CN102757052B - Method for separating and extracting silica micro powders from discarded quartz tailings - Google Patents
Method for separating and extracting silica micro powders from discarded quartz tailings Download PDFInfo
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- CN102757052B CN102757052B CN201210269135.9A CN201210269135A CN102757052B CN 102757052 B CN102757052 B CN 102757052B CN 201210269135 A CN201210269135 A CN 201210269135A CN 102757052 B CN102757052 B CN 102757052B
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- flotation
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Abstract
The invention discloses a method for separating and extracting silica micro powders from discarded quartz tailings. The method includes a surface processing, an ionic modification, a flotation separation and a post-processing, wherein the surface processing includes washing the quartz tailings, placing the washed quartz tailings in a ball grinding mill to subject the quartz tailings to a wet ball milling and washing the milled quartz tailings to obtain tailings which are subjected to the surface processing, the ionic modification includes adding the tailings which are subjected to the surface processing in a mixed solution to soak at the room temperature for 3 to 7 minutes to obtain tailings which are subjected to the ionic modification, and the flotation separation includes adding the tailings which are subjected to the ionic modification in a flotation solution to perform a flotation for 10 to 30 minutes and washing and drying the tailings after the flotation to obtain the silica micro powders. The method has the advantages that the method is suitable for discarded quartz tailings with any degree of fineness (in a range from several microns to 80 microns), numerous impurities can be effectively separated and removed once, and the quantity of removed impurities (generally 10% of the total quantity) far exceeds the quantity of removed impurities (generally 1% of the total quantity) from the existing coarse particle quartz flotation.
Description
One, technical field
The present invention relates to a kind of recycling method of quartz mine tailings, specifically a kind of from discarded quartz tail sand the method for separation and Extraction silicon powder, belong to comprehensive utilization of resources and field of environment protection.
Two, background technology
Quartz sand/powder (claiming again silicon powder) is important industrial raw material, is widely used in the fields such as opticfiber communication, silicon semiconductor, optics and building glass, electron and electrician, chemical industry and various weighting agents.
Preparing silicon powder is first by operations such as quartz mine exploitation, ore dressing, Mechanical Crushing and the separation of sand mud, is wherein separated and the tailings that abandons accounts for greatly the 15%-25% of quartz mine gross recovery.Incomplete statistics, the whole nation will produce the quartz tail sand of up to ten million tons every year.Although to be wherein used in cement or brickmaking etc. industrial for part, substantially do not change that it is abandoned in a large number, the destiny of contaminate environment and general layout.The healthy pollution of its discharge to atmosphere, river, soil and the people and harm are repeatedly by the media of central authorities and various places are exposed.Tailings is consisted of impurity compositions such as the clays, mica, feldspar, rhombohedral iron ore, magnetite, hornblende of a large amount of quartzy fine powders and part, granularity very thin (generally distributing to 80 micro-meter scales are interval from submicron), and general method for floating requires quartz particles granularity to be greater than 100 microns, be therefore difficult to separation and acquisition from tailings and go out high-quality silicon powder.Also have no report both at home and abroad.Therefore, finding a kind of new technology that goes out to have highly purified silicon powder by separation and acquisition in discarded quartz tail sand is a difficult problem urgently to be resolved hurrily.
Three, summary of the invention
The present invention aim to provide a kind of from discarded quartz tail sand the method for separation and Extraction silicon powder, technical problem to be solved is that separation and Extraction goes out highly purified silicon powder from the tailings of quartz mine.
The present invention is take the quartz tail sand discarded as raw material, mainly by surface treatment-ion modification-flotation process separation and acquisition go out to have high purity, diameter is the several microns of silicon powders to tens of micro-meter scales.
