CN1301902C - Method for producing high-purity Silicon dioxide - Google Patents
Method for producing high-purity Silicon dioxide Download PDFInfo
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- CN1301902C CN1301902C CNB2004100225938A CN200410022593A CN1301902C CN 1301902 C CN1301902 C CN 1301902C CN B2004100225938 A CNB2004100225938 A CN B2004100225938A CN 200410022593 A CN200410022593 A CN 200410022593A CN 1301902 C CN1301902 C CN 1301902C
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Abstract
The present invention discloses a method for producing high-purity silicon dioxide. In the method, industrial sodium fluorosilicate is used as a raw material and is dissolved in deionized water for being prepared into a saturated dissolvable solution; after the saturated solution is purified through recrystallization, the solution is dissolved in the deionized water and boiled; an ionic membrane caustic soda solution is added to the solution in drops, and the solution is stirred uniformly and filtered through vacuum pumping; a filter cake is blended uniformly with the ionized water, and sulfuric acid with the concentration of 25% to 35% is added to the ionized water which is stirred uniformly and filtered through vacuum pumping; the filter cake is washed by the deionized water at a temperature of 90 DEG C to 95 DEG C for 2 to 4 times, and dried, burnt, cooled and ground for several times to be a finished product of the high-purity silicon dioxide. The present invention has the advantages of cheap and easily obtained raw material, simple process, mild reaction conditions, low cost and good economic effect.
Description
Technical field
The present invention relates to silicon-dioxide, more particularly, the present invention relates to the production method of high-purity silicon dioxide.
Background technology
As everyone knows, high-purity silicon dioxide has stable and unique physical and chemical performance, its goods stable working state and life-span height, thereby be the indispensable base mateirals of high-tech sector such as semi-conductor industry, unicircuit, photoconductive fiber and function ceramics.
Up to now, the preparation high-purity silicon dioxide is divided into natural method and synthesis method two big classes.The natural genealogy of law adopts the HIGH-PURITY SILICON ore to make raw material, because the mineral crystal resource is few, purity is unstable, and ore hardness is big, the wearing and tearing meeting of grinding element pollutes breeze in process of lapping, cause in the breeze detrimental impurity such as iron to raise, have a strong impact on the quality of breeze.Synthesis method is divided into two kinds of dry method and wet methods again, and dry method is that the halogenide with silicon is raw material, by the vapor phase process manufacturing, though the quality product height, expensive raw material price, the equipment requirements height, investment and product cost are all higher.Wet method is to be raw material with the water glass, prepare with the precipitator method, but it relates to the issues of purification of raw material, especially used silicofluoric acid belongs to liquid strong acid, produce from Rock Phosphate (72Min BPL), and impurity is extremely many, it is following extremely difficult metal ion wherein will to be removed to 1PPm, but remove certain ionic often and simultaneously bring a kind of new ion into, purification procedures is increased, impurity but finally separates not thorough.Therefore, how to improve the purity of silicon-dioxide effectively, this is a long-term unsolved technical barrier.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide a kind of cost of material low, technical process is reasonable, and is easy and simple to handle, the production method of colory high-purity silicon dioxide.
Purpose of the present invention is achieved by following technical proposals.
Except as otherwise noted, the percentage ratio that is adopted among the present invention is weight percentage.
The invention provides a kind of production method of high-purity silicon dioxide, this method adopts the step of following order:
(1) is raw material with industrial Sodium Silicofluoride, dissolves, make saturated lysate, under-6 ℃～-3 ℃, through 3～5 recrystallization purifyings with deionized water;
(2) deionized water dissolving of 45～55 times of weight of adding boils, and slowly dripping concentration is 25%～35% sodium hydroxide solution, and sodium hydroxide and Sodium Silicofluoride weight ratio are 1: 1.1～1.3, stirs 8～12 minutes down at 90 ℃～95 ℃, then vacuum filtration;
(3) filter cake is with the deionized water mixing of 38～42 times of weight, add the deionized water volume 8%～10%, concentration is 25%～35% sulfuric acid, stirs vacuum filtration;
(4) operation of repeating step (3);
(5) filter cake is with 90 ℃～95 ℃ deionized water wash 2～4 times, 100 ℃～110 ℃ dry 20～30 minutes down, move in the electric furnace, 940 ℃～960 ℃ following calcinations 40～45 minutes, be cooled to room temperature;
(6) with the gains of step (5) with 90 ℃～95 ℃ deionized water wash 2～3 times, 100 ℃～110 ℃ following heat dryings 20～30 minutes, move in the electric furnace, 940 ℃～960 ℃ following calcinations 30～40 minutes; Be chilled to room temperature,, be required high-purity silicon dioxide finished product through grinding.
