CN117258995B - Method for extracting low-iron high-purity quartz and feldspar from granite pegmatite mineral dressing tailings - Google Patents
Method for extracting low-iron high-purity quartz and feldspar from granite pegmatite mineral dressing tailings Download PDFInfo
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- CN117258995B CN117258995B CN202311206080.1A CN202311206080A CN117258995B CN 117258995 B CN117258995 B CN 117258995B CN 202311206080 A CN202311206080 A CN 202311206080A CN 117258995 B CN117258995 B CN 117258995B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 239000010453 quartz Substances 0.000 title claims abstract description 160
- 239000010433 feldspar Substances 0.000 title claims abstract description 159
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000010438 granite Substances 0.000 title claims abstract description 29
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 25
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims description 41
- 239000011707 mineral Substances 0.000 title claims description 41
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 42
- 238000005188 flotation Methods 0.000 claims abstract description 155
- 239000012141 concentrate Substances 0.000 claims abstract description 134
- 239000002253 acid Substances 0.000 claims abstract description 64
- 238000007885 magnetic separation Methods 0.000 claims abstract description 33
- 238000002386 leaching Methods 0.000 claims abstract description 32
- 230000008569 process Effects 0.000 claims abstract description 27
- 230000002000 scavenging effect Effects 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 238000012216 screening Methods 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 28
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 23
- 239000004576 sand Substances 0.000 claims description 23
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 21
- 239000004088 foaming agent Substances 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- 238000012360 testing method Methods 0.000 claims description 18
- 150000002500 ions Chemical class 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000004566 building material Substances 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 5
- -1 alkaline earth metal cations Chemical class 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- 239000010665 pine oil Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 10
- 239000003814 drug Substances 0.000 abstract description 6
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 abstract description 5
- 125000002091 cationic group Chemical group 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 125000000129 anionic group Chemical group 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 132
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 13
- 239000012535 impurity Substances 0.000 description 11
- 239000010445 mica Substances 0.000 description 11
- 229910052618 mica group Inorganic materials 0.000 description 11
- 239000006004 Quartz sand Substances 0.000 description 9
- 229910010413 TiO 2 Inorganic materials 0.000 description 9
- 239000006260 foam Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 7
- 229910052629 lepidolite Inorganic materials 0.000 description 6
- 229910021642 ultra pure water Inorganic materials 0.000 description 6
- 239000012498 ultrapure water Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 4
- 238000007667 floating Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 229910052642 spodumene Inorganic materials 0.000 description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000005357 flat glass Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 239000006066 glass batch Substances 0.000 description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 239000006148 magnetic separator Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229960002050 hydrofluoric acid Drugs 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 241001070941 Castanea Species 0.000 description 1
- 235000014036 Castanea Nutrition 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000007497 glass batching Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 210000003462 vein Anatomy 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
-
- 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
- B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
-
- 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
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/30—Combinations with other devices, not otherwise provided for
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/002—Inorganic compounds
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/01—Organic compounds containing nitrogen
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/04—Frothers
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting low-iron high-purity quartz and feldspar from granite pegmatite tailings, which comprises the following steps: 1) Classifying by screening; 2) Performing strong magnetic separation; 3) Dan Yingzheng flotation; 4) Reverse flotation and rough separation of feldspar; 5) Reverse flotation and scavenging of feldspar 1; 6) Reverse flotation and scavenging of feldspar 2; 7) Hot-pressing acid leaching. The invention combines the forward flotation and the reverse flotation, has simple and novel process flow, can realize fluoride-free flotation, is better than the conventional single reverse flotation process, can efficiently realize the deep separation of quartz and feldspar by adopting the novel anionic and cationic medicament, has high purity of the obtained low-iron high-purity quartz concentrate and feldspar concentrate, is obviously better than the traditional medicament dodecylamine separation effect, effectively solves the current situations of resource waste and environmental pollution caused by the accumulation of the granite peganite tailings, improves the economic benefit and the social benefit of enterprises, has wide application range, accords with the green environment protection concept, and can realize the tailing-free treatment of mine tailings.
Description
Technical Field
The invention belongs to the technical field of tailing dressing, and particularly relates to a method for extracting low-iron high-purity quartz and feldspar from granite pegmatite dressing tailings.
