CN101254923B - Method for preparing high-purity ground quartz - Google Patents
Method for preparing high-purity ground quartz Download PDFInfo
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- CN101254923B CN101254923B CN2008100232836A CN200810023283A CN101254923B CN 101254923 B CN101254923 B CN 101254923B CN 2008100232836 A CN2008100232836 A CN 2008100232836A CN 200810023283 A CN200810023283 A CN 200810023283A CN 101254923 B CN101254923 B CN 101254923B
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Abstract
The invention provides a method for preparing high purity quartz flour, which belongs to the technology field of inorganic material impurity removal. The preparation method includes pulverizing high-quality vein quartz (SiO2 is more than or equal to 99%) as the material, adding NaCl, calcining at high temperature, quenching, floating, acid dipping, complexing, washing and drying to obtain high purity quartz flour. The product prepared in the method complies with the requirements for the high grade quartz material in electronic industry and optical communication industry owing to the SiO2 content of up to 99.99% and the impurity content of less than 100ppm.
Description
Technical field:
The invention belongs to inorganic materials impurity removing technology field, being specifically related to a kind of vein quartz that adopts is the method for feedstock production high-purity ground quartz.
Background technology:
High-purity ground quartz has good optics, thermal characteristics, chemical stability and radiation-resistant property, thereby has purposes widely at aspects such as electronic industry, optical communication, military projects.
Along with the development in fields such as electronic industry, optical communication, laser, optics, more and more higher to the requirement of high-purity ground quartz, demand is also increasing.Melting crystal and high-quality mineral crystal are the main raw materials of domestic and international high purity quartz material always, these supply of raw material worsening shortages.China's quartzite class rich in mineral resources, but owing to the association of plurality of impurities mineral is arranged during gangue Yingcheng ore deposit, and kind is because of becoming the ore deposit environment different, and general major impurity mineral have feldspar, mica group, clay class, rhombohedral iron ore etc.At present adopting vein quartz is the feedstock production quartz micropowder, and its technology is: raw material → coarse crushing → in broken → pickling → washing → drying → classification → product.SiO in the silica powder that this technology obtains
2Content is 99.0～99.6%, and SiO in the purified high purity quartz
2Content should reach 99.99%, and the impurity element total content is less than 100ppm.
Summary of the invention:
The purpose of this invention is to provide a kind of is the method for feedstock production high-purity ground quartz with the vein quartz.These method concrete steps are as follows:
(1) calcining
The employing vein quartz is a raw material, is crushed to 200～400 orders, adds an amount of NaCl solid and mixes, and the NaCl solid amount that is added is 2～4% of a vein quartz quality, calcines in 800～850 ℃ 2～4 hours;
(2) quenching and flotation
Material after the above-mentioned calcining poured in the flotation fluid while hot quench, used flotation fluid is the mixing solutions of 0.2～0.5g/kg amino dodecane and 0.2～0.5g/kg Sodium dodecylbenzene sulfonate, adjusting the pH value with dilute sulphuric acid is 2～3, the mass ratio of flotation fluid and silica powder is 3～10: 1, the flotation time of silica powder in flotation fluid is 3～10 minutes, and temperature keeps 10～70 ℃;
(3) acidleach
The silica powder of above-mentioned flotation fluid bottom is transferred in the mix acid liquor, soaked 6～12 hours at 10～60 ℃, used mixing acid is the mixing solutions of 10～20% hydrochloric acid and 1～5% hydrofluoric acid, and the mass ratio of mixing acid and silica powder is 2～6: 1;
(4) complexing
Silica powder after the above-mentioned acidleach is transferred in the complex liquid, soaked 3～8 hours at 10～60 ℃, used complex liquid is 0.2～1% citric acid and 0.2～1% lauric mixing solutions, and the mass ratio of complex liquid and silica powder is 1～5: 1;
(5) washing, drying
Silica powder after the above-mentioned complex liquid immersion is taken out, use deionized water wash, drying obtains the high-purity ground quartz product, SiO in the product
2Content is greater than 99.99%, and content of impurities is less than 100ppm.
