is mixed into the step 1 is dry or wet mixing.
Calcination temperature in the step 2 is 1150~1350 DEG C, and soaking time is 0.5~12 h.
Quenching mode in the step 2 is direct room temperature quenching or water quenching.
Mode is ground as dry grinding or wet-milling or air-flow crushing in the step 3, and Ball-milling Time is 1~12h.
The temperature of the water quenching is 5 ~ 30 DEG C.
The quartz sand is converted into the conversion ratio 92~99% of cristobalite.
The grain fineness of ultra-fine cristobalite powder made from the step 3 is D50=0.305~0.85 μm.
Outstanding advantage of the invention is: the present invention efficiently uses alkali metal alcoholates, acetate or alkaline-earth alkoxides, second
Hydrochlorate decomposes the alkali metal oxide or alkaline earth oxide generated, activates the Si-O key in quartz sand, promotes in quartz sand
The transformation of the opposite cristobalite phase of quartz carried out in relatively low temperature；Meanwhile decomposing the CO generated2And H2O gas is effective
It avoids and generates the serious agglomerations phenomenons such as agglomeration during calcining.More crucially the present invention makes full use of quartz opposite
Bulk effect, quenching of the transformation of cristobalite phase etc. crack quartz sand particle surface, even dusting, efficiently solves stone
English is difficult to levigate conventional difficulties.
Detailed description of the invention
Fig. 1 is the process flow of this patent；
Fig. 2 is the XRD spectrum that sample is made in embodiment 1；
Fig. 3 is the laser particle size map that sample is made in embodiment 1；
Fig. 4 is the XRD spectrum that sample is made in embodiment 2；
Fig. 5 is the laser particle size map that sample is made in embodiment 1.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to a kind of specific embodiment party for the method for preparing ultra-fine cristobalite powder with quartz sand proposed according to the present invention
Formula, method, step, feature and its effect, detailed description are as follows:
Embodiment 1
Weigh quartz sand 5000g, mineralizer sodium ethoxide 62.5g, dry grinding mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture；Mixture is in 1300 DEG C of heat preservation 3h, then by obtaining fluffy cristobalite powder, cristobalite after room temperature quenching
Conversion ratio is 98.6%, and cristobalite powder obtains the D of slurry through vibromill wet-milling 1h50=0.305μM obtains ultra-fine ashlar after dry
Ying Fen.
Embodiment 2
Quartz sand 5000g, 5 g of mineralizer lithium ethoxide are weighed, dry grinding mixed 80 meshes, and formed uniform quartz sand, mine
Agent mixture.Mixture is in 1350 DEG C of 6 h of heat preservation, then by obtaining fluffy cristobalite powder, cristobalite after room temperature quenching
Conversion ratio is 95.6%, and cristobalite powder is dry grinded 5h through planetary ball mill, obtains D50= 0.318μM, ultra-fine cristobalite powder.
Embodiment 3
Weigh 5000 g of quartz sand, 125 g of mineralizer magnesium ethylate, dry grinding mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture.Mixture is in 1330 DEG C of 0.5 h of heat preservation, then by obtaining fluffy cristobalite powder after 10 DEG C of water quenchings, side
Quartz transition rate is 95.2%, and cristobalite powder obtains D through planetary ball mill 12 h of dry grinding50=0.82μThe ultra-fine cristobalite powder of m.
Embodiment 4
Weigh 5000 g of quartz sand, 250 g of mineralizer calcium ethoxide, dry grinding mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture.Mixture is in 1150 DEG C of 12 h of heat preservation, then by obtaining fluffy cristobalite powder after 20 DEG C of water quenchings, side
Quartz transition rate is 92.6%, and cristobalite powder obtains D through planetary ball mill 12 h of dry grinding50=0.85μThe ultra-fine cristobalite powder of m.
Embodiment 5
Weigh 5000 g of quartz sand, mineralizer sodium acetate 62.5g, wet-milling mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture.Mixture is in 1250 DEG C of 6 h of heat preservation, then by obtaining fluffy cristobalite powder, ashlar after 25 DEG C of water quenchings
English conversion ratio is 95.2%, and cristobalite powder obtains D through 2 h of air-flow crushing50=0.58μThe ultra-fine cristobalite powder of m.