Background
The development and utilization of mine tailings are one of the fields with the greatest comprehensive utilization potential of minerals and the best economic and social benefits. The tailings are directly discarded after the main metal part is recovered in the traditional metal mine, non-metal resources in the tailings are not recovered, and non-metal ores such as quartz, feldspar, mica, fluorite, garnet and the like are all reserved in the tailings, so that the traditional metal mine is an important building material raw material. The non-metal resources are ignored, so that the economic benefits of enterprises are influenced, mineral resources are wasted, the service life of a tailing pond is greatly reduced, and the environmental hazard is serious. Therefore, research into recovery of nonmetallic resources from metallic ore tailings is particularly important.
After the pegmatite spodumene and lepidolite are floated, a large amount of tailings with feldspar and quartz as main components are generated, and the feldspar and quartz have wide application in various fields of building materials, ceramics, glass, refractory materials, electronic appliances and the like, so that the quartz and the feldspar in the tailings are recovered, and high-purity quartz sand and feldspar concentrate are prepared to achieve the purpose of comprehensive utilization.
With the rapid development of technology in recent years, high-purity quartz sand has become an indispensable key raw material in the emerging industrial fields such as high-technology fields of electronic information, semiconductors, photovoltaics, optical communication, quartz crucibles, monocrystalline silicon, polycrystalline silicon, new energy sources and the like. These industries have high requirements on purity and granularity of quartz sand, and generally require SiO 2 The content is more than 99.9 percent, fe 2 O 3 The content is less than 10 mug/g (Fe content is less than 7 mug/g), and the granularity is required to be 0.104mm-0.425mm (140 meshes-40 meshes). At present, only vein quartz, natural crystal and granite pegmatite which can be used as high-purity quartz raw materials in China have small resource reserves and cannot meet the huge demand of the high-purity quartz market, so that the recovery of quartz from the granite pegmatite tailing resources is a necessary development trend of the high-purity quartz industry.
Zhang Jie recovering feldspar and quartz from spodumene ore flotation tailings, and performing reverse flotation on the feldspar by using a hydrofluoric acid method to obtain K 2 O、Na 2 The feldspar concentrate with O grade of 4.13 percent and 7.46 percent and recovery rate of 98.03 percent and 98.42 percent respectively, and the SiO is obtained 2 Quartz concentrate with 98.94 percent of content, HF flotation pollutes environment, and quartz concentrate SiO obtained by single reverse flotation feldspar process 2 The content is 98.94%, the purity of the quartz concentrate is required to be further improved, and the standard of high-purity quartz with high added value is not achieved.
Chen the mineral analysis is carried out on the flotation tailings of a spodumene ore dressing plant, and the useful components such as mica, quartz, feldspar and the like in the tailings are recovered by adopting a flotation-magnetic separation-flotation dressing process flow. The flotation separation of feldspar and quartz adopts HF pulp mixing and dodecyl amine as a collector to reversely float the feldspar, the test obtains the mica concentrate with the yield of 18.31 percent, the yield of 37.38 percent, the potassium-sodium content of 13.30 percent and the calcination whiteness of 78.9 percent at 1200 ℃,yield 28.07% of SiO 2 Grade is 98.34 percent, fe 2 O 3 Quartz concentrate with a content of 0.038%. The process adopts HF size mixing and traditional agent dodecyl amine reverse flotation to separate quartz and feldspar, which not only pollutes the environment, but also obtains quartz concentrate SiO 2 The purity of 98.34% is lower to be further improved.
Peng Guangju the gravity tailings of the chestnut tin ore dressing plant are subjected to strong magnetic separation and de-ironing, and then subjected to mica, feldspar and quartz flotation separation research. The pH value is regulated by sulfuric acid, and the collector GL is used for reverse flotation of feldspar to obtain K 2 O +Na 2 10.18% O feldspar concentrate, siO 2 93.71 percent of quartz concentrate, wherein the quartz concentrate only meets the siliceous raw materials for the plate glass and has lower added value.
Duan Shutong the gold mine tailings from Liaoning area are used as research object, and a process of 'medium magnetism-strong magnetism-scrubbing-floatation' is adopted, wherein sulfuric acid scrubbing and HF are used as feldspar activator for floatation, thus obtaining K 2 O grade 9.62%, fe 2 O 3 The feldspar refined sand with the grade of 0.18 percent pollutes the environment by adopting HF as a feldspar activator, and the quartz is not recycled, so that the resource waste is caused.
Liu Shujie separating feldspar and quartz from certain tin tailings by adopting a fluorine-free process, and performing sulfuric acid slurry mixing to reversely float the feldspar to obtain SiO (silicon dioxide) in the quartz 2 The content is increased from 77.82% to 93.71%, and the K in feldspar is increased 2 O+Na 2 The O content is improved from 6.67% to 10.18%, and the quality of quartz concentrate is lower to be further improved.
