CN112619884A - Method for preparing electronic grade silicon micropowder by utilizing vein quartz flotation tailings - Google Patents
Method for preparing electronic grade silicon micropowder by utilizing vein quartz flotation tailings Download PDFInfo
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- CN112619884A CN112619884A CN202011490359.3A CN202011490359A CN112619884A CN 112619884 A CN112619884 A CN 112619884A CN 202011490359 A CN202011490359 A CN 202011490359A CN 112619884 A CN112619884 A CN 112619884A
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- flotation
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- quartz
- quartz sand
- grade silicon
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000005188 flotation Methods 0.000 title claims abstract description 75
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000010453 quartz Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 23
- 239000010703 silicon Substances 0.000 title claims abstract description 23
- 210000003462 vein Anatomy 0.000 title claims abstract description 17
- 239000006004 Quartz sand Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000004140 cleaning Methods 0.000 claims abstract description 24
- 238000007885 magnetic separation Methods 0.000 claims abstract description 17
- 239000004576 sand Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims description 51
- 239000000126 substance Substances 0.000 claims description 12
- 239000006148 magnetic separator Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000005201 scrubbing Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000011863 silicon-based powder Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 description 19
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000004566 building material Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a method for preparing electronic grade silicon micropowder by using vein quartz flotation tailings, which is characterized by comprising the following steps: the flotation tailing of natural vein quartz is used as a raw material, flotation circulating water is adopted to adjust the concentration of ore pulp, and through the steps of flotation, reagent removal, cleaning and drying, the adhesion of a reagent on the surface of fine sand of quartz sand is reduced, and the conductivity and K of an extraction liquid are reduced simultaneously+、Na+、Cl‑The content of the silicon powder is ensured to meet the raw material requirement of the electronic grade silicon powder. And finally preparing the electronic grade silicon micro powder by dry magnetic separation, grinding and classification. The invention has the advantages that: the flotation tailings are subjected to secondary flotation, quartz sand in the flotation tailings is recycled, tailing discharge is reduced, comprehensive utilization of resources is realized, the difficulty in treatment of acid-containing wastewater is reduced, and the prepared silicon micropowder and SiO thereof2≥99.0%、Fe2O3Less than or equal to 0.01 percent, the conductivity of the extract is less than or equal to 5 mu s/cm, K+、Na+、Cl‑The content is below 3ppm, which reaches the quality standard of electronic grade silicon micro powder and provides a method for high-value utilization of quartz tailings.
Description
Technical Field
The invention relates to the field of comprehensive utilization of nonmetallic ore tailings, and relates to a method for preparing electronic-grade silicon micropowder from quartz flotation tailings.
Background
Most of domestic quartz sand production enterprises do not carry out effective comprehensive utilization on the quartz tailings due to the reasons of more impurities, high iron content, finer granularity and the like, the treatment mode is mainly natural stacking or backfilling, a small part of the quartz tailings is sold to building material companies at low price, so that a large amount of resources are wasted, and the flotation tailings with the chemicals can also bring water body environment pollution. How to carry out deep processing on the quartz tailings to meet the requirements of more industries and efficiently utilize the quartz tailings is a problem which needs to be solved urgently in the industry.
The electronic grade silicon micro powder has excellent performances of high insulativity, high thermal conductivity, good thermal stability, low dielectric constant, low expansion coefficient, low friction coefficient and the like, and can be widely applied to plastic packaging materials and packaging materials of integrated circuits and electronic components.
The quartz tailings are deeply processed into electronic grade silicon micro powder, and a scheme is provided for high-value utilization of the tailings.