The method of the present invention's separation and Extraction silicon powder from discarded quartz tail sand, comprises the each unit process of surface treatment, ion modification, flotation separation and aftertreatment:
Described surface treatment is that quartz tail sand is cleaned and removes the domestic refuse thing of sneaking into and thick rock ballast etc., is then placed in ball mill, adds alkali lye wet ball mill, obtains surface-treated tailings after washing;
Described ion modification is that surface-treated tailings is added to CaO, CaCl
2, CaSO
4and Na
2siO
3mixing solutions in soaking at room temperature 3-7 minute obtain the tailings of ion modification, CaO, CaCl in mixing solutions
2, CaSO
4and Na
2siO
3mass ratio 1:1:1:1, in mixing solutions, the total concn of solute is 0.01-0.1kg/ton;
Described flotation separation is that the tailings of ion modification is added to flotation 10-30min in flotation fluid, the pH value of system is 6-8, in described flotation fluid, each component and concentration are sodium laurylsulfonate 0.1-0.5kg/ton, potassium oleate 0.05-0.5kg/ton, sodium lauryl sulphate 0.1-0.5kg/ton, oleic acid 0.01-0.05kg/ton, Na
2cO
30.01-0.05kg/ton, Na
2siO
30.05-0.5kg/ton; After flotation finishes, remove the impurity floating, by the tailings washing after flotation and in 90-110 ℃, obtain silicon powder, SiO after dry
2content>=99.7%, Fe
2o
3content≤0.01%, diameter is several microns to tens of microns.
Described alkali lye is the mixing solutions of sodium hydroxide and calcium hydroxide, and in mixing solutions, the total mass concentration of solute is 3 × 10
-3%, the mass ratio of sodium hydroxide and calcium hydroxide is 1.5-2.5:1.
The mass ratio of described surface-treated tailings and mixing solutions is 0.3-0.5:1.
The tailings of described ion modification and the mass ratio of flotation fluid are 1:2-3.
The technology of the present invention turns waste into wealth, and preparation technology is simple, and less demanding, with low cost to equipment administered quartz tail sand/tail sludge-polluted, protection of the environment, made mineral products increment; Energy-saving and cost-reducing, promotion structural transformation of the economy.
Compared with the prior art, beneficial effect of the present invention is embodied in:
The quartz tail sand (several microns to 80 micrometer ranges) of any fineness that 1, the inventive method is applicable to discard, and existing coarse particles quartz purification by floatation general requirement particle is greater than 100 microns to several millimeters of scopes;
2, the present invention adopts unique ion modification technology, can effectively disposable the impurity of One's name is legion be separated and be removed, the impurity level (general >10% total amount) of removing far exceedes the impurity level (general <1% total amount) that the flotation of existing coarse particles quartz is removed;
3, the present invention does not introduce acid pollution (carrying out in pH value is the neutral environment of 7 left and right without pickling and flotation) when polluting turning waste into wealth, administer, and existing coarse particles quartz purification by floatation generally carries out pH value 2-5(only a few and in alkaline environment, carries out pH value 8.5-10 in the environment that contains HF acid or sulfuric acid).
4, the quartzy resource of the alternative top grade of high purity silica powder (purity >=99.7%) that the inventive method makes, is applied to novel material, the high-tech sectors such as silicon semiconductor, optics and building glass, electron and electrician, chemical industry and even nano material.
Four, accompanying drawing explanation
Fig. 1 is the photo of the discarded quartz tail sand raw material that uses of the present invention.
Fig. 2 is the photo of the silicon powder prepared of the present invention.
Fig. 3 and Fig. 4 are the examining report of the silicon powder quality prepared of the present invention.
Fig. 5 is the sreen analysis of silicon powder of the present invention.
Five, embodiment
Embodiment 1:
1, surface treatment
Take 100 grams of quartz tail sands and be placed in beaker, wash with water 3 times, then quartz tail sand and 20mL alkali lye after washing are added to ball grinder wet ball mill 10min, the tailings that ball milling is crossed taking-up is washed with water to washings clarification and obtains surface-treated tailings.Alkali lye is the mixing solutions of sodium hydroxide and calcium hydroxide, and in mixing solutions, the total mass concentration of sodium hydroxide and calcium hydroxide is 3 × 10
-3%, the mass ratio of sodium hydroxide and calcium hydroxide is 2:1; Aluminum oxide abrading-ball and tailings mass ratio are 1.5: 1.
2, ion modification
In surface-treated tailings, add CaO, CaCl
2, CaSO
4and Na
2siO
3mixing solutions 50mL, the tailings that soaking at room temperature goes supernatant liquid to obtain ion modification in 5 minutes, CaO, CaCl in mixing solutions
2, CaSO
4and Na
2siO
3mass ratio 1:1:1:1, CaO, CaCl in mixing solutions
2, CaSO
4and Na
2siO
3total concn be 0.05kg/ton.
