CN101367609A - Preparation and purification process for arenaceous quartz and quartz powder, and products produced thereby - Google Patents
Preparation and purification process for arenaceous quartz and quartz powder, and products produced thereby Download PDFInfo
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- CN101367609A CN101367609A CNA200810131071XA CN200810131071A CN101367609A CN 101367609 A CN101367609 A CN 101367609A CN A200810131071X A CNA200810131071X A CN A200810131071XA CN 200810131071 A CN200810131071 A CN 200810131071A CN 101367609 A CN101367609 A CN 101367609A
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Abstract
The invention discloses a preparation and purification process of quartz sand and quartz powder and products thereof. The preparation and purification process of quartz sand comprises raw quartz ore, rough separation, fragmentation, water separation, roasting, water fragmentation, soaking in oxalic acid or citric acid, dry grinding or wet grinding, high-gradient magnetic separation, classification, combined process washing, floatation, deionized water washing, special drying. The preparation and purification process of quartz powder comprises quartz sand flotation, ultra fine grinding (dry grinding or wet grinding ), combined process washing, high-gradient magnetic separation, electrostatic separation, deionized water washing, classification, special drying, and vacuum packing. The quartz sand and quartz powder produced with the process of the invention can not foam in the production of glass and chips, an optical fibre and an optical cable can not be broken, the glass does not have water streaks, and the application area is widened. The quartz sand and the quartz powder is suitable for being applied in the fields of monocrystal line silicon, chips, optical fibre and optical cables, war industry, fine chemistry industry and micro-electronics.
Description
Technical field
The present invention relates to the preparation of a kind of quartz sand and silica powder and purifying technique and products thereof, its product specifically relates to the production and the method for purification of glass sand and high pure and ultra-fine silica powder, so that can be used at chip, silicon single crystal, optical fiber cable, military project, fine chemistry industry and microelectronic.
Background technology
At present, what the production of quartz sand and silica powder and purifying technique generally adopted is: and raw ore roughly selects → and fragmentation → roasting → water is broken → dry grinding or wet-milling → de-iron, make 10-325 purpose quartz sands; Or: quartzy raw ore roughly selects → surface modification → drying of common washing → dry grinding or wet-milling → mechanical de-iron → industrial sulphuric acid processing → machinery, make 10-800 purpose quartz sand and silica powders; Its production and purifying technique are simple, can not effectively remove the parcel impurity of quartz and the pollution impurity of surface impurity and production process, (purity of quartz sand is 99.5%-99.6% and the purity that causes quartz sand and silica powder is not high, the purity of silica powder is 99.1%-99.2%), the fineness of silica powder also has only 800 orders, in glass production, easily bubble, even generation water wave, in the casting applying filler, also easily bubble, influence quality product, can not in chip, silicon single crystal, optical fiber cable, military project, fine chemistry industry and microelectronic, use.
CN1413169A discloses a kind of " synthetic method of silicon dioxide granule, synthetic quartz powder, synthetic quartz glass ", and its objective is provides the manufacture method that can obtain the few synthetic quartz glass of silanol base content with high purity efficiently; Its method is to make the water-containing column dehydration by the moisture content that water-containing column is freezed, thaw, removes to separate ionized water, obtain silicon dioxide granule, again by to silicon dioxide granule wash, roasting makes the silica glass powder, make the water glass dealkalize, add oxygenant and acid, by argon type Zeo-karb, make this silicon-dioxide aqueous gelization, make synthetic quartz powder through washing, roasting again; Its deficiency is, dewatering is difficult to reach the requirement that necessarily contains water quality standard, partly the easy frozen liquid of silica powder is sticking poor, and the water ratio height is washed without deionization, the chemical liquid on silica powder surface has corrosive nature to equipment, influenced the work-ing life of equipment, it is broken not pass through water, and bubble in the silica powder and inclusion impurity difficulty are removed, and the not Ex-all of the chemical liquid of surface attachment, had a strong impact on purity requirement.