Disclosure of Invention
The invention aims to solve the problem of high-value utilization of quartz flotation tailings, and provides a method for preparing electronic-grade silicon micropowder from the flotation tailings.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing electronic grade silicon micropowder by using vein quartz flotation tailings is characterized by comprising the following steps:
a. size mixing: the natural vein quartz flotation tailing is used as a raw material, flotation circulating water is used for adjusting the natural vein quartz flotation tailing into ore pulp, the concentration of the ore pulp is controlled to be 40-60%, and H is added2SO4Adjusting the pH value of the ore pulp to 2-3;
b. flotation: introducing the pulp after size mixing into a flotation machine for flotation, adjusting the flotation concentration by using flotation circulating water, and controlling the flotation concentration to be 20-30% to obtain flotation concentrate;
c. removing the medicine, and cleaning: introducing the flotation concentrate into a spiral sand washer and a high-frequency dewatering screen in sequence to remove a quartz concentrate surface agent, introducing the flotation concentrate into a tandem scrubbing machine, and washing the flotation concentrate with clean water and deionized water successively to obtain quartz sand concentrate;
d. drying: drying the cleaned, dehydrated and concentrated quartz sand concentrate, and controlling the water content of the quartz sand concentrate to be below 0.1%;
e. magnetic separation: carrying out magnetic separation on the dried quartz sand concentrate, removing mechanical iron in the drying and transporting processes, reducing the content of magnetic substances, and increasing the magnetic separation field strength to be more than 0.8T;
f. grinding and grading: guiding the quartz sand concentrate after magnetic separation into a milling-grading system for milling and grading, and controlling the median particle diameter D50Preparing electronic-grade silicon powder at 8-10 μm, wherein the part of the whole grinding-grading system, which is in contact with quartz sand (powder), is made of silicon dioxide, aluminum oxide or polyurethane, so that the pollution of other impurities is avoided.
On the basis of the technical scheme, the following further technical scheme is provided:
step c, flotation concentrate and reagent removal, wherein a spiral sand washer and a high-frequency dewatering screen are sequentially adopted, the spiral sand washer reduces the water content of the flotation concentrate to 25-30%, the high-frequency dewatering screen reduces the water content of the flotation concentrate to 5-10%, and most of water and reagents in the flotation concentrate are removed; and then cleaning the flotation concentrate by using 3-6 scrubbing machines connected in series, cleaning the front 1-2 cleaning machines by using clean water, cleaning the rear cleaning machines by using deionized water, and dehydrating by using a high-frequency dehydration sieve after cleaning to obtain quartz sand concentrate with the water content of 5-10%.
And cleaning, dehydrating and concentrating the quartz sand concentrate, and drying the quartz sand concentrate by using a rotary kiln, wherein the water content of the quartz sand concentrate is controlled to be below 0.1%.
And (3) carrying out magnetic separation on the dried quartz sand concentrate, wherein a permanent magnet roller type magnetic separator is adopted, the field intensity of the magnetic separator is more than 0.8T, and the content of magnetic substances in the quartz sand concentrate is reduced to be below 3 ppm.
And g, quartz sand fine sand grinding and grading, namely grinding the quartz sand fine sand to the required granularity of electronic grade silicon micron (generally required median particle diameter D)508 to 10 μm) and reduces recontamination of impurities, particularly magnetic substances.
The invention has the advantages that: performing secondary flotation on the flotation tailings, recovering quartz sand in the flotation tailings, reducing tailing discharge and realizing comprehensive utilization of resources; circulating water is adopted for flotation, and a collecting agent is not required to be added, so that the medicament cost is greatly reduced; using very small amounts of H2SO4The flotation environment is adjusted, the acid consumption is greatly reduced, the treatment difficulty of acid-containing wastewater is reduced, and the method is environment-friendly; the deionized water can effectively reduce the conductivity and K of the quartz sand extract+、Na+、Cl-Content (c); reducing magnetic substances in the quartz sand through dry magnetic separation; the granularity reaches the requirement of electronic grade silicon micropowder by grinding and grading. The silicon powder, SiO thereof, prepared by the above process2≥99.5%、Fe2O3Less than or equal to 0.01 percent, the conductivity of the extract is less than or equal to 5 mu s/cm, K+、Na+、Cl-The content is below 3ppm, which reaches the quality standard of electronic grade silicon micro powder and provides a method for high-value utilization of quartz tailings.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed description of the invention
The invention is further illustrated with reference to fig. 1.
A method for preparing electronic grade silicon powder by using vein quartz flotation tailings, wherein the flotation tailings are from Kaihong quartz materials (Huangshan) Limited company, and are tailings obtained after the flotation of vein quartz ores of the company, the main components of the tailings are quartz and feldspar, a small amount of mica minerals, hematite and the like are also contained, and collecting agents are attached to the surfaces of the tailings.
