CN1065212C - High purity SiO2 superfine powder and its producing method - Google Patents
High purity SiO2 superfine powder and its producing method Download PDFInfo
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- CN1065212C CN1065212C CN96114680A CN96114680A CN1065212C CN 1065212 C CN1065212 C CN 1065212C CN 96114680 A CN96114680 A CN 96114680A CN 96114680 A CN96114680 A CN 96114680A CN 1065212 C CN1065212 C CN 1065212C
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Abstract
The present invention relates to high pure superfine silicon oxide powder, and a preparation method thereof. In the superfine powder, the content of SiO2 is 99.9%, the content of Fe2O3 is less than 0.01%, and the particle size reaches more than 10 to 2 mum. The superfine powder is prepared by the following steps: high pure ore of which the content of SiO2 is from 98 to 99.8% is adopted as raw material, and treated with the processes of water wash, primary crush, and ball milling to prepare coarse powder in the size of 100 to 200 meshes more or less; after being treated with the processes of magnetic separation and pickling for iron removal, the coarse powder is water washed, dried, and sent into a jet mill with supersonic airflow for pulverization and refinement by the self-crash of the coarse powder particles. The present invention which solves the problem of secondary pollution to ore powder from the traditional grinding body has the advantages of large yield, low energy consumption, etc.
Description
The present invention relates to a kind of production method of high purity SiO 2 superfine powder, SiO in this super-fine powder
2Content be 99.9%, Fe
2O
3Content be below 0.01%, its median size can reach 2-10 μ m.
The development of nearly more than ten years China's national industry has made China form the more complete industrial sector structure of class.But aspect basic industry, particularly the production technology of Mineral resources product and technology rest on the primary products process segment always.This has not only caused the loss of the low value of Chinese Mineral resources, has also caused the unfavorable situation that hinders the Chinese industrial comprehensive development.
As everyone knows, high purity, low iron, ultra-fine powdered ground silica are the indispensable base mateirals of producing semiconductor material, unicircuit, photoconductive fiber, glass fibre, the physicochemical property that it is stable can guarantee and strengthen the job stability and the life-span of finished product.The existing silica mine of nature is an example with the HIGH-PURITY SILICON ore, general SiO
2Content between 98-99.9%, Fe
2O
3Content be between the 0.1-0.02%.SiO in China's non-metallic minerals
2The reserves of ore are quite abundant, and its quality is high, SiO in the raw ore
2Purity generally can reach 98-99.8%, but in raw ore dry method or wet method tradition crushing processing process, need to adopt the broken and processing SiO of grinding element
2Ore makes it to become the breeze of different fineness.Because silicon-dioxide ore hardness is bigger, in using alligator and ball mill or twin rollers fining-off process, the wearing and tearing of its grinding element can cause certain pollution to ore, make Fe in the ore powder
2O
3Raise with detrimental impurity content such as free iron, thereby influenced the quality of silicon-dioxide breeze.In addition, utilize above-mentioned conventional process tools, SiO
2The breeze granularity is difficult to be worked into more than the 2 μ m, and the grinding element wearing and tearing are quite serious, needs often maintenance and replacing.About the prior art situation has detailed introduction in " special processing of nonmetalliferous ore and utilization " book 75-83 page or leaf that Science Press publishes in February, 1992.
In order to reduce the course of processing to SiO
2The secondary pollution that breeze causes has been adopted inwall cotton up to or additional plastic cement backplate mode to processing units such as alligator or ball mill in the prior art.Adopt abovementioned technology to alleviating the grinding element wearing and tearing, the secondary pollution that the reduction course of processing causes truly has certain effect, but the also corresponding raising of processing units cost, its processing mode does not finally break away from the constraint and the restriction of prior art yet, its unit time processing amount is relatively low, and its SiO
2Granularity and quality also difficulty reach desirable requirement.
The purpose of this invention is to provide a kind of high purity SiO 2 superfine powder production method, this method utilizes supersonic airstream to make carrier, dry meal about the 100-200 order that the preliminary working of feasible process is made, self collides mutually in micronizer mill, reaches fining-off and reduces grinding element secondary pollution purpose.
Above-mentioned purpose of the present invention is accomplished by the following technical programs.