Preparation method provided by the present invention obtains producing electronic-grade and microelectronics level high-purity ground quartz by the processing to the vein quartz powder, and its preparation technology adopts and adds the high-temperature calcination of NaCl solid, quenching, flotation, acidleach and complexing etc., to remove impurity, makes SiO
2Content reaches 99.99%, and total impurities content is less than 100ppm, and excellent product performance can be applicable to microelectronics industry and optical communication industry etc.
Embodiment:
Embodiment 1:
(1) calcining
The vein quartz nugget that adopts area, Anqing, Anhui Province to provide, SiO
2Content is greater than 99%, and foreign matter content through fragmentation and ball milling, obtains 200 purpose silica powders less than 1%, adds the NaCl solid of weight of material 2% in the silica powder after pulverizing, and mixes, and calcining is 2 hours in 850 ℃.
(2) quenching and flotation
Material after the above-mentioned calcining poured in the flotation fluid while hot quench, used flotation fluid is the mixing solutions of 0.2g/kg amino dodecane and 0.2g/kg Sodium dodecylbenzene sulfonate, adjusting the pH value with dilute sulphuric acid is 2, the mass ratio of flotation fluid and silica powder is 10: 1, the flotation time of silica powder in flotation fluid is 10 minutes, and temperature keeps 10 ℃.
(3) acidleach
The silica powder of above-mentioned flotation fluid bottom is transferred in the mixing acid that contains 10% hydrochloric acid and 5% hydrofluoric acid soaked 10 hours, 30 ℃ of acidleach temperature, the mass ratio of mixing acid and silica powder is 2: 1.
(4) complexing
Silica powder after the above-mentioned acidleach is transferred in the complex liquid, and adopting 0.2% citric acid and 0.2% lauric mixed solution is complexing agent, and complexing agent and silica powder mass ratio are 5: 1, and temperature remains on 60 ℃, soaks 8 hours.
(5) washing, drying
Silica powder after the above-mentioned complex liquid immersion is taken out, use deionized water wash, the consumption of deionized water is 10: 1 with the ratio of product, and the product after the washing is dried in 120 ℃ loft drier, obtains the high-purity ground quartz product, SiO in the product
2Content is greater than 99.99%, and content of impurities is less than 100ppm.
The main quality index of this embodiment prepared high-purity silica powder product is as follows:
SiO
2≥99.99％；Fe：1.6ppm；Al：16ppm；K：2ppm；Na：6ppm；Mg：1ppm；Ti：5ppm；Ca：2ppm；Cu：0.5ppm；Pb：0.01ppm；Mn：0.05ppm。
Embodiment 2:
(1) calcining
The vein quartz nugget that adopts area, Anqing, Anhui Province to provide, SiO
2Content is greater than 99%, and foreign matter content through fragmentation and ball milling, obtains 300 purpose silica powders less than 1%, adds the NaCl solid of weight of material 3% in the silica powder after pulverizing, and mixes, and calcining is 4 hours in 800 ℃.
(2) quenching and flotation
Material after the above-mentioned calcining poured in the flotation fluid while hot quench, used flotation fluid is the mixing solutions of 0.5g/kg amino dodecane and 0.5g/kg Sodium dodecylbenzene sulfonate, adjusting the pH value with dilute sulphuric acid is 3, the mass ratio of flotation fluid and silica powder is 3: 1, the flotation time of silica powder in flotation fluid is 3 minutes, and temperature keeps 70 ℃.
(3) acidleach
The silica powder of above-mentioned flotation fluid bottom is transferred in the mixing acid that contains 20% hydrochloric acid and 1% hydrofluoric acid soaked 6 hours, 60 ℃ of acidleach temperature, the mass ratio of mixing acid and silica powder is 6: 1.
(4) complexing
Silica powder after the above-mentioned acidleach is transferred in the complex liquid, and adopting 1% citric acid and 1% lauric mixed solution is complexing agent, and complexing agent and silica powder mass ratio are 1: 1, and temperature remains on 10 ℃, soaks 3 hours.