Miao Xing the method comprises the steps of preliminary sedimentation desliming, strong magnetic separation iron removal, reverse flotation iron removal and SiO 2 The flotation purification process is tested to obtain SiO 2 Content 98.46%, al 2 O 3 0.65% of Fe 2 O 3 Quartz sand concentrate with the content of 0.09 percent reaches the secondary quality standard of national grade glass raw materials. But the purified quartz sand concentrate SiO 2 Low content of Fe 2 O 3 And Al 2 O 3 The content is higher, the glass raw material can be only used, and the added value of the product is lower to be further improved.
Chinese patent CN107511251 a discloses a method for recovering mica and feldspar from kaolin tailingsAnd quartz sand, and through the process of heavy-magnetic-floating-reverse floatation of feldspar, siO is obtained 2 99.2%、Al 2 O 3 0.46%、Fe 2 O 3 0.012% of quartz sand concentrate to obtain K 2 O 9.3%、Na 2 O 0.56%、Fe 2 O 3 0.085% of feldspar concentrate is fully recovered, but the obtained quartz sand concentrate does not reach high purity, and the quality of the quartz concentrate and the added value of the product are required to be improved.
Chinese patent CN 115178363A discloses a process for preparing ultra-high purity quartz powder from mudstone and comprehensively utilizing the same, wherein HF is adopted to adjust pH to 2.5, and mixed reagent of dodecyl sodium sulfate and dodecyl sodium sulfate is adopted to carry out floatation to obtain high purity quartz powder SiO 2 More than 99.9%, but the quartz granularity is finer, the application range is limited, and the F ion causes environmental pollution and is not friendly to the environment.
The present invention has been made in view of this.
Disclosure of Invention
The invention aims to overcome the defect that the prior art uses an HF method to adjust the ore pulp to pollute the environment, and the conventional reagent reverse flotation to separate quartz and feldspar leads to low quality of concentrate, and provides a method for extracting low-iron high-purity quartz and feldspar from the granite pegmatite tailings, wherein the fluorine-free acid method is adopted for pulping, and the novel reagent with good selectivity and excellent synergistic effect is adopted for the novel reagent, so that the novel process combining the reverse flotation and the forward flotation is adopted to realize the efficient deep separation of the quartz and the feldspar, thereby providing the method for preparing the low-iron high-purity quartz and the feldspar from the granite pegmatite tailings.
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that:
a method for extracting low-iron high-purity quartz and feldspar from granite pegmatite mineral tailings comprises the following steps:
(1) And (5) screening and classifying: taking granite peganite tailings as an input raw ore, and screening and grading to obtain a +0.425mm material, -0.425+0.074mm material and-0.074 mm material;
(2) And (3) strong magnetic separation: carrying out two-stage strong magnetic separation tests on the materials with the diameters of between (1) and (0.425+0.074 mm) to obtain magnetic sand and nonmagnetic substances;
(3) Flotation of Dan Yingzheng: regulating the pH value of the ore pulp of the non-magnetic matters in the step (2) to 10-11 by using alkali, and then adding a novel Dan Yingyang ion collector DS-01 to perform a quartz forward flotation test to obtain quartz rough concentrate and alkaline feldspar concentrate;
meanwhile, combining the materials of 0.425mm and the magnetic separation sand of 0.425mm in the step (1) and the step (2) to be used as building materials;
(4) Reverse flotation roughing: adjusting the pH value of ore pulp to 2-3 by using acid in the quartz coarse concentrate in the step (3), then adding a novel feldspar negative and positive ion collector XK-02 and a foaming agent KW-03, and performing a reverse flotation coarse flotation feldspar test to obtain quartz coarse concentrate and feldspar concentrate 1;
(5) Reverse flotation and scavenging 1: adding acid into the quartz rough concentrate obtained in the step (4) to adjust the pH value of the ore pulp to 2-3, then adding a novel feldspar negative and positive ion collector XK-02 and a foaming agent KW-03, and performing a reverse flotation scavenging 1 test to obtain quartz rough concentrate and feldspar concentrate 2;
(6) Reverse flotation and scavenging 2: adding acid into the quartz rough concentrate in the step (5) to adjust the pH value of the ore pulp to 2-3, then adding a novel feldspar negative and positive ion collector XK-02 and a foaming agent KW-03, and performing a reverse flotation scavenging 2 test to obtain flotation quartz concentrate and feldspar concentrate 3;
(7) Hot-pressing acid leaching: combining the feldspar concentrate 1 in the step (4), the feldspar concentrate 2 in the step (5) and the feldspar concentrate 3 in the step (6) to be used as acid feldspar concentrate; carrying out hot-pressing acid leaching, washing and drying on the flotation quartz concentrate in the step (6) to obtain high-purity quartz concentrate;
wherein Dan Yingzheng flotation collector DS-01 is a polymer of alkaline earth metal cations and alkyl sulfonate; the feldspar negative and positive ion collector XK-02 is a mixture of compound amine, fatty acid and silicate inhibitor; the foaming agent KW-03 is a mixture of hydrocarbon oil and pine oil.
