CN1557881A - Method for preparing superfine high-purity quartz material from vein quartz - Google Patents
Method for preparing superfine high-purity quartz material from vein quartz Download PDFInfo
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- CN1557881A CN1557881A CNA2004100140588A CN200410014058A CN1557881A CN 1557881 A CN1557881 A CN 1557881A CN A2004100140588 A CNA2004100140588 A CN A2004100140588A CN 200410014058 A CN200410014058 A CN 200410014058A CN 1557881 A CN1557881 A CN 1557881A
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Abstract
The superfine high purity quartz material preparing process with high quality vein quartz as material includes coarse crushing, electrostatic selection, superfine crushing, microwave treatment, complexing to eliminate impurity, post-treatment and other steps. The produced electronics level and microelectronics level superfine and high purity quartz material has SiO2 content up to 99.99 %, impurity content less than 100 ppm, size of 800-2500 mesh and excellent performance, and may be used in high grade plastic sealing material for electronic element, microelectronic element and integrated circuit.
Description
Technical field
The present invention relates to a kind of ultra-fine high purity quartz preparation methods, being specifically related to a kind of is the method for the ultra-fine high purity quartz material of feedstock production with the vein quartz.This ultra-fine high purity quartz material is applied to the fields such as high-grade capsulation material of electronic component, microelectronic element and unicircuit.
Background technology
Ultra-fine high-purity ground quartz possesses the excellent in chemical physical property, fusing point is at 1715 ℃, the Structure Conversion temperature of alpha-beta is 573 ℃, no cleavage, have tool shelly fracture, have fabulous chemical stability, high dielectric voltage withstand ability, voltage breakdown 32-34KV/mm, low-thermal-expansion is applied to unicircuit, microelectronic product, capsulation material etc. as the high-quality stopping composition.
Along with new high-tech industry fast developments such as optical fiber industry, electronic industry, microelectronics industry, more and more higher to the requirement of ultra-fine high purity quartz material, demand is also increasing.Traditional industry generally adopts the high-quality mineral crystal to process the high purity quartz product as raw material, but high-quality mineral crystal resource shortage, and the cost height.China's quartzite class Mineral resources are extremely abundant, and these class mineral generally can only be used as the silicon raw material in the past, were applied to conventional industries such as glass industry, building materials industry, chemical industry.But once had employing high-quality natural quartz mineral aggregate to make the feedstock production quartz micropowder, its technical process is: raw material (crystalline, vein quartz) → coarse crushing → in broken → pickling → washing → drying → dry method superfine grinding → classification → product.Because 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, general major impurity mineral have feldspar, mica group, clay class, carbonate etc., and all the other contain a small amount of magnetite, limonite, ilmenite, pyrite, rhombohedral iron ore, zircon, phosphatic rock etc.Therefore, the shortcoming that adopts this method to produce is: 1, SiO
2Content is 99.0%-99.6%, whiteness about 90, and specific conductivity 5-40 μ sm, the product precision is low, and is of poor quality, is difficult to satisfy the needs of high-precision electronics, microelectronic product, and it is bigger to want further to improve the technical difficulty of quartz material purity.2, water easily causes environmental pollution in the washing of pickling operation.3, the whole production flow process is poor to constant product quality control, unstable product quality.
The purpose of this invention is to provide that a kind of to adopt homemade high-quality vein quartz be the novel method of the ultra-fine high purity quartz material of feedstock production.
Summary of the invention
For achieving the above object, the technical solution used in the present invention is: a kind of method that adopts vein quartz to prepare ultra-fine high purity quartz material, and its content is: the employing vein quartz is a raw material, follows these steps to be prepared:
(1), the raw material mineral are pulverized, associated mineral and quartz are dissociated, and meet electrostatic separation technology selected material granularity requirement;
(2), employing electrostatic separation method is carried out the physics removal of impurities to the material after pulverizing, removal material andesine class, mica group impurity;
(3), the material after the static removal of impurities is carried out superfine grinding, grinding particle size is 800～2500 orders;
(4), the material after adopting high-gradient magnetic method to superfine grinding carries out the physics removal of impurities, removes magnetite, the strong magnetic of ilmenite class and weak magnetic mineral;
(5), the material after adopting microwave to high-gradient magnetic separation handles, activator metal class foreign ion improves the foreign ion activity;
(6), the material after adopting complexometry to microwave treatment carries out chemical subtraction, wherein, complexing agent and metal ion carry out complex reaction, generate water-soluble complex compound, remove residual impurities such as clay mineral, carbonate, metal oxide then by the solid, liquid separation method;
(7), the solid materials after separating is carried out aftertreatment and get finished product.
The related content of technique scheme is explained as follows:
1, major ingredient is a vein quartz in the vein quartz mineral, and this quartz is a kind of crystal quartz (and fused quartz is noncrystalline quartz).