(5) washing, drying
Silica powder after the above-mentioned complex liquid immersion is taken out, use deionized water wash, the consumption of deionized water is 10: 1 with the ratio of product, and the product after the washing is dried in 120 ℃ loft drier, obtains the high-purity ground quartz product, SiO in the product
2Content is greater than 99.99%, and content of impurities is less than 100ppm.
The main quality index of this embodiment prepared high-purity silica powder product is as follows:
SiO
2≥99.99％；Fe：1.4ppm；Al：18ppm；K：1.2ppm；Na：3ppm；Mg：2ppm；Ti：4ppm；Ca：3ppm；Cu：0.5ppm；Pb：0.01ppm；Mn：0.06ppm。
Embodiment 3:
(1) calcining
The vein quartz nugget that adopts area, Anqing, Anhui Province to provide, SiO
2Content is greater than 99%, and foreign matter content through fragmentation and ball milling, obtains 400 purpose silica powders less than 1%, adds the NaCl solid of weight of material 4% in the silica powder after pulverizing, and mixes, and calcining is 3 hours in 830 ℃.
(2) quenching and flotation
Material after the above-mentioned calcining poured in the flotation fluid while hot quench, used flotation fluid is the mixing solutions of 0.3g/kg amino dodecane and 0.3g/kg Sodium dodecylbenzene sulfonate, adjusting the pH value with dilute sulphuric acid is 2.5, the mass ratio of flotation fluid and silica powder is 5: 1, the flotation time of silica powder in flotation fluid is 6 minutes, and temperature keeps 40 ℃.
(3) acidleach
The silica powder of above-mentioned flotation fluid bottom is transferred in the mixing acid that contains 15% hydrochloric acid and 2% hydrofluoric acid soaked 12 hours, 10 ℃ of acidleach temperature, the mass ratio of mixing acid and silica powder is 4: 1.
(4) complexing
Silica powder after the above-mentioned acidleach is transferred in the complex liquid, and adopting 0.5% citric acid and 0.5% lauric mixed solution is complexing agent, and complexing agent and silica powder mass ratio are 3: 1, and temperature remains on 30 ℃, soaks 6 hours.
(5) washing, drying
Silica powder after the above-mentioned complex liquid immersion is taken out, use deionized water wash, the consumption of deionized water is 10: 1 with the ratio of product, and the product after the washing is dried in 120 ℃ loft drier, obtains the high-purity ground quartz product, SiO in the product
2Content is greater than 99.99%, and content of impurities is less than 100ppm.
The main quality index of this embodiment prepared high-purity silica powder product is as follows:
SiO
2≥99.99％；Fe：0.7ppm；Al：16ppm；K：0.8ppm；Na：1.2ppm；Mg：0.8ppm；Ti：2ppm；Ca：2.8ppm；Cu：0.7ppm；Pb：0.01ppm；Mn：0.02ppm。
Claims (1)
1. method for preparing high-purity ground quartz is characterized in that these method concrete steps are as follows:
(1) calcining
The employing vein quartz is a raw material, is crushed to 200～400 orders, adds an amount of NaCl solid and mixes, and the NaCl solid amount that is added is 2～4% of a vein quartz quality, calcines in 800～850 ℃ 2～4 hours;
(2) quenching and flotation
Material after the above-mentioned calcining poured in the flotation fluid while hot quench, used flotation fluid is the mixing solutions of 0.2～0.5g/kg amino dodecane and 0.2～0.5g/kg Sodium dodecylbenzene sulfonate, adjusting the pH value with dilute sulphuric acid is 2～3, the mass ratio of flotation fluid and silica powder is 3～10: 1, the flotation time of silica powder in flotation fluid is 3～10 minutes, and temperature keeps 10～70 ℃;
(3) acidleach
The silica powder of above-mentioned flotation fluid bottom is transferred in the mix acid liquor, soaked 6～12 hours at 10～60 ℃, used mixing acid is the mixing solutions of 10～20% hydrochloric acid and 1～5% hydrofluoric acid, and the mass ratio of mixing acid and silica powder is 2～6: 1;
(4) complexing
Silica powder after the above-mentioned acidleach is transferred in the complex liquid, soaked 3～8 hours at 10～60 ℃, used complex liquid is 0.2～1% citric acid and 0.2～1% lauric mixing solutions, and the mass ratio of complex liquid and silica powder is 1～5: 1;
(5) washing, drying
Silica powder after the above-mentioned complex liquid immersion is taken out, use deionized water wash, drying obtains the high-purity ground quartz product, SiO in the product
2Content is greater than 99.99%, and content of impurities is less than 100ppm.
