CN114534905A - Quartz sand tail mud recycling method - Google Patents
Quartz sand tail mud recycling method Download PDFInfo
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- CN114534905A CN114534905A CN202210144515.3A CN202210144515A CN114534905A CN 114534905 A CN114534905 A CN 114534905A CN 202210144515 A CN202210144515 A CN 202210144515A CN 114534905 A CN114534905 A CN 114534905A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000004064 recycling Methods 0.000 title claims abstract description 30
- 239000010453 quartz Substances 0.000 claims abstract description 48
- 238000005406 washing Methods 0.000 claims abstract description 45
- 238000005188 flotation Methods 0.000 claims abstract description 41
- 239000012535 impurity Substances 0.000 claims abstract description 24
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 19
- 238000007885 magnetic separation Methods 0.000 claims abstract description 19
- 239000011734 sodium Substances 0.000 claims abstract description 19
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 16
- 230000005291 magnetic effect Effects 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims description 52
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 16
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000002378 acidificating effect Effects 0.000 claims description 15
- 239000003112 inhibitor Substances 0.000 claims description 13
- 239000003921 oil Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 125000002091 cationic group Chemical group 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- -1 hydrogen ions Chemical class 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 5
- 239000013307 optical fiber Substances 0.000 claims description 5
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011825 aerospace material Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000010433 feldspar Substances 0.000 abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 15
- 239000013078 crystal Substances 0.000 abstract description 8
- 239000012530 fluid Substances 0.000 abstract description 7
- 150000001768 cations Chemical class 0.000 abstract description 3
- 239000004927 clay Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000005294 ferromagnetic effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000013068 control sample Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- MDIBXLWYZGZAKL-UHFFFAOYSA-N 1,1,3-triethoxybutane Chemical compound CCOC(C)CC(OCC)OCC MDIBXLWYZGZAKL-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The application discloses a quartz sand tailings recycling method, metal impurities in clay mud are removed through washing, magnetic metal impurities and ferromagnetic ores in the quartz sand tailings mud are removed through magnetic separation, then fluid inclusion and quartz crystal lattices are damaged through low-temperature crushing, aluminum impurities in the fluid inclusion and the quartz crystal lattices are exposed, the aluminum impurities are removed through acid washing, and aluminum and other impurities which are not removed in feldspar are removed through a flotation method, the feldspar is floated through a cation collecting agent, sodium silicofluoride is adopted to activate the feldspar and inhibit the quartz, and finally the high-purity and high-yield quartz is obtained.
Description
Technical Field
The application relates to the field of deep processing of quartz sand tailing mud, in particular to a method for recycling quartz sand tailing mud.
Background
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 annual discharge amount of quartz sand tailings in China is tens of millions of tons, and the discharge of a large amount of quartz tailings directly causes serious environmental pollution, farmland occupation, silting of rivers and reservoirs and other adverse effects, so that resource utilization becomes a necessary trend.
The high-purity quartz powder has excellent optical performance, thermal stability, chemical stability and radiation resistance, is a main raw material for producing high-performance materials such as monocrystalline silicon, polycrystalline silicon, quartz glass, optical fibers, solar cells, integrated circuit substrate materials and the like, and has wide application in the aspects of electronic industry, electric light sources, optical communication, military industry and the like. With the development of the fields of electronic industry, optical communication, laser, optics and the like, the requirement of enterprises on high-purity quartz materials is higher and higher, and the demand is also higher and higher.
Some enterprises apply the quartz sand tail mud to products such as ceramic glaze, aggregate for coating, special mortar, nutrient soil, firework and firecracker filling material, fire-resistant silicon mud, building ceramsite, hydrated calcium silicate and the like after washing, grading, magnetic separation, acid washing and drying, but the products are low-end products, and how to highly purify the quartz sand tail mud is applied to monocrystalline silicon, polycrystalline silicon, quartz glass, optical fibers, solar cells, integrated circuit substrate materials and the like, so that the application value of the quartz sand tail mud is improved, and the technical problem to be solved by the application is solved.