Wherein, described deionization electrical conductivity of water is 1.0～0.1 μ S/cm.
Sodium hydroxide solution described in the above-mentioned steps (2) is an ion film caustic soda solution.
Sulfuric acid described in the above-mentioned steps (3) is chemically pure reagent.
The present invention comprises that further be that 0.149 millimeter industry is screened with the material through grinding in the above-mentioned steps (6) by diameter of bore.
Also have Sodium Fluoride to generate in the production process of the present invention, the solution that concentration is high obtains the byproduct Sodium Fluoride through evaporating, concentrating and crystallizing, and the solution that concentration is low adds in the milk of lime and the back qualified discharge.
Product of the present invention adopts the ICP method to measure through Yunnan Agriculatural Academy plant protection clay fertilizer test analysis center, and the content of silicon-dioxide is up to 99.992%, and measurement result sees Table 1.
Table 1
| Composition | Content (%) | Composition | Content (%) |
| Silicon-dioxide (SiO 2) | 99.992 | Iron (Fe) | 0.0005 |
| Potassium (K) | Do not detect | Aluminium (Al) | 0.0001 |
| Sodium (Na) | Do not detect | Copper (Cu) | 0.00005 |
| Calcium (Ca) | 0.001 | Nickel (Ni) | 0.0001 |
| Magnesium (Mg) | 0.0001 |
Compared with prior art, the present invention has following outstanding advantage:
1. the wet processing of existing preparation high-purity silicon dioxide, generally all be with the reaction of putting together of several industrial goods raw materials, in reactive system, remove impurity then again, because of there being different kinds of ions in the system simultaneously, the removal of impurities process is loaded down with trivial details, and is difficult for thoroughly removing because of multiple effect causes impurity.The present invention concentrates on attention on the raw material from a new thinking.Promptly before chemical reaction, earlier Sodium Silicofluoride is carried out recrystallization 3～5 times with deionized water, it is highly purified; And adopt ion film caustic soda solution also to guarantee the purity of sodium hydroxide; Thereby make the silicon-dioxide of generation have high purity, this is a distinctive feature of the present invention.
2. the present invention is a raw material with Sodium Silicofluoride and sodium hydroxide first, and has determined concentration sodium hydroxide and addition by Optimized by Orthogonal Test, is higher than this point, and the silicon-dioxide of separating out forms reverse dissolution, is lower than this silicon-dioxide and separates out imperfect.
3. the present invention has added sulfuric acid and has made finishing agent, and the effect of finishing agent is to prevent that effectively other metal ion in the raw material from separating out with silicon-dioxide, has further improved the purity of product.
4. processing condition gentleness of the present invention is easy to control, and whole technology is all carried out under normal pressure except vacuum filtration, and last calcination temperature also only needs 940 ℃～960 ℃, and technology is simple, and is easy to operate.
5. the present invention adopts economically viable operational path, goes out high-quality product with cheap raw material production, is that product profit after tax per ton has the excellent development application prospect more than 40,000 yuan under 80,000 yuan/ton the situation in sale price.
Embodiment
By specific embodiment given below, can further be well understood to the present invention.But they are not limitation of the invention.
Embodiment 1
With industrial Sodium Silicofluoride is raw material, dissolves with deionized water, makes saturated lysate, under one-5 ℃, through 4 recrystallization purifyings.Add the deionized water dissolving of 50 times of weight, boil, slowly drip concentration and be 30% sodium hydroxide solution, sodium hydroxide and Sodium Silicofluoride weight ratio are 1: 1.1～1.3, at 90 ℃ of stirrings 12 minutes down, vacuum filtrations then.Filter cake adds 10% of deionized water volume with the deionized water mixing of 40 times of weight, and concentration is 30% sulfuric acid, stirs vacuum filtration; Filter cake is used the deionized water mixing of 40 times of weight again, adds 100 ml concns and be 30% sulfuric acid, stirs vacuum filtration.Filter cake is with 95 ℃ of deionized water wash 3 times, 105 ℃ dry 25 minutes down, move in the electric furnace, 940 ℃ of following calcinations 45 minutes, be cooled to room temperature.With 90 ℃ of deionized water wash 3 times,, move in the electric furnace, 950 ℃ of following calcinations 30 minutes 105 ℃ of following heat dryings 25 minutes; Be chilled to room temperature,, promptly obtain purity and be 99.992% silica product through grinding.
Embodiment 2～9
Repeat the process of embodiment 1, the variation of test conditions and the results are shown in Table 2.