Further, the granite pegmatite tailings include, but are not limited to, lepidolite, spodumene, niobium, tantalum, beryllium, tungsten tailings; the fineness of the mineral dressing tailings is-0.425+0.074mm, the proportion of quartz mineral is 30-70%, and the proportion of feldspar mineral is 30-60%.
Further, in the step (1), the screening equipment is a standard screen for laboratory, and the standard screen meets the requirements of high-purity quartz granularity of 0.425mm (40 meshes) and 0.074mm (200 meshes).
Further, in the step (2), the strong magnetic separation is high-gradient magnetic separation, the magnetic separation operation comprises first-stage magnetic separation and second-stage magnetic separation, and the non-magnetic substance subjected to first-stage magnetic separation enters into the second-stage magnetic separation, and the magnetic field strength is 0.8-1.8T. The high-intensity magnetic separation and impurity removal operation can be carried out for a plurality of times according to the actual conditions of the granite pegmatite tailings.
Further, in the step (3), dan Yingzheng flotation is aerated flotation, the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding alkali to adjust the pH of ore pulp to 10-11, wherein the alkali is one or a mixture of sodium hydroxide and sodium carbonate, the concentration of the quartz positive flotation ore pulp is 20-35%, the dosage of the novel quartz cation collector is 300-800 g/t, the stirring speed is 800-1200 r/min, and the flotation time is 2-5 min.
Further, in the step (4), reverse flotation and roughing of feldspar are aerated flotation, a flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding acid to adjust the pH of ore pulp to 2-3, wherein the acid is one or a mixture of sulfuric acid, oxalic acid, nitric acid and hydrochloric acid, the concentration of quartz rough concentrate reverse flotation ore pulp is 15-30%, the dosage of the novel feldspar anion-cation mixed collector is 400-600 g/t, the dosage of the foaming agent is 50-100 g/t, the stirring rate is 800-1200 r/min, and the flotation time is 2-5 min.
Further, in the step (5), the reverse flotation and scavenging 1 is air flotation, the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding a small amount of acid to adjust the pH of ore pulp to 2-3, wherein the acid is one or a mixture of sulfuric acid, oxalic acid, nitric acid and hydrochloric acid, the concentration of the reverse flotation 1 ore pulp is 15-25%, the consumption of the novel feldspar anion-cation mixed collector is 100-300 g/t, the consumption of the foaming agent is 30-50g/t, the stirring rate is 800-1200 r/min, and the flotation time is 2-3 min.
Further, in the step (6), the reverse flotation 2 is aerated flotation, the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding a small amount of acid to adjust the pH of ore pulp to 2-3, wherein the acid is one or a mixture of sulfuric acid, oxalic acid, nitric acid and hydrochloric acid, the concentration of the reverse flotation 2 ore pulp is 10-25%, the consumption of the novel feldspar cation-anion mixed collector is 60-150 g/t, the consumption of the foaming agent is 20-40 g/t, the stirring rate is 800-1200 r/min, and the flotation time is 1-2 min.
In the process of reverse flotation of feldspar impurities, in order to obtain high-quality quartz concentrate, multiple reverse flotation can be performed according to actual conditions.
Further, in the step (5), the acid leaching process is as follows: at least one of ultrasonic acid leaching, stirring acid leaching and heating acid leaching, wherein the acid is mixed acid, and the mixed acid is a combination of two or more of nitric acid, hydrochloric acid, sulfuric acid and oxalic acid, and the leaching time is 4-24 hours.
Further, the SiO after the flotation of the quartz concentrate in the step (7) is pickled 2 More than or equal to 99.95 percent and Fe less than or equal to 10 mug/g, can be used as high-purity quartz concentrate.