Aluminum is an impurity which is difficult to remove from quartz powder, and the aluminum content in quartz is difficult to reach the standard of high-purity quartz. The aluminum element exists in quartz sand mainly in 3 forms: the first is in the aluminum-containing minerals such as feldspar, mica and clay; secondly, the quartz crystal is in a wrapping body form; and the third is in the form of a homogeneous image in the quartz crystal lattice. The removal mode also differs for the aluminium element present in different forms: (1) clay minerals are generally removed by desliming. (2) For aluminum impurities and fluid inclusions existing in the quartz crystal grid network instead of silicon atoms, the aluminum impurities and the fluid inclusions are difficult to remove by a common treatment method, and high-temperature roasting and hydrofluoric acid pickling can be adopted. (3) For feldspar containing aluminum ore, since feldspar is Si in quartz crystal4+Is covered with Al3+After substitution, mixing in K+、Na+And the feldspar and the quartz are difficult to separate by gravity separation and magnetic separation, and flotation is the most effective method for separating the feldspar from the quartz. For feldspar and mica oresAccording to the method, a good removal effect can be achieved only by using a hydrofluoric acid flotation process, and when the pH value is 2-3, a proper amount of HF and a cation collector are added into ore pulp to preferentially float feldspar, so that the purpose of flotation and separation of feldspar and quartz is achieved. At present, the hydrofluoric acid method has better effect in industrial application, is a main process for separating feldspar and quartz, but has strong harm to the environment because HF has high toxicity.
Disclosure of Invention
Therefore, the application provides a method for recycling the quartz sand tailings, and fluorine-free flotation and feldspar flotation are adopted to obtain high-purity quartz.
The technical scheme of the application is realized as follows:
a quartz sand tail mud recycling method comprises the following steps:
(1) washing with water: washing quartz sand tail mud with water to remove mud;
(2) magnetic separation: carrying out magnetic separation on the washed quartz sand tailings to remove magnetic metal impurities and strong magnetic ores;
(3) grading: grading the quartz sand tailings after the magnetic separation to obtain ultrafine-grained quartz sand tailings, fine-grained quartz sand tailings and coarse-grained quartz sand tailings;
(4) low-temperature grinding, namely grinding the quartz sand tailings with fine granularity and coarse granularity at low temperature, and mixing the ground quartz sand tailings with the superfine granularity obtained in the step (3) to form superfine powder;
(5) flotation: preparing a cationic collector tetraethylammonium chloride aqueous solution, adding an inhibitor, adjusting the pH to be neutral or alkalescent by using a sodium hydroxide solution with the molar concentration of 0.15-10mol/L, and adding the ultrafine powder subjected to acid washing and filtering and No. 4 flotation oil for flotation; the inhibitor is a specific mixture of sodium sulfide and sodium silicofluoride; the feldspar is activated by adopting the sodium silicofluoride, the sodium sulfide and the sodium silicofluoride cooperatively inhibit quartz, the purity of the quartz is not high, and the purity of the quartz can be obviously improved by matching the sodium sulfide and the sodium silicofluoride. The No. 4 flotation oil belongs to an alkoxy hydrocarbon foaming agent, and the main component of the flotation oil is 1, 1, 3-triethoxy butane. (6) Water washing, dewatering and drying: washing, dehydrating and drying the residual materials after flotation to obtain quartz.
The further technical scheme is that the ultrafine-grained quartz sand tailings in the step (3) are 150-150 meshes, the fine-grained quartz sand tailings are 80-150 meshes, and the coarse-grained quartz sand tailings are 20-80 meshes.
The further technical proposal is that the low-temperature crushing condition in the step (4) is the temperature of-65 ℃ to 0 ℃.
The further technical scheme is that the aqueous solution of the tetraethylammonium chloride as the cationic collector prepared in the step (5) is diluted by softened water to form the aqueous solution of the tetraethylammonium chloride with the molar concentration of 0.005-0.015 mol/L. Because hard water contains calcium and magnesium salts, softened water is used for flotation in order to prevent calcium and magnesium ions from activating quartz.
The further technical proposal is that the molar concentration of the sodium sulfide in the tetraethylammonium chloride aqueous solution in the step (5) is 0.003-0.025mol/L, and the molar concentration of the sodium silicofluoride is 0.002-0.008mol/L
The further technical scheme is that the acid washing in the step (5) is to add superfine powder into an acidic aqueous solution for washing, wherein the acidic aqueous solution comprises one or more of hydrochloric acid aqueous solution, sulfuric acid aqueous solution and nitric acid aqueous solution, the molar concentration of hydrogen ions in the acidic aqueous solution is 0.55-1.35mol/L, and the acid washing temperature is 80-100 ℃. The purpose of the acid washing here is to remove impurities such as fluid wrapping the surface of the ultrafine powder to sufficiently expose feldspar and quartz.
The further technical proposal is that the volume ratio of the No. 4 flotation oil to the tetraethylammonium chloride aqueous solution in the step (5) is 1: 7000-8000.