The specific implementation steps are as follows:
a. size mixing: flotation tailing is used as a raw material, flotation circulating water is used for adjusting the concentration of ore pulp, and H is used2SO4Adjusting the pH value of the ore pulp to 2-3, and controlling the pulp adjusting concentration to 50%;
b. flotation: the pulp after size mixing flows into a self-suction flotation machine automatically, flotation circulating water is still used for adjusting the concentration, the concentration is controlled to be 20%, and flotation is directly carried out without adding a collecting agent to obtain flotation concentrate.
Removing the medicine, and cleaning: and removing the surface agent from the flotation concentrate after flotation through a spiral sand washer and a high-frequency dewatering screen. And cleaning the flotation concentrate sand by using a tandem type cleaning machine, wherein the cleaning machines are connected in series by 5 cleaning machines, the front 2 cleaning machines are cleaned by using clean water, the rear 3 cleaning machines are cleaned by using deionized water, the using amount of the clean water is 3 times of the quartz sand amount, and the using amount of the deionized water is 5 times of the flotation concentrate sand amount, so that the quartz sand concentrate sand is finally obtained.
And drying: concentrating, dewatering and drying the cleaned quartz sand concentrate, and controlling the water content to be below 0.1%. The index of the quartz sand is SiO2 99.7%、Fe2O30.0068%, conductivity less than or equal to 3 mu s/cm, K+、Na+、Cl-The content is below 3ppm, and the content of magnetic substance is 2.5 ppm.
And magnetic separation: and a permanent magnet roller type dry magnetic separator is adopted to carry out magnetic separation on the quartz sand concentrate, mechanical iron brought in the drying and conveying processes is removed, and the content of magnetic substances is reduced. The field intensity of the magnetic separator is 1.0T, the magnetic separator is of a three-section type, and the content of magnetic substances after magnetic separation is reduced to 1.0 ppm.
Grinding-grading: and (3) introducing the quartz sand refined sand subjected to magnetic separation into the milled powder of the ball mill, wherein the milling medium and the lining of the ball mill are made of quartz stone, the pipeline is coated with polyurethane, and the granularity is controlled by cyclone classification to prepare the electronic-grade silicon micropowder.
The indexes of the silicon powder prepared by the process are shown in table 1:
TABLE 1 indexes of electronic grade silica powder prepared by the present invention
The results show that: the silicon powder prepared by the method reaches the electronic grade silicon powder standard (refer to SJ/T10675-.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Those skilled in the art can make possible variations and modifications, or modify equivalents, to the embodiments using the methods and techniques disclosed above, while remaining within the scope of the invention.
Claims (6)
1. A method for preparing electronic grade silicon micropowder by using vein quartz flotation tailings is characterized by comprising the following steps:
a. size mixing: the natural vein quartz flotation tailing is used as a raw material, flotation circulating water is used for adjusting the natural vein quartz flotation tailing into ore pulp, the concentration of the ore pulp is controlled to be 40-60%, and H is added2SO4Adjusting the pH value of the ore pulp to 2-3;
b. flotation: introducing the pulp after size mixing into a flotation machine for flotation, adjusting the flotation concentration by using flotation circulating water, and controlling the flotation concentration to be 20-30% to obtain flotation concentrate;
c. removing the medicine, and cleaning: introducing the flotation concentrate into a spiral sand washer and a high-frequency dewatering screen in sequence to remove a quartz concentrate surface agent, introducing the flotation concentrate into a tandem scrubbing machine, and washing the flotation concentrate with clean water and deionized water successively to obtain quartz sand concentrate;
d. drying: drying the cleaned, dehydrated and concentrated quartz sand concentrate, and controlling the water content of the quartz sand concentrate to be below 0.1%;
e. magnetic separation: carrying out magnetic separation on the dried quartz sand concentrate, removing mechanical iron in the drying and transporting processes, reducing the content of magnetic substances, and increasing the magnetic separation field strength to be more than 0.8T;
f. grinding and grading: guiding the quartz sand concentrate after magnetic separation into a milling-grading system for milling and grading, and obtaining the median particle diameter D50Controlling the particle size to be 8-10 mu m, and preparing the electronic grade silicon micro powder.