2, in order to make the better effects if of above-mentioned the first step coarse crushing, earlier the raw material mineral are carried out high-temperature calcination before pulverizing, shrend is then then pulverized.It is 40～160 orders generally speaking that described electrostatic separation technology requires selected material granularity.
3, dry method and two kinds of technologies of wet method are adopted in above-mentioned the 3rd step superfine grinding, and dry ground adopts airflow milling, and wet pulverization adopts ultra-fine homogenous medium mill.
4, after above-mentioned the 3rd step superfine grinding, then material is carried out stage treatment.
5, in above-mentioned second step, described electrostatic separation is according to the different minerals electrical property difference, carries out isolating method in high-voltage electric field.
6, in above-mentioned the 4th step, described high-gradient magnetic separation is in uneven high magnetic field intensity (1-2 tesla) magnetic field, utilizes the magnetic contrast between the mineral to make different minerals realize the method for sorting.For raw material mineral of the present invention, the quartzy non magnetic ore that belongs to; The magnetite of association, pyrrhotite, maghemite belong to strongly magnetic mineral; The rhombohedral iron ore of association, limonite, spathic iron ore, ilmenite, network iron ore, mica, monazite, chlorite belong to weak magnetic mineral.
7, microwave is a kind of high-frequency hertzian wave (ultrahigh-frequency microwaves of per second 2,400,000,000 543 magnetic), in above-mentioned the 5th step, described microwave treatment is to utilize the penetrance and the absorptivity of microwave, make the metal ion between quartz crystal, slit, quick oscillation, off normal, the active raising, be convenient to next step complexing and handle, as the treatment technology that gives of complexing processing.
8, in above-mentioned the 6th step, it is to adopt complexing agent such as oxalic acid, citric acid and sodium salt thereof, HF, EDTA-sodium salt, carry out complexing with iron, sodium, lead, calcium, magnesium plasma in the quartz that described complexing is handled, and generates water-soluble stable comple.
9, above-mentioned the 7th step aftertreatment is mainly washing and dried for two steps, and wherein, washing step is to adopt the deionized water wash solid materials, to reduce the electric conductivity of material.
Principle of work of the present invention is: adopt advanced technology to remove impurity and purify and superfine grinding, superfine grinding will be adopted dry method and wet method super-fine disintegrating apparatus, and dry ground adopts airflow milling, and wet pulverization adopts ultra-fine homogenous medium mill.Removing impurity adopts the electrostatic separation method to remove mica group, feldspathoid; Adopt high gradient magnetic separator to remove magnetite, the strong magnetic of ilmenite class and weak magnetic mineral: to adopt microwave treatment and complexometry to remove residual impurities such as clay mineral, carbonate, metal oxide, make product reach ultra-fine high-purity effect.Conclusion is got up, and its gordian technique content is:
1., electrostatic separation method is removed mica group, feldspar impurity technology;
2., microwave treatment activator impurity ion, improve the foreign ion activity;
3., complexometry is removed microwave treatment activated foreign ion;
4., high-gradient magnetic method is removed magnetite, ilmenite class magnetic impurity mineral;
5., superfine technique;
6., deionized water wash reduces the electric conductivity technology.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1, to adopt homemade high-quality vein quartz ore deposit be raw material in the present invention, electronic-grade and the ultra-fine high purity quartz novel material of microelectronics level are produced in research and development, its preparation technology adopts modern techniquies such as electrostatic separation method, high-gradient magnetic method, microwave treatment and complexometry to remove impurity, make SiO2 content reach 99.99-99.999%, foreign matter content＜100ppm, granularity 800-2500 order, meet electronic-grade, the service requirements of microelectronics level, product with its excellent performance applications in high-grade capsulation material of electronic component, microelectronic element and unicircuit etc.
2, the present invention prepares the high purity quartz product with the vein quartz ore deposit, can increase substantially quartzy value-added content of product, and raw material is provided convenience low price, alternative import, the demand of adaptation China's electronic industry and microelectronics industry development.
3, the present invention makes raw material with high-quality vein quartz mineral aggregate, relative mineral crystal, and aboundresources, and cost is low.
4, the present invention adopts the electrostatic separation method in impurity elimination is purified in high-voltage electric field, utilize difference quartzy and impure mineral (mica, feldspar, metal oxide etc.) electrical performance indexes, the realization quartz separates with impure mineral, its effect is remarkable, for removal feldspar, mica group impurity have played keying action.
5, the present invention adopts advanced microwave treatment technology activator metal class foreign ion, improves the activity of foreign ion, and the foreign ion in the lattice is offed normal, and is convenient to remove.Carry out complexing with complexing agent such as oxalic acid, citric acid or organic complexing agent etc. with metal ion then, generate water-soluble complex compound, reach the purpose of removing this class impurity by solid-liquid separation.In addition, present method does not produce any problem of environmental pollution.