Summary of the invention
Purpose of the present invention aims to provide the production and the method for purification of a kind of glass sand and high pure and ultra-fine silica powder, thereby make quartz sand and silica powder because purity is not high, in production application, easily produce water wave and foaming for a long time, a difficult problem that has a strong impact on quality product is solved, and enlarge its Application Areas, satisfied the production requirement of relevant new high-tech products such as chip, silicon single crystal, optical fiber cable, military project, fine chemistry industry and microelectronics.
To achieve these goals, quartz sand of the present invention preparation with purifying technique is: each quartz-like raw ore → roughly select → fragmentation → primary election → roasting → water is broken → and oxalic acid or lemon acidleach → dry grinding or wet-milling → high terraced magnetic magnetic separation → classification → close technology to wash → flotation → deionization washing → special drying → vacuum packaging;
Roughly select: be coarse impurities in each quartz-like raw ore and significantly foreign material removal;
Broken: as to be that the professional crusher of employing is the particle of 0.5-8mm to particle diameter with quartzy crushing raw ore;
Primary election: be meant the artificial hand selection, with the Impurity removal in the quartzy raw ore particle;
Roasting: be meant and adopt professional roasting kiln, place stove to fire in a quartzy raw ore material, 300 ℃ of-1200 ℃ of roasting temperatures 2-8 hours;
Water is broken: be to place cold water to cool off fast quartz particles after the roasting, make quartz particles explosion in water, remove the interior impurity of steam bubble, water wave and inclusion in the quartz crystal, the water wave season crack;
Dry grinding or wet-milling: be meant anhydrous or have under the condition of water, use specific equipment to carry out ore grinding (quartz particles), make 10-325 purpose quartz sands;
High terraced magnetic magnetic separation: be meant that adopting magnetic strength is 50-15000 Gausses' magnetic plant, the irony of polluting in irony in the quartz sand and the production process is removed;
Classification: be the quartz sand that 10-325 purpose quartz sands is divided into 10-50 orders, 60-100 orders, 110-150 orders, 160-200 orders, 210-250 orders, 260-300 orders, the multiple fineness of 310-325 orders by standard;
Closing technology washes: be that the different quartz sand of various order numbers is placed on the different aspects of temperature control reactor, add oxalic acid or citric acid, and other a small amount of adjuvant system, constant temperature is at 60 ℃-90 ℃, reacted 3-8 hours, to remove deleterious trace metal and nonmetallic impurity in the quartz sand;
Flotation: chemical agent after ECDC technology washed and proportion are less than the Impurity removal of water;
Deionization washing: in staticizing the workshop, further, make pH value reach standard with chemical agent and quartz sand surface Impurity removal remaining after the flotation;
Special drying: adopt special equipment, the quartz sand after the deionization dehydration is washed is built in the drying machine staticizing the workshop, carries out drying, makes the glass sand of 10-325 order different stages, and promptly purity is 99.9%-99.995%;
Vacuum-packed: as in staticizing the workshop, the glass sand of 10-325 order different stages to be carried out vacuum packaging respectively, avoid atmospheric pollution.
Silica powder of the present invention preparation with purifying technique is: with the quartz sand after the flotation → ultra-fine mill (dry grinding or wet-milling) → close technology to wash → high terraced magnetic magnetic separation → electrostatic separation → deionization washing → classification → special drying → vacuum packaging;
Ultra-fine mill (dry grinding or wet-milling): be meant anhydrous or have under the condition of water, quartz sand is levigate to 325-4000 purpose ultrafine quartz powders;
Classification: adopt waterpower swirling flow machine, by carrying out classification between standard regions, as 325-400 orders, 400-500 orders, the rest may be inferred with 325-4000 purpose ultrafine quartz powders;
Closing technology washes: be that ultrafine quartz powder with different stage places respectively on the different aspects of temperature control reactor, add oxalic acid or citric acid, constant temperature is at 70 ℃---and 100 ℃, reacted 2-8 hours, remove deleterious trace metal and nonmetallic impurity in the ultrafine quartz powder;
High terraced magnetic magnetic separation: be meant that adopting magnetic strength is 50-15000 Gausses' magnetic plant, the micro-irony in the ultrafine quartz powder is removed;
Electrostatic separation: be meant the detrimental impurity of trace in the ultrafine quartz powder is removed;
Deionization washing: in staticizing the workshop, remove with closing chemical agent after technology is washed and harmful trace impurity on silica powder surface;
Special drying: adopt special equipment, ultrafine quartz powder after the deionization washing is inserted in staticizing the workshop in the drying machine, carry out drying, make the high pure and ultra-fine silica powder of 325-4000 order different stages, its purity is 99.9%-99.9996%, and water content is 0.003%-0.01%;
Really wear packing: various other ultrafine quartz powders of level are carried out vacuum packaging respectively, avoid atmospheric pollution.