The further technical proposal is that the concentration of the ultrafine powder in the tetraethylammonium chloride aqueous solution in the step (5) is 300 g/L.
The further technical scheme is that the pH value in the step (5) is 7.0-8.5, and the flotation time is 15-30 min.
The quartz obtained by the method for recycling the quartz sand tail mud is applied to the production of monocrystalline silicon, polycrystalline silicon, quartz glass, optical fibers, solar cells, integrated circuit substrates and aerospace materials.
Compared with the prior art, the beneficial effects of this application are:
(1) according to the method, metal impurities in clay mud are removed through water washing, magnetic metal impurities and strong magnetic ores in quartz sand tail mud are removed through magnetic separation, then fluid inclusion and quartz crystal lattices are damaged through low-temperature crushing, aluminum impurities in the fluid inclusion and the quartz crystal lattices are exposed, and then the aluminum impurities are removed through acid washing, and impurities such as aluminum which are not removed in feldspar are removed through a flotation method, feldspar is floated through a cation collecting agent, sodium silicofluoride is adopted to activate the feldspar and inhibit the quartz, and finally high-purity quartz is obtained.
(2) According to the method for recycling the quartz sand tail mud, the obtained quartz has high purity and high yield-to-liquid ratio, and can be applied to production of high-end products such as monocrystalline silicon, polycrystalline silicon, quartz glass, optical fibers, solar cells, integrated circuit substrates, aerospace materials and the like.
Detailed Description
In order to better understand the technical content of the application, specific examples are provided below for further explanation of the application.
Example 1
A quartz sand tail mud recycling method comprises the following steps:
(1) washing with water: washing quartz sand tail mud with water to remove mud;
(2) magnetic separation: carrying out magnetic separation on the washed quartz sand tailings to remove magnetic metal impurities and strong magnetic ores;
(3) grading: grading the quartz sand tailings after magnetic separation to obtain 150-mesh 300-mesh ultrafine-grained quartz sand tailings, 80-150-mesh fine-grained quartz sand tailings and 20-80-mesh coarse-grained quartz sand tailings;
(4) low-temperature crushing, namely crushing the quartz sand tailings with fine granularity and coarse granularity at the temperature of-65 ℃, and mixing the crushed quartz sand tailings with the superfine granularity quartz sand tailings obtained in the step (3) to form superfine powder;
(5) flotation: preparing a cationic collector tetraethylammonium chloride aqueous solution, adding an inhibitor, adjusting the pH to 7.0 by using sodium hydroxide, adding the acid-washed and filtered ultrafine powder and No. 4 flotation oil, and performing flotation for 30 min; the inhibitor is a mixture of sodium sulfide and sodium silicofluoride;
(6) water washing, dewatering and drying: washing, dehydrating and drying the residual materials after flotation to obtain quartz.
And (5) preparing the cationic collector tetraethylammonium chloride aqueous solution, namely diluting the tetraethylammonium chloride aqueous solution with softened water to 0.005 mol/L. The molar concentration of the sodium sulfide in the tetraethylammonium chloride aqueous solution is 0.003mol/L, the molar concentration of the sodium silicofluoride is 0.002mol/L, and the concentration of the superfine powder is 100 g/L. The volume ratio of the No. 4 flotation oil to the tetraethylammonium chloride aqueous solution is 1: 7000.
And (5) the acid washing is to add the superfine powder into an acidic aqueous solution for washing, wherein the acidic aqueous solution is a hydrochloric acid aqueous solution, the molar concentration of hydrogen ions in the acidic aqueous solution is 0.55mol/L, and the acid washing temperature is 100 ℃.
Example 2
A quartz sand tail mud recycling method comprises the following steps:
(1) washing with water: washing quartz sand tail mud with water to remove mud;
(2) magnetic separation: carrying out magnetic separation on the washed quartz sand tailings to remove magnetic metal impurities and strong magnetic ores;
(3) grading: grading the quartz sand tailings after magnetic separation to obtain 150-mesh 300-mesh ultrafine-grained quartz sand tailings, 80-150-mesh fine-grained quartz sand tailings and 20-80-mesh coarse-grained quartz sand tailings;
(4) low-temperature crushing, namely crushing the quartz sand tailings with fine granularity and coarse granularity at the temperature of-10 ℃, and mixing the crushed quartz sand tailings with the superfine granularity quartz sand tailings obtained in the step (3) to form superfine powder;
(5) flotation: adding an inhibitor after preparing a cationic collector tetraethylammonium chloride aqueous solution, adjusting the pH to 7.8 by using sodium hydroxide, adding the acid-washed and filtered ultrafine powder and No. 4 flotation oil for flotation for 20 min; the inhibitor is a mixture of sodium sulfide and sodium silicofluoride;
(6) water washing, dewatering and drying: washing, dehydrating and drying the residual materials after flotation to obtain quartz.