The main components in the granite pegmatite mineral tailings are feldspar, quartz and mica, the content ratio of quartz minerals is only 30% or more, the feldspar and the feldspar are recovered from low-grade nonmetallic tailings, and are frame-shaped silicate rock-making minerals, the feldspar and the quartz are similar in crystal structure, physical property, chemical composition and the like, so that the flotation separation of the feldspar and the quartz is a mineral separation heavy difficulty, a fluoric acid method is the most widely used method, but fluoride ions pollute the environment, a fluoride-containing waste liquid treatment process is complex, a product purification facility is required, and the cost is increased.
According to the invention, the mineral components of the granite pegmatite mineral tailings are obtained by XRD, and the forward flotation quartz and reverse flotation feldspar are the technological innovation points of the invention. Under the condition of strong alkaline pH 10-11, the novel quartz cationic collector is adopted to realize the separation of quartz, the difference of collecting performance on the strong quartz collecting capability and the weak feldspar collecting capability is preferential to the forward flotation of quartz, after most feldspar is separated, the quartz rough concentrate is fully enriched and the quality is improved, then the quartz rough concentrate is used for regulating the pH 2-3 of ore pulp by sulfuric acid, the novel feldspar anionic-cationic mixed collector and the foaming agent are adopted to reversely float the feldspar, the reverse flotation times are carried out according to the actual condition of the ore, the product in the tank is the high-quality flotation quartz concentrate, the flotation foam product is the acid feldspar, and the quartz mineral content is 20-80% and the method is suitable for all.
According to the invention, through the combination and association of the novel medicament, the forward flotation Dan Yingyang ion collector can be used as a strong inhibitor of feldspar under alkaline conditions to drastically reduce the floatability of the forward flotation Dan Yingyang ion collector, so that the forward flotation Dan Yingyang ion collector is selectively adsorbed on the surface of quartz minerals to change the hydrophobicity of the surface of the quartz minerals, thereby achieving the purpose of separating the forward flotation Dan Yingyang ion collector from the feldspar; the negative and positive ion collector for reverse flotation of feldspar only forms weak electrostatic adsorption and molecular adsorption on the quartz surface, and has active Al on the feldspar surface 3+ Chemisorption of anionic collectors, also with K in the feldspar lattice + Or Na (or) + The positive charge cavity formed after dissolving in ore pulp is used for electrostatic adsorption of the cationic collector, so that various adsorption interaction and synergistic effects are formed, and the floatability of the feldspar is greatly improved. The selective synergistic effect of the novel medicament opens up a new path for fluoride-free flotation of quartz and feldspar, and greatly improves the precision and resource utilization efficiency of the quartz and the feldspar.
The invention belongs to comprehensive utilization of tailing resources, a large amount of pegmatite tailings are piled up in advance, the economic value is low, the nonmetallic beneficiation technology is poor, quartz and feldspar can be recovered by the novel method, no solid waste is discharged, the economic benefit is high, and under the environment-friendly concept, low-iron high-purity quartz concentrate and feldspar concentrate are produced by the invention, so that the high-valued comprehensive utilization of the granite pegmatite beneficiation tailings is realized, the idea of a green mine is met, the economic benefit of enterprises is increased, and the time development trend is met. In addition, the invention has strong applicability and wide applicability range, and has wider applicable market.
The invention obtains quartz concentrate SiO after hot-pressing acid leaching 2 More than or equal to 99.95 percent, fe less than or equal to 10 mug/g can be used as low-iron quartz concentrate, and at present SiO 2 More than or equal to 99.5 to 99.8 percent, and the content of Fe10-30 mug/g of exquisite quartz sand with market value of 3000-4000 yuan/ton, and the obtained feldspar concentrate contains Al 2 O 3 ≥14%、Fe 2 O 3 Less than or equal to 0.2 percent can be used as a high-quality raw material in the plate glass and ceramic industries, the market value is 200-300 yuan/ton, the magnetic separation mineral and the coarse sand with the grain size of +0.425mm are used as building materials, the fine sand with the grain size of-0.074 mm is used as glass ingredients, the ton treatment cost of the tailings of the process is about 200-300 yuan, the whole utilization of the tailings of the pegmatite is truly realized, and the economic value of mines is greatly improved.
By adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects.
The invention combines the forward flotation and the reverse flotation, has simple and novel process flow, can realize fluoride-free flotation, is better than the conventional single reverse flotation process, can efficiently realize the deep separation of quartz and feldspar by adopting the novel anionic and cationic medicament, has high purity of the obtained low-iron high-purity quartz concentrate and feldspar concentrate, is obviously better than the traditional medicament dodecylamine separation effect, effectively solves the current situations of resource waste and environmental pollution caused by the accumulation of the granite peganite tailings, improves the economic benefit and the social benefit of enterprises, has wide application range, accords with the green environment protection concept, and can realize the tailing-free treatment of mine tailings.