Close the specific equipment that technology washes and the special equipment of special drying, all are the metallic surfaces that contact with quartz sand or silica powder at existing temperature control reactor and drying machine, adopt high silicon materials of liner or stupalith or insulation fat material, avoid the pollution of equipment quartz sand or silica powder.
The specific equipment of dry grinding or wet-milling also is that the mill spare that will have dry grinder or wet wheeling machine now adopts high silicon materials to manufacture, and avoids grinding the pollution of part to quartz sand or silica powder.
The present invention compared with prior art has following excellent effect:
1) in production and purifying technique, adopted the specific equipment of the high silicon materials of liner, avoided the pollution of equipment, thereby made the raising of purity that the guarantee on the hardware arranged quartz sand or silica powder;
2) high terraced magnetic magnetic separation is to adopt the high-frequency and high-voltage high-gradient electric field to replace electrostatic field, and the effect of utilizing the mineral specific inductivity to change with electric field frequency improves ore dressing resolving power, makes that irony is able to Ex-all in quartz sand or the silica powder, has guaranteed high purity from processing sequence;
3) ultra-fine mill is the ultra-fine mill of steam flow that adopts the high silicon materials of band liner, makes the fineness of silica powder reach the requirement that relevant new high-tech product is used;
4) close technology and wash and broken traditional sulfuric acid or hydrochloric acid production ore-dressing technique, adopt oxalic acid or citric acid, saved material, reduced cost, avoided pollution, reach national requirements for environmental protection, improved ore dressing rate and precision, prescription rationally;
5) use product of the present invention, the glass and the chip of production are non-foaming, and optical fiber cable can not break, and glass does not have water wave, use on military project and can satisfy hardness height, requirement that purity is high, and Application Areas is expanded;
6) whole processing sequence reprogramming according to circumstances also, and do not influence quality product.
Embodiment
Quarrying English raw ore is after roughly selecting, be crushed to 1-4 tons in the particle quartz of 1-10mm, behind the artificial hand selection, place the roasting kiln to fire, 300 ℃ of-1200 ℃ of roasting temperatures 2-8 hours, place water cooling pond to cool off fast in the particle quartz after the roasting, make quartz particles explosion in water, remove the steam bubble in the quartz crystal, impurity in water wave and the inclusion, the citric acid or the oxalic acid solution that add 600L-2400L again, under 40 ℃-60 ℃ temperature, soaked 0.5-2 hours, afterwards, the particle quartz placed in dry grinder or the wet wheeling machine roughly grind, make 10-325 purpose quartz sands, with magnetic strength is 50-15000 Gausses' high-gradient magnetic separation apparatus, remove the irony in the quartz sand, be divided into 10-50 orders by standard then, 60-100 orders, 110-150 orders, 160-200 orders, 210-250 orders, 260-300 orders, the quartz sand of the multiple fineness of 310-325 orders, the quartz sand of different stage is placed respectively on the different aspects of temperature control reactor, add 200L-700L oxalic acid or citric acid solution, constant temperature is at 60 ℃-90 ℃, reaction was also stirred 3-8 hours, remove deleterious trace metal and nonmetallic impurity in the quartz sand, add the water flotation afterwards, remove the chemical agent close after technology is washed and proportion, staticizing the workshop again less than the impurity of water, the washing of employing deionization, make the Impurity removal of chemical agent remaining after the flotation and quartz sand surface clean, pH value reaches standard, afterwards, the quartz sand of cleaning is placed the drying machine that is lined with high silicon materials, carry out drying, thereby make the glass sand of 10-325 order different stages, its purity is 99.9%-99.995%, in staticizing the workshop, carrying out vacuum packaging respectively is the finished product glass sand at last.
