CN112408826A - Method for preparing plate silicon micropowder by using vein quartz tail mud - Google Patents
Method for preparing plate silicon micropowder by using vein quartz tail mud Download PDFInfo
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- CN112408826A CN112408826A CN202011305159.6A CN202011305159A CN112408826A CN 112408826 A CN112408826 A CN 112408826A CN 202011305159 A CN202011305159 A CN 202011305159A CN 112408826 A CN112408826 A CN 112408826A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
- C04B14/062—Microsilica, e.g. colloïdal silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/026—Comminuting, e.g. by grinding or breaking; Defibrillating fibres other than asbestos
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a method for preparing plate silicon micropowder by using vein quartz tail mud, which relates to the technical field of silicon micropowder preparation and comprises the following steps: (1) separating fine sand; (2) performing multi-section magnetic separation; (3) heating and pickling; (4) cleaning; (5) ball milling; (6) and (6) screening. The invention has the beneficial effects that: the method can be used for simultaneously preparing two kinds of silicon micro powder, wherein the quartz fine powder with the granularity of less than 800 meshes can be used as superfine plate micro powder, and the quartz fine powder with the granularity of more than 800 meshes can be used as plate silicon micro powder. The silicon content in the silicon powder prepared by the method is more than 99.5 percent, the whiteness is more than 95, and the Fe content is higher than that of the silicon powder2O3The content is less than 0.0051%.
Description
Technical Field
The invention relates to the technical field of silicon powder preparation, in particular to a method for preparing plate silicon powder by using vein quartz tail mud.
Background
The vein quartz sand tailings are valuable mineral resources, and the vein quartz tailings are mainly waste residues in ore mining and tailings in a processing process. After the quartz sand is washed out, the sand is precipitated again by using the sand washing water, and the sand is called as quartz sand tail mud. The conventional vein quartz tail mud is used for making bricks and other conventional products, and the utilization value is not high.
The plate silicon micropowder is used as a raw material for manufacturing plates, and the market demand is continuously increased in recent years. Compared with other common inorganic fillers, the silicon micropowder filler shows better mechanical properties, heat resistance, dispersibility, electrical properties and the like. In addition, compared with talcum powder, aluminum hydroxide, E-glass fiber and the like, the composite material has lower dielectric constant, lower water absorption and the like. Patent publication No. CN101417806A discloses silica micropowder and a method for producing the same, which uses raw quartz sand ore as a raw material to produce silica micropowder, but tail mud generated in the process of processing the raw quartz sand ore cannot be utilized.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing plate silicon micropowder by using vein quartz tail mud.
The invention solves the technical problems through the following technical means:
a method for preparing plate silicon micropowder by using vein quartz tail mud comprises the following steps:
(1) fine sand separation: separating and screening the vein quartz tail mud at the bottom of the thickener, and screening fine sand with more than 300 meshes;
(2) multi-stage magnetic separation: carrying out magnetic separation on the fine sand in the tail mud by using 1.0T and 1.5T, and removing iron components in the fine sand to obtain fine sand;
(3) heating and pickling: putting the refined sand subjected to magnetic separation into a pickling tank, and heating and pickling the refined sand by adopting mixed acid, wherein the mixed acid comprises hydrochloric acid and oxalic acid, and the volume ratio of the hydrochloric acid to the oxalic acid is 1.8: 1;
(4) cleaning: washing the washed concentrate with tap water until the pH value is 6-8;
(5) ball milling: performing dry ball milling on the cleaned refined sand by using zirconia balls as an ore grinding medium;
(6) screening: and screening the ball-milled quartz powder to screen out the silicon micro powder with the granularity smaller than 800 meshes and the granularity larger than 800 meshes.
Has the advantages that: the method can be used for simultaneously preparing two kinds of silicon micro powder, wherein the quartz fine powder with the granularity of less than 800 meshes can be used as superfine plate micro powder, and the quartz fine powder with the granularity of more than 800 meshes can be used as plate silicon micro powder. The silicon content in the silicon powder prepared by the method is more than 99.5 percent, the whiteness is more than 95, and the Fe content is higher than that of the silicon powder2O3The content is less than 0.0051%.