1., raw material resources are abundant in sum, the technology of the present invention characteristics are:; 2., the product quality indicator height, the class height; 3., impurity removing technology efficient height, targetedly, be easy to control; 4., non-environmental-pollution problem; 5., process structure is reasonable, can guarantee product quality stability.
Description of drawings
Accompanying drawing 1 is the process flow sheet of embodiment one;
Accompanying drawing 2 is the process flow sheet of embodiment two.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one: a kind of method that adopts vein quartz to prepare ultra-fine high purity quartz material, and the employing vein quartz is a raw material, its technical process is referring to shown in the accompanying drawing 1;
Specify as follows:
1, raw ore: the vein quartz that employing Shangrao, Jiangxi Xi Keng quartz mine provides (lump ore overall dimension≤10cm), SiO
2Content is 99.5～99.8%, and foreign matter content is 0.5～0.2%.
2, fragmentation: adopt jaw crusher and to the rod crusher.The roller of jaw crusher Hubei Province plate and roll crusher high density ceramic processing procedure, crushed product size are the 40-80 order;
3, electrostatic separation: adopt electrostatic separator, 15～25 kilovolts of voltages, concentrate yield 88～93%, product SiO
2〉=99.8%, aluminium, iron contamination content remove to 60ppm with below the 100ppm respectively.
4, superfine grinding: adopt airflow milling and grading machine that quartz mine (40～80 order) is crushed to 800 orders～1250 orders.
5, high-gradient magnetic separation: adopt SHP-500 type high-gradient wet magnetic separator, magneticstrength 1.5-1.9 tesla, the iron level of magnetic separation product removes to 10ppm respectively.
6, microwave treatment: the specified microwave frequency of microwave treatment machine is 2450MHz.
7, complexing is handled and washing: adopt oxalic acid as complexing agent, and addition 30g/L, through deionized water washing after, reduce to 100ppm below again by total impurities for product after complexing is handled.The deionized water consumption is 10: 1 with the ratio of product.
8, oven dry: adopt QG type pneumatic drier to carry out drying, this equipment does not have any pollution, product moisture≤1%.
9, the main quality index analysis of product:
①、SiO
2≥99.98％，Fe3ppm，Al20ppm，Ti1ppm，K5ppm，Na6ppm，Cr6ppm，Mg3ppm。
2., granularity-10 μ m content 〉=90%.
3., water extract specific conductivity: 1 μ sm.
Embodiment two: a kind of method that adopts vein quartz to prepare ultra-fine high purity quartz material, and the employing vein quartz is a raw material, its technical process is referring to shown in the accompanying drawing 2;
Specify as follows:
1, raw ore: adopting Laiwu, Shandong vein quartz is raw material (SiO
299.1-99.5%; Foreign matter content 0.5-0.9%)
2, high-temperature calcination: raw ore is carried out high-temperature calcination, calcining temperature 600-800 ℃, time 1-2 hour.
3, shrend: the piece material after the high-temperature calcination is soaked with cold water.
4, coarse crushing: the raw material mineral are pulverized, associated mineral and quartz are dissociated, granularity is 60～100 orders.
5, electrostatic separation: adopt the electrostatic separation method that the material after pulverizing is carried out the physics removal of impurities, remove material andesine class, mica group impurity.
6, superfine grinding: the material after the static removal of impurities is carried out superfine grinding, and dry method and wet method two procedures are successively adopted in superfine grinding, and dry ground adopts airflow milling, and wet pulverization adopts ultra-fine homogenous medium mill, and grinding particle size is the 1250-2500 order.
7, classification: the material after the superfine grinding is carried out stage treatment.
8, high-gradient magnetic separation: adopt high-gradient magnetic method that material is carried out the physics removal of impurities, remove magnetite, the strong magnetic of ilmenite class and weak magnetic mineral.
9, microwave treatment: adopt microwave that material is handled, activator metal class foreign ion improves the foreign ion activity.
10, complexing is handled: adopt citric acid to carry out complex reaction as complexing agent and material, complexing agent and complexing of metal ion, generate water-soluble complex compound, remove residual impurities such as clay mineral, carbonate, metal oxide then by the solid, liquid separation method.
11, washing: adopt the deionized water wash solid materials, to reduce the electric conductivity of material.
12, oven dry: with the oven dry of QG type pneumatic drier, drying temperature 150-220 ℃, product moisture≤0.5%.