The further more ultra-fine mill of quartz sand after the flotation is promptly dry grinded or wet-milling, adopt the ultra-fine mill of steam flow of band liner catalytic body, anhydrous or have under the condition of water, quartz sand (10-325 order) is levigate to 325-4000 purpose ultrafine quartz powders, afterwards, adopt waterpower swirling flow machine with 325-4000 purpose ultrafine quartz powders by carrying out classification between standard regions, as 800-900 orders, 900-1000 orders, 2000-2100 orders, 3000-3100 orders, 3900-4000 orders, the rest may be inferred; Then the ultrafine quartz powder of different stage is placed respectively on the different aspects of temperature control reactor, add 150L-600L oxalic acid or citric acid solution, constant temperature is at 70 ℃-100 ℃, reaction was also stirred 2-8 hours, remove deleterious trace metal and nonmetallic impurity in the ultrafine quartz powder, be that 50-15000 Gausses' high-gradient magnetic separation apparatus carries out high terraced magnetic magnetic separation with magnetic strength again, remove the micro-irony in the ultrafine quartz powder, afterwards, remove the detrimental impurity of trace in the ultrafine quartz powder with electrostatic separation, in staticizing the workshop, to wash with deionized water, chemical agent after technology is washed and harmful trace impurity on silica powder surface are closed in Ex-all, afterwards, place the drying machine of the high silicon materials of liner to carry out drying ultrafine quartz powder, make the high pure and ultra-fine silica powder of 325-4000 order different stages, its purity is 99.9%-99.9996%, water ratio is 0.003%-0.01%, at last, various other silica powders of level are carried out vacuum packaging, i.e. finished product high pure and ultra-fine silica powder respectively.
Above-mentioned processing sequence can be according to circumstances and reprogramming, do not influence the quality of product.
Claims (9)
1. the preparation of a quartz sand and purifying technique, be each quartz-like raw ore → roughly select → fragmentation → primary election → roasting → water is broken, de-iron after dry grinding or wet-milling, after it is characterized in that water is broken, employing oxalic acid or lemon acidleach → dry grinding or wet-milling → high terraced magnetic magnetic separation → classification → close technology to wash → flotation → deionization washing → special drying → vacuum packaging.
2. the preparation of quartz sand according to claim 1 and purifying technique, it is characterized in that it is through being to add 600L-2400L oxalic acid or citric acid solution in 1-10mm particle quartz at 14 tons grain that described oxalic acid or citric acid solution soak, constant temperature soaked 0.5-2 hours between 40 ℃-60 ℃.
3. the preparation of quartz sand according to claim 1 and purifying technique, it is characterized in that described to close that technology washes be that 1-4 tons of different quartz sands of order number are placed respectively on the different aspects of temperature control reactor, add 200L-700L oxalic acid or citric acid solution, constant temperature is at 60 ℃-90 ℃, stirring reaction 3-8 hours.
4. the preparation of quartz sand according to claim 1 and purifying technique, the purity that it is characterized in that 10-325 order quartz sands that described technology is made is 99.9%-99.995%.
5. the preparation of a silica powder and purifying technique is characterized in that the quartz sand → ultra-fine mill (dry grinding or wet-milling) → close technology to wash → high terraced magnetic magnetic separation → clean electric separation → deionization washing → classification → special drying → vacuum packaging after the described flotation.
6. the preparation of silica powder according to claim 5 and purifying technique is characterized in that described ultra-fine mill is that 10-325 purpose quartz sands are levigate to 325-4000 purpose ultrafine quartz powders.
7. the preparation of silica powder according to claim 5 and purifying technique, it is characterized in that described to close that technology washes be that ultrafine quartz powder with 1-4 tons of different meshes places respectively on the different aspects of temperature control reactor, add 150L-600L oxalic acid or citric acid, constant temperature between 70 ℃-100 ℃, stirring reaction 2-8 hours.
8. the preparation of silica powder according to claim 5 and purifying technique, the purity that it is characterized in that the ultrafine quartz powder that described technology is made is 99.9%-99.9996%.
9. according to the preparation and the purifying technique of claim 1 and 5 described quartz sands and silica powder, it is characterized in that described technological process can change.