The mixed acid adopted by the invention can remove iron-containing minerals and has good removal effect on nonmetallic impurity minerals in the tail mud.
Preferably, in the step (1), a cyclone machine is adopted to separate and screen the vein quartz tail mud at the bottom of the thickener, and the feeding pressure of the cyclone machine is 0.1-0.6 MPa.
Preferably, the heating temperature in the step (3) is 80-100 ℃.
Preferably, in the step (5), a non-ore ball mill is adopted for dry grinding, wherein the length-diameter ratio of the ball mill is 1: 1-1: 3.
Preferably, in the step (6), the ball-milled quartz powder is classified by two air flow classifiers, the quartz powder with the granularity larger than 400 meshes, which is classified by the first classifier, returns to the non-ore ball mill for secondary ore grinding, the quartz powder with the granularity smaller than 400 meshes enters the second classifier, the classified quartz powder with the granularity smaller than 800 meshes is collected, and the quartz powder with the granularity larger than 800 meshes is collected.
Preferably, a dispersing agent is added during the dry ball milling process of the step (5).
Preferably, the zirconia balls have a diameter of 0.2 to 1.0 mm.
Preferably, the dispersant comprises a silane coupling agent.
Preferably, the dispersant is a silane coupling agent KH570 or a silane coupling agent KH 560.
Has the advantages that: a silane coupling agent KH570 or a silane coupling agent KH560 is adopted as a grinding aid dispersant.
Preferably, the addition amount of the dispersing agent is 0.1 per mill of the mass of the fine sand.
The invention has the advantages that: the method can be used for simultaneously preparing two kinds of silicon micro powder, wherein the quartz fine powder with the granularity of less than 800 meshes can be used as superfine plate micro powder, and the quartz fine powder with the granularity of more than 800 meshes can be used as plate silicon micro powder. The silicon content in the silicon powder prepared by the method is more than 99.5 percent, the whiteness is more than 95, and the Fe content is higher than that of the silicon powder2O3The content is less than 0.0051%.
The mixed acid adopted by the invention can remove iron-containing minerals and has good removal effect on nonmetallic impurity minerals in the tail mud.
The invention uses the waste material to purify the raw material which can be used for manufacturing the plate, improves the utilization rate and increases the practical value of the plate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
The method for preparing the plate silicon micropowder by using the vein quartz tail mud comprises the following steps:
(1) fine sand separation: separating and screening the vein quartz tailings at the bottom of the thickener by using a cyclone machine, and screening fine sand with the granularity of more than 300 meshes, wherein the cyclone machine is in the prior art, the equipment diameter of the cyclone machine is 150mm, the feeding pressure of the cyclone machine is adjusted to be 0.1MPa, and the fine sand with 300 meshes in the tailings is discharged from the bottom of the cyclone machine;
(2) multi-stage magnetic separation: carrying out magnetic separation on the fine sand in the tail mud by using 1.0T and 1.5T, and removing iron components in the fine sand to obtain fine sand;
(3) heating and pickling: and (3) putting the refined sand subjected to magnetic separation into a pickling tank, and heating and pickling the refined sand by using mixed acid, wherein the heating temperature is 80 ℃, and the mixed acid comprises hydrochloric acid and oxalic acid, and the volume ratio of the hydrochloric acid to the oxalic acid is 1.8: 1.
(4) Cleaning: washing the washed concentrate with tap water until the pH value is 6;
(5) ball milling: performing dry ball milling on cleaned refined sand by using zirconia balls as an ore milling medium, wherein the mass ratio of the zirconia balls to the refined sand is 1:1, and the ball milling time is 50 min;
(6) screening: and grading the ball-milled quartz powder by adopting two air flow grading machines, returning the quartz powder with the granularity of more than 400 meshes, which is separated by the first grading machine, to a non-ore ball mill for secondary ore grinding, feeding the quartz powder with the granularity of less than 400 meshes to the second grading machine, grading to obtain the quartz powder with the granularity of less than 800 meshes, and collecting the quartz powder with the granularity of more than 800 meshes.