A kind of method of producing high purity SiO 2 superfine powder, this method is selected SiO for use
2Content is 98-99.8%, Fe
2O
3Content is that the high purity ore of 0.1-0.02% is a raw material, through washing, just ore grinding broken and that the ball milling complete processing will just be broken becomes 100-200 order left and right sides meal, removes iron contamination in the meal with magnetic separation and acid cleaning process, makes Fe
2O
3Content is reduced to below 0.01%, SiO
2Content be 99.9%, after washing and oven dry, form dry meal again, the method is characterized in that above-mentioned dry meal is sent in the micronizer mill under the supersonic speed swirling eddy drives, utilize high velocity air that the meal particle self is collided mutually, make meal granularity median size reach 2-10 μ m.Above-mentioned supersonic airstream speed is the swirling eddy that exceeds the speed limit more than 1.5 Mach, and its transfer pressure is 0.6-1.2MPa.And this supersonic airstream makes aeroscope reach medical grade in advance preferably through overcooling, oil removing and dehumidifying pre-treatment, prevents that air from polluting the SiO2 super-fine powder.In order to ensure super-fine powder Fe
2O
3Content is reduced to below 0.01%, above-mentioned super-fine powder can packed after overpickling, alkali cleaning, washing and oven dry.The detailed processing process of the present invention is referring to shown in Figure 1.
SiO provided by the present invention
2The production technique of super-fine powder has following characteristics:
1, the low impurity of high purity (low iron): adopt this technology, not only the impurity that produces in the process of manufacture is removed but also can be with further purification, particularly objectionable constituent Fe of former stone itself
2O
3Reduce greatly.For example former stone SiO
2-99.5%, Fe
2O
3-0.05%, finished product can reach SiO
2-99.9%, Fe
2O
3Below 0.01%, and the present state-of-the-art working method of world's technology, SiO
2Finished product content be 99.8%.
2, ultrafine powder: the fineness of this technology can reach more than the 2 μ m (median size).
3, output height: output can reach more than the 200kg/h, and conventional machining process can only reach 50-75kg/h.
4, pollution-free: as owing to adopt advanced equipment (sealing), to have eliminated the dust pollution that is produced in the general processing, and added and alkalinely neutralize and eliminated sour pollution through recycling with the pollution of acid in the acid cleaning process.
5, in the slave unit preparation: technical process of the present invention has run through all processes from the preliminary working to the retrofit, is a kind of complete high-purity, low iron, the mode of production of ultra micro ground silica.Simultaneously, because the micronizer mill that the present invention adopts on key equipment is to be based upon the mutual bump of material self to reach the purpose of pulverizing, single machine yield can reach every month 150 tons, is a kind of relative low consumption, low cost, high efficiency disintegrating apparatus.
6, on the method for deironing: the present invention adopts physics and the chemistry and the mode of usefulness, and implements twice acid cleaning process flow process respectively during with finished product to guarantee 0.01% low iron standard about 200 orders.
Introduce concrete machining process of the present invention and specific embodiment in detail below in conjunction with accompanying drawing.
Fig. 1 is SiO 2 superfine powder processing process figure of the present invention.
In the present embodiment: 1. buying ore and selected: choose and finished ore is SiO
2Content is the high-purity silica more than 99.8%.
2. washing: by water-washing method, remove the impurity of mineral surface, be same as the cleaning process of an ore.
3. just broken: as use alligator, and the mode by " cotton up to " to reduce grinding element to the pollution of ore and reach the desired standard of next technical process.
4. mechanical milling process: use ball mill, purpose be will be just broken ore grinding to 100-200 purpose powdery standard.In order to reduce the pollution of metal oxide, in ball mill, will carry out specific modifications to the ore in sand form meal:
(1) inwall is done special processing, promptly at the inwall cotton up to or add attached plastic cement backplate;
(2) meson adopts the grinding element of chromium, nickel or chromium, molybdenum alloy.
This remodeling is to carry out for the quality standard that guarantees product, is once to special adaptations and innovation that conventional ball mill carried out, makes it more to be adapted to the development in breeze market.
5. magnetic force machine deironing: ore is by behind first broken, the ball milling, because the effect of ore hardness makes formed ore in sand form many remelted pig irons that exist with unbound state occur, so sorting step by step by the high-intensity magnetic separator made with neodymium iron boron, the remelted pig iron impurity that exists with unbound state in the ore in sand form can be accomplished effectively with ganister sand and be separated, be a kind of iron removal technology of physics mode.
6. pickling: the Fe in the ore in sand form
2O
3Be a kind of impurity that is an impediment to quality product that exists with the compound state, must adopt this chemical means of pickling to be carried and remove, remove Fe in the ore in sand form
2O
3Deng impurity, product itself is further purified.
7. washing: the ore in sand form of the mode that washes with water after to pickling implemented cleaning.
8. oven dry: the ore in sand form oven dry is reduced into dry powder, free iron from the technical process of 1-8 in the ore in sand form and Fe
2O
3Content reach below 0.01%.