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CN101844886A (en) * | 2010-04-22 | 2010-09-29 | 裴海明 | Method for producing sand by using sandstone |
WO2011003777A1 (en) * | 2009-07-09 | 2011-01-13 | Qsil Ag Quarzschmelze Ilmenau | Method for producing a highly pure quartz granulate |
CN101503194B (en) * | 2009-03-02 | 2011-03-30 | 申士富 | Preparation of active high purity silica flour |
CN102070150A (en) * | 2010-09-08 | 2011-05-25 | 刘少云 | Processes for preparing and purifying quartz sand and quartz powder and products thereof |
CN102126727A (en) * | 2010-11-25 | 2011-07-20 | 黄山恒源石英材料有限公司 | Method for purifying vein quartz under non-pickling condition |
CN102180584A (en) * | 2011-02-18 | 2011-09-14 | 银锐明 | Method for removing gas-liquid inclusion and impurity during high-purity quartz sand production |
CN102225766A (en) * | 2011-03-29 | 2011-10-26 | 东海县圣达石英制品有限公司 | Preparation method for ultra pure silicon material used in solar energy photovoltaic industry |
CN102417184A (en) * | 2011-08-26 | 2012-04-18 | 田辉明 | Method for preparing high-purity ultrafine silicon powder from vein quartz |
CN103318898A (en) * | 2012-03-20 | 2013-09-25 | 东海县圣达石英制品有限公司 | Micron-scale low hydroxyl OH<-> crystal powder production process method |
CN103332694A (en) * | 2013-06-09 | 2013-10-02 | 宁夏富乐德石英材料有限公司 | Preparation method of raw material sand for quartz crucible |
CN103613103A (en) * | 2013-12-04 | 2014-03-05 | 南京工业大学东海先进硅基材料研究院 | Method for preparing filler-level silicon micropowder by using waste quartz crucibles as raw materials |
CN104071792A (en) * | 2013-03-26 | 2014-10-01 | 南京大学连云港高新技术研究院 | Preparing process of high-purity quartz sand used for quartz steelyard weight production |
CN104150489A (en) * | 2014-07-23 | 2014-11-19 | 湖南鑫生矿冶废弃物综合利用科技有限公司 | Quartz ore purification method and quartz product thereof |
CN105948062A (en) * | 2016-04-28 | 2016-09-21 | 江苏凯达石英有限公司 | Preparation method of highly pure quartz sands |
CN106645382A (en) * | 2017-01-19 | 2017-05-10 | 安徽科技学院 | Method for detecting content of iron in quartz sand by applying isothermal remanent magnetization |
CN106753317A (en) * | 2016-11-21 | 2017-05-31 | 四川南联环资科技股份有限公司 | A kind of method that utilization quartz tail sand produces oil well proppant |
CN107032600A (en) * | 2017-03-20 | 2017-08-11 | 凯盛石英材料(黄山)有限公司 | A kind of method that utilization vein quartz tailings prepares TFT LCD silicon powders |
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CN111393022A (en) * | 2020-03-23 | 2020-07-10 | 黄冈师范学院 | Preparation method of high-purity low-hydroxyl quartz glass raw material |
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CN112897877A (en) * | 2021-02-02 | 2021-06-04 | 台玻安徽玻璃有限公司 | Separation and purification method of high purity quartz material for float glass |
CN115849393A (en) * | 2022-08-01 | 2023-03-28 | 西南科技大学 | High-purity quartz and preparation method thereof |
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2008
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WO2011003777A1 (en) * | 2009-07-09 | 2011-01-13 | Qsil Ag Quarzschmelze Ilmenau | Method for producing a highly pure quartz granulate |
CN101844886A (en) * | 2010-04-22 | 2010-09-29 | 裴海明 | Method for producing sand by using sandstone |
CN102070150A (en) * | 2010-09-08 | 2011-05-25 | 刘少云 | Processes for preparing and purifying quartz sand and quartz powder and products thereof |
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CN107539992A (en) * | 2017-09-29 | 2018-01-05 | 江苏闽江矿业有限公司 | A kind of preparation method of glass sand |
CN111393022A (en) * | 2020-03-23 | 2020-07-10 | 黄冈师范学院 | Preparation method of high-purity low-hydroxyl quartz glass raw material |
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