Example 2
The method for preparing the plate silicon micropowder by using the vein quartz tail mud comprises the following steps:
(1) fine sand separation: separating and screening the vein quartz tailings at the bottom of the thickener by using a cyclone machine, and screening fine sand with the granularity of more than 300 meshes, wherein the cyclone machine is in the prior art, the equipment diameter of the cyclone machine is 150mm, the feeding pressure of the cyclone machine is adjusted to be 0.3MPa, and the fine sand with 300 meshes in the tailings is discharged from the bottom of the cyclone machine;
(2) multi-stage magnetic separation: carrying out magnetic separation on the fine sand in the tail mud by using 1.0T and 1.5T, and removing iron components in the fine sand to obtain fine sand;
(3) heating and pickling: and (3) putting the refined sand subjected to magnetic separation into a pickling tank, and heating and pickling the refined sand by using mixed acid, wherein the heating temperature is 90 ℃, and the mixed acid comprises hydrochloric acid and oxalic acid, and the volume ratio of the hydrochloric acid to the oxalic acid is 1.8: 1.
(4) Cleaning: washing the washed concentrate with tap water until the pH value is 6;
(5) ball milling: performing dry ball milling on cleaned refined sand by using zirconia balls as an ore milling medium, wherein the mass ratio of the zirconia balls to the refined sand is 2:1, and the ball milling time is 50 min;
(6) screening: and grading the ball-milled quartz powder by adopting two air flow grading machines, returning the quartz powder with the granularity of more than 400 meshes, which is separated by the first grading machine, to a non-ore ball mill for secondary ore grinding, feeding the quartz powder with the granularity of less than 400 meshes to the second grading machine, grading to obtain the quartz powder with the granularity of less than 800 meshes, and collecting the quartz powder with the granularity of more than 800 meshes.
Example 3
The method for preparing the plate silicon micropowder by using the vein quartz tail mud comprises the following steps:
(1) fine sand separation: separating and screening the vein quartz tailings at the bottom of the thickener by using a cyclone machine, and screening fine sand with the granularity of more than 300 meshes, wherein the cyclone machine is in the prior art, the equipment diameter of the cyclone machine is 150mm, the feeding pressure of the cyclone machine is adjusted to be 0.6MPa, and the fine sand with 300 meshes in the tailings is discharged from the bottom of the cyclone machine;
(2) multi-stage magnetic separation: carrying out magnetic separation on the fine sand in the tail mud by using 1.0T and 1.5T, and removing iron components in the fine sand to obtain fine sand;
(3) heating and pickling: and (3) putting the refined sand subjected to magnetic separation into a pickling tank, and heating and pickling the refined sand by using mixed acid, wherein the heating temperature is 100 ℃, and the mixed acid comprises hydrochloric acid and oxalic acid, and the volume ratio of the hydrochloric acid to the oxalic acid is 1.8: 1.
(4) Cleaning: washing the washed concentrate with tap water until the pH value is 8;
(5) ball milling: adopting zirconia balls as an ore grinding medium, carrying out dry ball milling on cleaned refined sand, adding a silane coupling agent KH570, wherein the addition amount of the silane coupling agent KH570 is 0.1 per mill of the mass of the refined sand, the mass ratio of the zirconia balls to the refined sand is 1:2, and the ball milling time is 60 min;
(6) screening: and grading the ball-milled quartz powder by adopting two air flow grading machines, returning the quartz powder with the granularity of more than 400 meshes, which is separated by the first grading machine, to a non-ore ball mill for secondary ore grinding, feeding the quartz powder with the granularity of less than 400 meshes to the second grading machine, grading to obtain the quartz powder with the granularity of less than 800 meshes, and collecting the quartz powder with the granularity of more than 800 meshes.
The product in example 1 was tested according to the prior art, and the test results are shown in table 1.