And (5) preparing the cationic collector tetraethylammonium chloride aqueous solution, namely diluting the tetraethylammonium chloride aqueous solution into a tetraethylammonium chloride aqueous solution with a molar concentration of 0.015mol/L by using softened water. The molar concentration of the sodium sulfide in the tetraethylammonium chloride aqueous solution is 0.025mol/L, the molar concentration of the sodium silicofluoride is 0.008mol/L, and the concentration of the superfine powder is 300 g/L. The volume ratio of the No. 4 flotation oil to the tetraethylammonium chloride aqueous solution is 1: 8000.
And (5) the acid washing is to add the superfine powder into an acidic aqueous solution for washing, wherein the acidic aqueous solution is a sulfuric acid aqueous solution, the molar concentration of hydrogen ions in the acidic aqueous solution is 1.35mol/L, and the acid washing temperature is 80 ℃.
Example 3
A method for recycling quartz sand tailing mud comprises the following steps:
(1) washing with water: washing quartz sand tail mud with water to remove mud;
(2) magnetic separation: carrying out magnetic separation on the washed quartz sand tailings to remove magnetic metal impurities and strong magnetic ores;
(3) grading: grading the quartz sand tailings after magnetic separation to obtain 150-mesh 300-mesh ultrafine-grained quartz sand tailings, 80-150-mesh fine-grained quartz sand tailings and 20-80-mesh coarse-grained quartz sand tailings;
(4) low-temperature grinding, namely grinding the quartz sand tailings with fine granularity and coarse granularity at the temperature of 0 ℃, and mixing the ground quartz sand tailings with the superfine granularity obtained in the step (3) to form superfine powder;
(5) flotation: preparing a cationic collector tetraethylammonium chloride aqueous solution, adding an inhibitor, adjusting the pH to 8.5 by using sodium hydroxide, adding the acid-washed and filtered ultrafine powder and No. 4 flotation oil, and performing flotation for 15-30 min; the inhibitor is a mixture of sodium sulfide and sodium silicofluoride;
(6) water washing, dewatering and drying: washing, dehydrating and drying the residual materials after flotation to obtain quartz.
And (5) preparing the cationic collector tetraethylammonium chloride aqueous solution, namely diluting the tetraethylammonium chloride aqueous solution with softened water to 0.010 mol/L. The molar concentration of the sodium sulfide in the tetraethylammonium chloride aqueous solution is 0.015mol/L, the molar concentration of the sodium silicofluoride is 0.005mol/L, and the concentration of the superfine powder is 200 g/L. The volume ratio of the No. 4 flotation oil to the tetraethyl ammonium chloride aqueous solution is 1: 7680.
And (5) the acid washing is to add the superfine powder into an acidic aqueous solution for washing, wherein the acidic aqueous solution is a nitric acid aqueous solution, the molar concentration of hydrogen ions in the acidic aqueous solution is 1.15mol/L, and the acid washing temperature is 90 ℃.
Comparative example 1
Compared with the embodiment 2, the low-temperature crushing in the step (4) in the quartz sand tail mud recycling method is performed at the temperature of 4 ℃, and other steps are the same as the embodiment 2.
Comparative example 2
Compared with the example 2, the low-temperature crushing in the step (4) of the quartz sand tail mud recycling method is crushed at the temperature of 25 ℃, and other steps are the same as the example 2.
Comparative example 3
Compared with the example 2, the pH value of the flotation in the step (5) in the quartz sand tailing slurry recycling method is 9.0, and other steps are the same as the example 2.
Comparative example 4
Compared with the example 2, the inhibitor for flotation in the step (5) in the quartz sand tail mud recycling method is free of sodium silicofluoride, and other steps are the same as the example 2.
Comparative example 5
Compared with the example 2, the inhibitor for flotation in the step (5) in the quartz sand tail mud recycling method is free of sodium sulfide, and other steps are the same as the example 2.
Detection results of quartz yield and purity
TABLE 1
As is clear from Table 1, the Al contents (average of 14.68X 10) in examples 1 to 3-6) Are significantly lower than the control sample, removing about 85% of the aluminum impurities; fe contents of examples 1 to 3 (average 28.68X 10)-6) Are significantly lower than the control sample, removing about 36% of the iron impurity; ga contents of examples 1 to 3 (average 52.19X 10)-6) Are significantly lower than the control sample, removing about 40% of calcium impurities; mg contents of examples 1 to 3 (average 0.45X 10)-6) Are significantly lower than the control sample, removing about 67% of the magnesium impurity.
