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 PDF

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Publication number
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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China
Prior art keywords
flotation
concentrate
quartz
quartz sand
grade silicon
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CN202011490359.3A
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Chinese (zh)
Inventor
潘力
彭善志
杜祥国
方志武
孙翔
宋志达
汪国军
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Kaisheng Quartz Material Huangshan Co ltd
CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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Kaisheng Quartz Material Huangshan Co ltd
CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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Priority to CN202011490359.3A priority Critical patent/CN112619884A/en
Publication of CN112619884A publication Critical patent/CN112619884A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B7/00Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00General arrangement of separating plant, e.g. flow sheets
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional 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+、ClThe 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+、ClThe 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

Method for preparing electronic grade silicon micropowder by utilizing vein quartz flotation tailings
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
Figure 36312DEST_PATH_IMAGE002
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.
CN202011490359.3A 2020-12-16 2020-12-16 Method for preparing electronic grade silicon micropowder by utilizing vein quartz flotation tailings Pending CN112619884A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
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