Embodiment 6
Weigh 5000 g of quartz sand, mineralizer magnesium acetate 62.5g, wet-milling mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture.Mixture is in 1330 DEG C of 3 h of heat preservation, then by obtaining fluffy cristobalite powder, ashlar after room temperature quenching
English conversion ratio is 98.4%, and cristobalite powder handles 2 h through sand mill, obtains D50=0.36μThe slurry of m, slurry are surpassed through drying
Thin cristobalite powder.
Embodiment 7
Weigh quartz sand 5000g, mineralizer lithium acetate 62.5g, wet-milling mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture.Mixture is in 1300 DEG C of 3 h of heat preservation, then by obtaining fluffy cristobalite powder, ashlar after room temperature quenching
English conversion ratio is 93.8%, and cristobalite powder handles 1 h through sand mill, obtains D50=0.46μThe slurry of m, slurry are surpassed through drying
Thin cristobalite powder.
Embodiment 8
Weigh quartz sand 5000g, mineralizer calcium acetate 62.5g, wet-milling mixed 80 meshes, formed uniform quartz sand,
Mineralizer mixture.Mixture is in 1300 DEG C of 3 h of heat preservation, then by obtaining fluffy cristobalite powder, ashlar after room temperature quenching
English conversion ratio is 93.8%, and cristobalite powder handles 5 h through sand mill, obtains D50=0.82μThe ultra-fine cristobalite powder of m.
Claims (7)
1. a kind of method for preparing ultra-fine cristobalite powder with quartz sand, feature include the following steps:
Step 1: using quartz sand as raw material, a certain amount of mineralizer being mixed into quartz sand by certain mode, mixed through ball milling
80 meshes are crossed after even, form uniform quartz sand, mineralizer mixture；
Step 2: mixture is calcined in certain temperature, and then quenching, obtains fluffy cristobalite powder；
Step 3: cristobalite powder obtains ultra-fine cristobalite powder through certain way grinding treatment；
Mineralizer is sodium ethoxide, lithium ethoxide, magnesium ethylate, calcium ethoxide, sodium acetate, lithium acetate, magnesium acetate, acetic acid in the step 1
One of calcium；
The additive amount of the mineralizer is the 0.1~5% of quartz sand weight；
Calcination temperature in the step 2 is 1150~1350 DEG C, and soaking time is 0.5~12 h.
2. according to the method described in claim 1, it is characterized by: the mode that is mixed into the step 1 is dry or wet mixing.
3. according to the method described in claim 1, it is characterized by: the quenching mode in the step 2 is direct room temperature quenching
Or water quenching.
4. according to the method described in claim 1, it is characterized by: grinding mode in the step 3 as dry grinding or wet-milling
Or air-flow crushing, Ball-milling Time are 1~12h.
5. according to the method described in claim 3, it is characterized by: the temperature of the water quenching is 5 ~ 30 DEG C.
6. according to the method described in claim 1, it is characterized by: the quartz sand be converted into the conversion ratio 92 of cristobalite~
99%。
7. according to the method described in claim 1, it is characterized by: the particle of ultra-fine cristobalite powder made from the step 3
Fineness is D50=0.305~0.85 μm.
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| CN110303116A (en) * | 2019-08-11 | 2019-10-08 | 桑超 | A kind of overlay film sand shell mould coating and preparation method thereof |
| CN112938996A (en) * | 2021-04-09 | 2021-06-11 | 佛山市道易生科技有限公司 | Whitening process method of quartz sand/powder |
| CN114455594A (en) * | 2022-02-13 | 2022-05-10 | 段晓文 | Cristobalite prepared by electric melting method |
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| CN107473231A (en) * | 2017-09-19 | 2017-12-15 | 江苏凯达石英股份有限公司 | A kind of processing purifying technique to glass sand mine tailing |
| CN107555442A (en) * | 2017-09-19 | 2018-01-09 | 江苏凯达石英股份有限公司 | A kind of method that glass sand is refined using common quartz sand |
| 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107473231A (en) * | 2017-09-19 | 2017-12-15 | 江苏凯达石英股份有限公司 | A kind of processing purifying technique to glass sand mine tailing |
| CN107555442A (en) * | 2017-09-19 | 2018-01-09 | 江苏凯达石英股份有限公司 | A kind of method that glass sand is refined using common quartz sand |
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Application publication date: 20190423 Assignee: Guangxi Sanhuan Enterprise Group Holding Co.,Ltd. Assignor: JINGDEZHEN CERAMIC INSTITUTE Contract record no.: X2021990000582 Denomination of invention: A method for preparing ultrafine cristobalite powder from quartz sand Granted publication date: 20191022 License type: Exclusive License Record date: 20210922 |
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