Table 1 shows the results of product index measurements
The silicon content of the silicon powder prepared by the method in the embodiment 1 of the invention is more than 99.5 percent, the whiteness is more than 95, and the Fe content2O3The content is less than 0.0051 percent, and the index in YB/T115-one 2004 standard is met.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing plate silicon micropowder by using vein quartz tail mud is characterized by comprising the following steps: the method comprises the following steps:
(1) fine sand separation: separating and screening the vein quartz tail mud at the bottom of the thickener, and screening fine sand with more than 300 meshes;
(2) multi-stage magnetic separation: carrying out magnetic separation on the fine sand in the tail mud by using 1.0T and 1.5T, and removing iron components in the fine sand to obtain fine sand;
(3) heating and pickling: putting the refined sand subjected to magnetic separation into a pickling tank, and heating and pickling the refined sand by adopting mixed acid, wherein the mixed acid comprises hydrochloric acid and oxalic acid, and the volume ratio of the hydrochloric acid to the oxalic acid is 1.8: 1;
(4) cleaning: washing the washed concentrate with tap water until the pH value is 6-8;
(5) ball milling: performing dry ball milling on the cleaned refined sand by using zirconia balls as an ore grinding medium;
(6) screening: and screening the ball-milled quartz powder to screen out the silicon micro powder with the granularity smaller than 800 meshes and the granularity larger than 800 meshes.
2. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: and (2) separating and screening the vein quartz tail mud at the bottom of the thickener by adopting a cyclone machine in the step (1), wherein the feeding pressure of the cyclone machine is 0.1-0.6 MPa.
3. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: the heating temperature in the step (3) is 80-100 ℃.
4. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: and (5) carrying out dry grinding by using a non-ore ball mill, wherein the length-diameter ratio of the ball mill is 1: 1-1: 3.
5. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: and (6) grading the ball-milled quartz powder by adopting two air flow grading machines, returning the quartz powder with the granularity of more than 400 meshes, which is separated by the first grading machine, to the non-ore ball mill for secondary ore grinding, feeding the quartz powder with the granularity of less than 400 meshes to the second grading machine, grading the quartz powder with the granularity of less than 800 meshes, and collecting the quartz powder with the granularity of more than 800 meshes.
6. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: and (5) adding a dispersing agent in the dry ball milling process of the step (5).
7. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: the diameter of the zirconia ball is 0.2-1.0 mm.
8. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: the dispersant includes a silane coupling agent.
9. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 1, which is characterized in that: the dispersing agent is a silane coupling agent KH570 or a silane coupling agent KH 560.
10. The method for preparing the plate silicon micropowder by using the vein quartz tail mud as claimed in claim 9, wherein the method comprises the following steps: the addition of the dispersant is 0.1 per mill of the mass of the fine sand.
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| CN202011305159.6A CN112408826A (en) | 2020-11-20 | 2020-11-20 | Method for preparing plate silicon micropowder by using vein quartz tail mud |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613103A (en) * | 2013-12-04 | 2014-03-05 | 南京工业大学东海先进硅基材料研究院 | Method for preparing filler-level silicon micropowder by using waste quartz crucibles as raw materials |
| CN103627215A (en) * | 2013-11-27 | 2014-03-12 | 连云港东海硅微粉有限责任公司 | Preparation method of submicron silica powder |
| 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 |
| 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 |
| CN108975679A (en) * | 2018-09-05 | 2018-12-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of TFT-LCD glass substrate silicon powder preparation method |
| CN109809411A (en) * | 2017-11-22 | 2019-05-28 | 连云港浩森矿产品有限公司 | A method of high pure and ultra-fine silica flour is prepared with waste and old quartz crucible |
-
2020
- 2020-11-20 CN CN202011305159.6A patent/CN112408826A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627215A (en) * | 2013-11-27 | 2014-03-12 | 连云港东海硅微粉有限责任公司 | Preparation method of submicron silica powder |
| CN103613103A (en) * | 2013-12-04 | 2014-03-05 | 南京工业大学东海先进硅基材料研究院 | Method for preparing filler-level silicon micropowder by using waste quartz crucibles as raw materials |
| 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 |
| 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 |
| CN109809411A (en) * | 2017-11-22 | 2019-05-28 | 连云港浩森矿产品有限公司 | A method of high pure and ultra-fine silica flour is prepared with waste and old quartz crucible |
| CN108975679A (en) * | 2018-09-05 | 2018-12-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of TFT-LCD glass substrate silicon powder preparation method |
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Application publication date: 20210226 |