Compared with example 2, the low-temperature crushing temperature changes of comparative examples 1 and 2 directly affect the contents of Al, Fe, Ga and Mg in quartz; comparative example 3 has a high pH value during flotation, and has certain influence on Al and Fe contents in quartz.
Comparative example 4 has high content of each element, but the quartz yield is close to that of example 2; comparative example 5 has low content of each element, but the quartz yield is significantly lower than that of example 2; it is illustrated that in comparative example 4, since sodium silicofluoride is not present, a part of feldspar and quartz are inhibited by sodium sulfide, resulting in obtaining quartz which is impure (containing feldspar) although having a high yield; in comparative example 5, since sodium sulfide was not contained, sodium silicofluoride activated feldspar, quartz was suppressed, and high purity quartz was obtained, but the yield was low.
On the other hand, in example 2, sodium sulfide and sodium silicofluoride are used as inhibitors, and the obtained quartz has low contents of Al, Fe, Ga, Mg and the like and high yield, which shows that the quartz with high yield and high purity is obtained in example 2.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for recycling quartz sand tailing mud is characterized by comprising the following steps: the method comprises the following steps:
(1) washing with water: washing quartz sand tail mud with water to remove mud;
(2) magnetic separation: carrying out magnetic separation on the washed quartz sand tailings to remove magnetic metal impurities and strong magnetic ores;
(3) grading: grading the quartz sand tailings after the magnetic separation to obtain superfine-granularity quartz sand tailings, fine-granularity quartz sand tailings and coarse-granularity quartz sand tailings;
(4) low-temperature grinding, namely grinding the quartz sand tailings with fine granularity and coarse granularity at low temperature, and mixing the ground quartz sand tailings with the superfine granularity obtained in the step (3) to form superfine powder;
(5) flotation: preparing a cationic collector tetraethylammonium chloride aqueous solution, adding an inhibitor, adjusting the pH to be neutral or alkalescent by using sodium hydroxide, and adding the ultrafine powder subjected to acid washing and filtering and No. 4 flotation oil for flotation; the inhibitor is a mixture of sodium sulfide and sodium silicofluoride;
(6) water washing, dewatering and drying: washing, dehydrating and drying the residual materials after flotation to obtain quartz.
2. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: the superfine-granularity quartz sand tailings in the step (3) are 150-mesh and 300-mesh, the fine-granularity quartz sand tailings are 80-150-mesh, and the coarse-granularity quartz sand tailings are 20-80-mesh.
3. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: the low-temperature crushing condition in the step (4) is a temperature of-65 ℃ to 0 ℃.
4. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: and (5) preparing the cationic collector tetraethylammonium chloride aqueous solution, namely diluting softened water into a tetraethylammonium chloride aqueous solution with the molar concentration of 0.005-0.015 mol/L.
5. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: and (5) the molar concentration of the sodium sulfide in the tetraethylammonium chloride aqueous solution in the step (5) is 0.003-0.025mol/L, and the molar concentration of the sodium silicofluoride is 0.002-0.008 mol/L.
6. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: and (5) the acid washing is to add superfine powder into an acidic aqueous solution for washing, wherein the acidic aqueous solution comprises one or more of hydrochloric acid aqueous solution, sulfuric acid aqueous solution and nitric acid aqueous solution, the molar concentration of hydrogen ions in the acidic aqueous solution is 0.55-1.35mol/L, and the acid washing temperature is 80-100 ℃.
7. The method for recycling the quartz sand tailing mud according to claim 1, characterized by comprising the following steps: the volume ratio of the No. 4 flotation oil to the tetraethylammonium chloride aqueous solution in the step (5) is 1: 7000-8000.
8. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: the concentration of the ultrafine powder in the tetraethylammonium chloride aqueous solution in the step (5) is 300 g/L.
9. The method for recycling the quartz sand tailings as claimed in claim 1, wherein the method comprises the following steps: the pH value in the step (5) is 7.0-8.5, and the flotation time is 15-30 min.
10. Use of quartz obtained by a method of recycling quartz sand tailings according to claims 1-9 for the production of monocrystalline silicon, polycrystalline silicon, quartz glass, optical fibers, solar cells, integrated circuit substrates, aerospace materials.
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