3, flotation separation
The tailings of ion modification is added to flotation 15min in 180mL flotation fluid, and in described flotation fluid, each component and concentration are sodium laurylsulfonate 0.3kg/ton, potassium oleate 0.2kg/ton, sodium lauryl sulphate 0.2kg/ton, oleic acid 0.05kg/ton, Na
2cO
30.05kg/ton, Na
2siO
30.05kg/ton; After flotation finishes, remove the impurity floating, by the tailings washing after flotation and in 100 ℃ dry 2 hours, obtain 82g silicon powder.Its SiO
2content is 98.58%, Fe
2o
3content is 0.037%.
Embodiment 2:
The preparation method of the present embodiment is with embodiment 1, and different is that in step 3, flotation time is 20min.
The silicon powder 79g preparing, its SiO
2content is 98.98%, Fe
2o
3content is 0.030%.
Embodiment 3:
The preparation method of the present embodiment is with embodiment 1, and different is that in step 3, flotation time is 30min.
The silicon powder 77.7g preparing, its SiO
2content is 99.73%, Fe
2o
3content is 0.010%.
Claims (4)
1. a method for separation and Extraction silicon powder from discarded quartz tail sand, comprises the each unit process of surface treatment, ion modification, flotation separation and aftertreatment, it is characterized in that:
Described surface treatment is that quartz tail sand is cleaned and is placed in ball mill, adds alkali lye wet ball mill, obtains surface-treated tailings after washing;
Described ion modification is that surface-treated tailings is added to CaO, CaCl
2, CaSO
4and Na
2siO
3mixing solutions in soaking at room temperature 3-7 minute obtain the tailings of ion modification, CaO, CaCl in mixing solutions
2, CaSO
4and Na
2siO
3mass ratio 1:1:1:1, in mixing solutions, the total concn of solute is 0.01-0.1kg/ton;
Described flotation separation is that the tailings of ion modification is added to flotation 10-30min in flotation fluid, in described flotation fluid, each component and concentration are sodium laurylsulfonate 0.1-0.5kg/ton, potassium oleate 0.05-0.5kg/ton, sodium lauryl sulphate 0.1-0.5kg/ton, oleic acid 0.01-0.05kg/ton, Na
2cO
30.01-0.05kg/ton, Na
2siO
30.05-0.5kg/ton; After flotation finishes, remove the impurity floating, after the tailings after flotation is washed and is dried, obtain silicon powder.
2. extracting method according to claim 1, is characterized in that:
Described alkali lye is the mixing solutions of sodium hydroxide and calcium hydroxide, and in mixing solutions, the total mass concentration of solute is 3 × 10
-3%, the mass ratio of sodium hydroxide and calcium hydroxide is 1.5-2.5:1.
3. extracting method according to claim 1, is characterized in that:
The mass ratio of described surface-treated tailings and mixing solutions is 0.3-0.5:1.
4. extracting method according to claim 1, is characterized in that:
The tailings of described ion modification and the mass ratio of flotation fluid are 1:2-3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210269135.9A CN102757052B (en) | 2012-07-31 | 2012-07-31 | Method for separating and extracting silica micro powders from discarded quartz tailings |
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|---|---|---|---|
| CN201210269135.9A CN102757052B (en) | 2012-07-31 | 2012-07-31 | Method for separating and extracting silica micro powders from discarded quartz tailings |
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| CN102757052A CN102757052A (en) | 2012-10-31 |
| CN102757052B true CN102757052B (en) | 2014-04-30 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098783A (en) * | 2017-05-27 | 2017-08-29 | 镇江环太硅科技有限公司 | The technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting |
| CN110775979B (en) * | 2019-12-05 | 2020-09-25 | 中国科学院合肥物质科学研究院 | Method for recovering high-purity silicon and silicon carbide from crystalline silicon cutting waste |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958446A (en) * | 2006-11-17 | 2007-05-09 | 四川大学 | Method for preparing high purity super fine silicon miropowder by using powder of natural quartz |
| CN101033068A (en) * | 2007-02-13 | 2007-09-12 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN101817533A (en) * | 2010-04-27 | 2010-09-01 | 中国地质大学（武汉） | Preparation method of electronic-level crystalline silicon powder |
-
2012
- 2012-07-31 CN CN201210269135.9A patent/CN102757052B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958446A (en) * | 2006-11-17 | 2007-05-09 | 四川大学 | Method for preparing high purity super fine silicon miropowder by using powder of natural quartz |
| CN101033068A (en) * | 2007-02-13 | 2007-09-12 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN101817533A (en) * | 2010-04-27 | 2010-09-01 | 中国地质大学（武汉） | Preparation method of electronic-level crystalline silicon powder |
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