13, the main quality index analysis of product:
①、SiO
2≥99.99％，Fe3ppm，Al10ppm，Ti0.5ppm，K2ppm，Na3ppm，Cr2ppm，Mg4ppm。
2., water extract specific conductivity: 1 μ sm
Claims (5)
1, a kind of method that adopts vein quartz to prepare ultra-fine high purity quartz material is characterized in that: the employing vein quartz is a raw material, follows these steps to be prepared:
(1), the raw material mineral are pulverized, associated mineral and quartz are dissociated, and meet electrostatic separation technology selected material granularity requirement;
(2), employing electrostatic separation method is carried out the physics removal of impurities to the material after pulverizing, removal material andesine class, mica group impurity;
(3), the material after the static removal of impurities is carried out superfine grinding, grinding particle size is 800～2500 orders;
(4), the material after adopting high-gradient magnetic method to superfine grinding carries out the physics removal of impurities, removes magnetite, the strong magnetic of ilmenite class and weak magnetic mineral;
(5), the material after adopting microwave to high-gradient magnetic separation handles, activator metal class foreign ion improves the foreign ion activity;
(6), the material after adopting complexometry to microwave treatment carries out chemical subtraction, wherein, complexing agent and metal ion carry out complex reaction, generate water-soluble complex compound, remove residual impurities such as clay mineral, carbonate, metal oxide then by the solid, liquid separation method;
(7), the solid materials after separating is carried out aftertreatment and get finished product.
2, the method for the ultra-fine high purity quartz material of preparation according to claim 1 is characterized in that: before the above-mentioned the first step pulverization process, earlier the raw material mineral are carried out high-temperature calcination, shrend then.
3, the method for the ultra-fine high purity quartz material of preparation according to claim 1 is characterized in that: dry method and wet method two procedures are successively adopted in above-mentioned the 3rd step superfine grinding, and dry ground adopts airflow milling, and wet pulverization adopts ultra-fine homogenous medium mill.
4, the method for the ultra-fine high purity quartz material of preparation according to claim 1 is characterized in that: after above-mentioned the 3rd step superfine grinding, then material is carried out stage treatment.
5, the method for the ultra-fine high purity quartz material of preparation according to claim 1 is characterized in that: in above-mentioned the 7th step aftertreatment, comprise washing step, this washing step is to adopt the deionized water wash solid materials, to reduce the electric conductivity of material.
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| CN 200410014058 CN1225513C (en) | 2004-02-12 | 2004-02-12 | Method for preparing superfine high-purity quartz material from vein quartz |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN102417184A (en) * | 2011-08-26 | 2012-04-18 | 田辉明 | Method for preparing high-purity ultrafine silicon powder from vein quartz |
| CN102432022A (en) * | 2011-08-26 | 2012-05-02 | 田辉明 | Method for producing ultra-pure quartz sand by vein quartz and high-temperature chlorination device |
| CN102674377A (en) * | 2012-05-04 | 2012-09-19 | 武汉理工大学 | Quartz crystal type conversion metal element gasification integration purification method |
| CN103627215A (en) * | 2013-11-27 | 2014-03-12 | 连云港东海硅微粉有限责任公司 | Preparation method of submicron silica powder |
| CN104549719A (en) * | 2007-01-05 | 2015-04-29 | 氰特技术公司 | Process for the removal of impurities from carbonate minerals |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549719A (en) * | 2007-01-05 | 2015-04-29 | 氰特技术公司 | Process for the removal of impurities from carbonate minerals |
| 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 |
| CN102417184A (en) * | 2011-08-26 | 2012-04-18 | 田辉明 | Method for preparing high-purity ultrafine silicon powder from vein quartz |
| CN102432022A (en) * | 2011-08-26 | 2012-05-02 | 田辉明 | Method for producing ultra-pure quartz sand by vein quartz and high-temperature chlorination device |
| 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 |
| CN102417184B (en) * | 2011-08-26 | 2013-04-03 | 田辉明 | Method for preparing high-purity ultrafine silicon powder from vein quartz |
| CN102674377A (en) * | 2012-05-04 | 2012-09-19 | 武汉理工大学 | Quartz crystal type conversion metal element gasification integration purification method |
| CN103627215A (en) * | 2013-11-27 | 2014-03-12 | 连云港东海硅微粉有限责任公司 | Preparation method of submicron silica powder |
| CN103627215B (en) * | 2013-11-27 | 2016-05-11 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of submicron order silicon powder |
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Assignee: Xiamen ISO Standard Sand Co., Ltd. Assignor: Suzhou Sino-materials Non-Metallic Minerals Industry Design and Research Institu Contract fulfillment period: 2008.12.1 to 2013.12.1 Contract record no.: 2008351000075 Denomination of invention: Method for preparing superfine high-purity quartz material from vein quartz Granted publication date: 20051102 License type: Exclusive license Record date: 20081212 |
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