Table 2
| Numbering | The recrystallization number of times | The weight ratio of sodium hydroxide and Sodium Silicofluoride | Add vitriolic concentration (%) | The calcination number of times | The filter cake washing total degree | Silica product purity (%) | Potassium, sodium, calcium, magnesium, iron, aluminium, copper, 7 kinds of content of impurities of nickel (%) |
| 2 | 2 | 1∶1.1 | 20 | 1 | 8 | 99.511 | 0.01721 |
| 3 | 2 | 1∶1.1 | 20 | 1 | 8 | 99.616 | 0.01464 |
| 4 | 3 | 1∶1.15 | 25 | 1 | 8 | 99.846 | 0.00764 |
| 5 | 3 | 1∶1.15 | 25 | 1 | 8 | 99.823 | 0.00616 |
| 6 | 4 | 1∶1.2 | 30 | 2 | 10 | 99.964 | 0.00242 |
| 7 | 4 | 1∶1.2 | 30 | 2 | 10 | 99.979 | 0.00203 |
| 8 | 5 | 1∶1.3 | 35 | 2 | 14 | 99.992 | 0.00185 |
| 9 | 5 | 1∶1.3 | 35 | 2 | 14 | 99.992 | 0.00185 |
Claims (5)
1. the production method of a high-purity silicon dioxide, this method comprises the step of following order:
(2) be raw material with industrial Sodium Silicofluoride, dissolve, make saturated lysate, under-6 ℃～-3 ℃, through 3～5 recrystallization purifyings with deionized water;
(2) deionized water dissolving of 45～55 times of weight of adding boils, and slowly dripping concentration is 25%～35% sodium hydroxide solution, and sodium hydroxide and Sodium Silicofluoride weight ratio are 1: 1.1～1.3, stirs 8～12 minutes down at 90 ℃～95 ℃, then vacuum filtration;
(3) filter cake is with the deionized water mixing of 38～42 times of weight, add the deionized water volume 8%～10%, concentration is 25%～35% sulfuric acid, stirs vacuum filtration;
(4) operation of repeating step (3);
(5) filter cake is with 90 ℃～95 ℃ deionized water wash 2～4 times, 100 ℃～110 ℃ dry 20～30 minutes down, move in the electric furnace, 940 ℃～960 ℃ following calcinations 40～45 minutes, be cooled to room temperature;
(6) with the gains of step (5) with 90 ℃～95 ℃ deionized water wash 2～3 times, 100 ℃～110 ℃ following heat dryings 20～30 minutes, move in the electric furnace, 940 ℃～960 ℃ following calcinations 30～40 minutes; Be chilled to room temperature,, be required high-purity silicon dioxide finished product through grinding.
2. the production method of high-purity silicon dioxide according to claim 1, wherein, described deionization electrical conductivity of water is 1.0～0.1 μ S/cm.
3. the production method of high-purity silicon dioxide according to claim 1 is an ion film caustic soda solution at the sodium hydroxide solution described in the step (2) wherein.
4. the production method of high-purity silicon dioxide according to claim 1 is a chemically pure reagent at the sulfuric acid described in the step (3) wherein.
5. the production method of high-purity silicon dioxide according to claim 1 comprises that further be that 0.149 millimeter industry is screened with the material through grinding in the above-mentioned steps (6) by diameter of bore.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100225938A CN1301902C (en) | 2004-05-21 | 2004-05-21 | Method for producing high-purity Silicon dioxide |
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| CNB2004100225938A CN1301902C (en) | 2004-05-21 | 2004-05-21 | Method for producing high-purity Silicon dioxide |
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| CN1579936A CN1579936A (en) | 2005-02-16 |
| CN1301902C true CN1301902C (en) | 2007-02-28 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080202387A1 (en) * | 2005-06-08 | 2008-08-28 | Yuanjian Lu | Process For Producing Silica and Sodium Sulfite With Sodium Sulfate |
| CN102249249A (en) * | 2011-06-22 | 2011-11-23 | 武汉大学 | Method for purifying quartz sand by molten salt method |
| CN103695875A (en) * | 2013-12-06 | 2014-04-02 | 湖洲三峰能源科技有限公司 | Chemical composition for accelerating growth of silicon oxide on surface of substrate |
| CN110562988B (en) * | 2019-09-12 | 2023-10-31 | 青岛美高集团有限公司 | Heat insulation material and production method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4213952A (en) * | 1978-10-23 | 1980-07-22 | Occidental Research Corporation | Recovery of hydrofluoric acid from fluosilicic acid with high pH hydrolysis |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4213952A (en) * | 1978-10-23 | 1980-07-22 | Occidental Research Corporation | Recovery of hydrofluoric acid from fluosilicic acid with high pH hydrolysis |
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