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| CN2008100232836A CN101254923B (en) | 2008-04-07 | 2008-04-07 | Method for preparing high-purity ground quartz |
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| CN101254923B true CN101254923B (en) | 2011-05-04 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481203B (en) * | 2009-02-19 | 2011-03-02 | 申士富 | Preparation of fused silica material |
| CN102432022B (en) * | 2011-08-26 | 2013-03-13 | 田辉明 | Method for producing ultra-pure quartz sand by vein quartz and high-temperature chlorination device |
| CN102674377B (en) * | 2012-05-04 | 2013-11-20 | 武汉理工大学 | Quartz crystal type conversion metal element gasification integration purification method |
| CN102674372B (en) * | 2012-05-04 | 2013-12-25 | 武汉理工大学 | Purification method for high-purity quartz with ultra-low metal elements |
| CN102897993A (en) * | 2012-10-25 | 2013-01-30 | 中国地质大学（北京） | Method for preparing high-purity quartz sands by using natural vein quartz ores |
| CN103539129B (en) * | 2013-10-30 | 2015-11-11 | 武汉大学 | A kind of method of purification of silicon-dioxide |
| CN104743779B (en) * | 2015-03-23 | 2017-03-29 | 连云港福东正佑照明电器有限公司 | Suitable for the preparation method of the low deformation rate crucible quartz raw material of monocrystalline production |
| CN110143596A (en) * | 2018-02-12 | 2019-08-20 | 韩小凤 | The method for purifying earth silicon material and its application in glass sand preparation |
| CN109293225A (en) * | 2018-11-08 | 2019-02-01 | 连云港善发石英制品有限公司 | A kind of production method of thick-walled quartz glass tubes |
| CN111573680A (en) * | 2020-05-20 | 2020-08-25 | 安徽科技学院 | Method for removing iron in quartz sand |
| CN112916199A (en) * | 2021-02-05 | 2021-06-08 | 中国科学技术大学 | Quartz raw material purification method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5037625A (en) * | 1990-02-06 | 1991-08-06 | The Feldspar Corporation | Purified quartz and process for purifying quartz |
| CN1891625A (en) * | 2005-07-08 | 2007-01-10 | 中南大学 | Method for producing superfine high-purity silicon dioxide |
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2008
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5037625A (en) * | 1990-02-06 | 1991-08-06 | The Feldspar Corporation | Purified quartz and process for purifying quartz |
| CN1891625A (en) * | 2005-07-08 | 2007-01-10 | 中南大学 | Method for producing superfine high-purity silicon dioxide |
Non-Patent Citations (2)
| Title |
|---|
| 沈久明.石英微粉提纯研究.《非金属矿》.2006,第29卷(第4期),第39-41页. * |
| 金达表等.高纯石英的加工工艺研究.《中国非金属矿工业导刊》.2004,(第4期),第44-46,48页. * |
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Assignee: Huangshan Hengyuan Quartz Material Co.,Ltd. Assignor: Anhui gifted Biotechnology Co., Ltd.|Anhui University of Technology Contract record no.: 2011340000175 Denomination of invention: Method for preparing high-purity ground quartz Granted publication date: 20110504 License type: Exclusive License Open date: 20080903 Record date: 20110726 |
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Assignee: Huangshan Hengyuan Quartz Material Co.,Ltd. Assignor: Anhui gifted Biotechnology Co., Ltd.|Anhui University of Technology Contract record no.: 2011340000413 Denomination of invention: Method for preparing high-purity ground quartz Granted publication date: 20110504 License type: Exclusive License Open date: 20080903 Record date: 20110926 |
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