2. The method for preparing electronic grade silicon micropowder by using the vein quartz flotation tailings as claimed in claim 1, wherein the method comprises the following steps:
step c, flotation concentrate and reagent removal, wherein a spiral sand washer and a high-frequency dewatering screen are sequentially adopted, the spiral sand washer reduces the water content of the flotation concentrate to 25-30%, the high-frequency dewatering screen reduces the water content of the flotation concentrate to 5-10%, and most of water and reagents in the flotation concentrate are removed; and then cleaning the flotation concentrate by using 3-6 scrubbing machines connected in series, cleaning the front 1-2 cleaning machines by using clean water, cleaning the rear cleaning machines by using deionized water, and dehydrating by using a high-frequency dehydration sieve after cleaning to obtain quartz sand concentrate with the water content of 5-10%.
3. The method for preparing electronic grade silicon micropowder by using the vein quartz flotation tailings as claimed in claim 1 or 2, wherein the method comprises the following steps: and cleaning, dehydrating and concentrating the quartz sand concentrate, and drying the quartz sand concentrate by using a rotary kiln, wherein the water content of the quartz sand concentrate is controlled to be below 0.1%.
4. The method for preparing electronic grade silicon micropowder by using the vein quartz flotation tailings as claimed in claim 1 or 2, wherein the method comprises the following steps: and (3) carrying out magnetic separation on the dried quartz sand concentrate, wherein a permanent magnet roller type magnetic separator is adopted, the field intensity of the magnetic separator is more than 0.8T, and the content of magnetic substances in the quartz sand concentrate is reduced to be below 3 ppm.
5. The method for preparing electronic grade silicon micropowder by using the vein quartz flotation tailings as claimed in claim 3, wherein the method comprises the following steps: and (3) carrying out magnetic separation on the dried quartz sand concentrate, wherein a permanent magnet roller type magnetic separator is adopted, the field intensity of the magnetic separator is more than 0.8T, and the content of magnetic substances in the quartz sand concentrate is reduced to be below 3 ppm.
6. The method for preparing electronic grade silicon micropowder by using the vein quartz flotation tailings as claimed in claim 1, wherein the method comprises the following steps: and g, quartz sand fine sand grinding and grading, namely grinding the quartz sand fine sand to the required granularity of electronic grade silicon micron, and controlling the median particle diameter D50At 8-10 μm, the recontamination of impurities, especially magnetic substances, is reduced.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6098810A (en) * | 1998-06-26 | 2000-08-08 | Pueblo Process, Llc | Flotation process for separating silica from feldspar to form a feed material for making glass |
CN103111364A (en) * | 2013-03-06 | 2013-05-22 | 合肥万泉非金属矿科技有限公司 | Technology of extracting quartz and feldspar from gangue |
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 |
CN107162008A (en) * | 2017-06-20 | 2017-09-15 | 合肥市惠科精密模具有限公司 | A kind of preparation technology of TFT LCD substrates glass quartz sand powder |
CN107188190A (en) * | 2017-07-07 | 2017-09-22 | 临沂昊泉硅业科技有限公司 | A kind of method that utilization quartz sand tailings produces silicon powder |
CN111841870A (en) * | 2019-04-28 | 2020-10-30 | 抚顺罕王傲牛矿业股份有限公司 | Energy-saving and environment-friendly ultra-pure fine iron powder continuous production process |
-
2020
- 2020-12-16 CN CN202011490359.3A patent/CN112619884A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6098810A (en) * | 1998-06-26 | 2000-08-08 | Pueblo Process, Llc | Flotation process for separating silica from feldspar to form a feed material for making glass |
CN103111364A (en) * | 2013-03-06 | 2013-05-22 | 合肥万泉非金属矿科技有限公司 | Technology of extracting quartz and feldspar from gangue |
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 |
CN107162008A (en) * | 2017-06-20 | 2017-09-15 | 合肥市惠科精密模具有限公司 | A kind of preparation technology of TFT LCD substrates glass quartz sand powder |
CN107188190A (en) * | 2017-07-07 | 2017-09-22 | 临沂昊泉硅业科技有限公司 | A kind of method that utilization quartz sand tailings produces silicon powder |
CN111841870A (en) * | 2019-04-28 | 2020-10-30 | 抚顺罕王傲牛矿业股份有限公司 | Energy-saving and environment-friendly ultra-pure fine iron powder continuous production process |
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Application publication date: 20210409 |