9. pulverizer: use micronizer mill, gas by cooling, oil removing and dehumidifying is under transfer pressure 0.9MPa effect, make gas form 1.5 Mach of supersonic speed swirling eddies, under the effect of this air-flow, make ore in sand form in pulverizer, carry out self colliding mutually, to reach the ultrafine powder state that is ground into to the thinnest 2 μ m with high speed.Characteristics such as this equipment is in operation owing to fundamentally having solved the pollution problem of grinding element to breeze, and it is big to have output, and it is little to consume energy, this equipment yield can reach more than the 200kg/h, super-fine powder SiO
2Content is 99.9%.
10.-13. step: this multiple pickling, alkali cleaning, washing, drying course are to make as guaranteeing on the basis of quality product.
Claims (4)
1. method of producing high purity SiO 2 superfine powder, this method is selected SiO for use
2Content is 98-99.8%, Fe
2O
3Content is that the high purity ore of 0.1-0.02% is a raw material, through washing, just ore grinding broken and that the ball milling complete processing will just be broken becomes 100-200 purpose meal, removes iron contamination in the meal with magnetic separation and acid cleaning process, makes Fe
2O
3Content is reduced to below 0.01%, SiO
2Content be 99.9%, after washing and oven dry, form dry meal again, the method is characterized in that above-mentioned dry meal is sent in the micronizer mill under supersonic airstream drives, utilize swirling eddy that the meal particle self is collided mutually, make meal granularity median size reach 2-10 μ m.
2. super-fine powder production method according to claim 1 is characterized in that the super-fine powder that the process comminution by gas stream is machined to, and packs after overpickling, alkali cleaning, washing and oven dry.
3. super-fine powder production method according to claim 1 is characterized in that said supersonic airstream speed is more than 1.5 Mach, and its transfer pressure is 0.6-1.2MPa.
4. according to claim 1 or 3 described super-fine powder production methods, the supersonic airstream that it is characterized in that adopting is in advance through overcooling, oil removing and dehumidifying pre-treatment, and this aeroscope is the medical grade air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96114680A CN1065212C (en) | 1996-12-30 | 1996-12-30 | High purity SiO2 superfine powder and its producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96114680A CN1065212C (en) | 1996-12-30 | 1996-12-30 | High purity SiO2 superfine powder and its producing method |
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| Publication Number | Publication Date |
|---|---|
| CN1186772A CN1186772A (en) | 1998-07-08 |
| CN1065212C true CN1065212C (en) | 2001-05-02 |
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ID=5122248
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96114680A Expired - Fee Related CN1065212C (en) | 1996-12-30 | 1996-12-30 | High purity SiO2 superfine powder and its producing method |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305764C (en) * | 2004-03-31 | 2007-03-21 | 张永 | Hyperpure, superfine silicon powder and preparation method |
| CN101219791B (en) * | 2008-01-29 | 2010-11-03 | 山东华昊硅业科技有限公司 | Method for producing high purity ultra-fine silicon dioxide |
| CN102235950A (en) * | 2010-04-27 | 2011-11-09 | 深圳市比克电池有限公司 | Method for detecting magnetic substances in powder material of lithium ion battery |
| CN102815713B (en) * | 2012-08-06 | 2014-08-27 | 东海县晶盛源硅微粉有限公司 | Method for preparing silicon dioxide powder |
| CN103130405B (en) * | 2013-03-15 | 2015-04-22 | 连云港利思特电子材料有限公司 | Preparation method of precision casting fused quartz powder and quartz powder produced by same |
| WO2015016359A1 (en) | 2013-08-01 | 2015-02-05 | 日揮触媒化成株式会社 | Method for producing crushed silica particles, and resin composition containing said particles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104402A (en) * | 1985-06-27 | 1987-01-28 | 日东化学工业株式会社 | The preparation method of high-purity silicon dioxide |
| CN1063087A (en) * | 1992-01-25 | 1992-07-29 | 交通部公路科学研究所 | The method of extraction of highly pure silica in the rice husk |
| CN1070891A (en) * | 1991-10-02 | 1993-04-14 | 尤尼利弗公司 | Silicon-dioxide |
-
1996
- 1996-12-30 CN CN96114680A patent/CN1065212C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104402A (en) * | 1985-06-27 | 1987-01-28 | 日东化学工业株式会社 | The preparation method of high-purity silicon dioxide |
| CN1070891A (en) * | 1991-10-02 | 1993-04-14 | 尤尼利弗公司 | Silicon-dioxide |
| CN1063087A (en) * | 1992-01-25 | 1992-07-29 | 交通部公路科学研究所 | The method of extraction of highly pure silica in the rice husk |
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| Publication number | Publication date |
|---|---|
| CN1186772A (en) | 1998-07-08 |
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