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiments of the invention and together with the description serve to explain the invention, without limitation to the invention. It is evident that the drawings in the following description are only examples, from which other drawings can be obtained by a person skilled in the art without the inventive effort. In the drawings:
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph comparing tailings from example 1 with a flotation concentrate of the present invention using ethylenediamine;
FIG. 3 is a graph comparing tailings from example 2 with a flotation concentrate of the present invention using ethylenediamine;
FIG. 4 is a graph comparing tailings from example 3 with a flotation concentrate of the present invention using ethylenediamine;
figure 5 lepidolite tailing XRD pattern.
It should be noted that these drawings and the written description are not intended to limit the scope of the inventive concept in any way, but to illustrate the inventive concept to those skilled in the art by referring to the specific embodiments.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments will be clearly and completely described with reference to the accompanying drawings in the embodiments of the present invention, and the following embodiments are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
The invention relates to a method for extracting low-iron high-purity quartz and feldspar from granite pegmatite mineral dressing tailings, which belongs to the technical field of tailings dressing, adopts a high-efficiency environment-friendly novel collector and a foaming agent to carry out deep flotation separation on quartz and feldspar under the condition of a fluorine-free acid method, obtains mineral components of the granite pegmatite mineral dressing tailings according to XRD, and designs and sorts the mineral components, carries out high-intensity magnetic separation, positive flotation, reverse flotation and hot-pressure acid leaching to obtain low-iron high-purity quartz and feldspar concentrate, and comprises the following steps: 1) Classifying by screening; 2) Performing strong magnetic separation; 3) Dan Yingzheng flotation; 4) Reverse flotation and rough separation of feldspar; 5) Reverse floating scavenging 1; 6) Reverse floating scavenging 2; 7) Hot-pressing acid leaching. The specific flow is as follows: firstly classifying materials to obtain +0.425mm coarse sand as building materials, classifying the materials with-0.425 mm grain size by a 0.074mm sieve to obtain-0.074 mm fine sand as glass ingredients, then performing twice strong magnetic separation on the materials with-0.425 mm+0.074mm grain size to obtain magnetic separation sand, wherein the magnetic separation sand can also be applied to the building materials, the non-magnetic materials are subjected to alkaline adjustment of pH value of ore pulp, a novel quartz cation collector DS-01 is adopted to perform positive flotation to obtain quartz coarse concentrate and alkaline feldspar concentrate, the quartz coarse concentrate is subjected to fluorine-free acid method to adjust pH value of ore pulp, a novel feldspar cation mixed collector XK-02 and a foaming agent KW-03 are added, acid feldspar concentrate and flotation quartz concentrate are obtained through one-time roughing and two-time scavenging, and the flotation quartz concentrate is subjected to hot-pressing acid leaching to obtain low-iron high-purity quartz concentrateAnd (5) ore. The feldspar concentrate produced by the forward flotation and reverse flotation processes contains Al 2 O 3 ≥14%、Fe 2 O 3 Less than or equal to 0.2 percent can be used as a high-quality raw material in the flat glass and ceramic industry, and the SiO after the flotation quartz concentrate is pickled 2 More than or equal to 99.95 percent and Fe less than or equal to 10 mug/g, can be used as high-purity quartz concentrate.
Examples
The ingredients of lepidolite mill tailings in a certain place in Hunan are shown in table 1.
TABLE 1 Multi-element analysis results of tailings (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
Content of | 78.20 | 11.09 | 0.804 | 0.032 | 3.15 | 2.90 | 1.27 | 0.374 |
Referring to FIG. 5, the tailings mainly comprise 62.99% of quartz mineral, 30.48% of feldspar mineral, 6.53% of mica mineral, 93.47% of the sum of quartz and feldspar mineral, 23.95% of tailings fineness of-0.074 mm and 72.28% of tailings fineness of-0.425+0.074mm.
Key equipment: a sieving machine, a standard sleeve sieve, a wet type strong magnetic separator, an XFD12 flotation machine, an electrothermal oven and a high-pressure reaction kettle.
The test flow is as in FIG. 1, and tailings are subjected to screening classification to obtain +0.425mm material, -0.425+0.074mm material and-0.074 mm material. Carrying out two-stage strong magnetic separation test on a material with the thickness of-0.425+0.074mm, wherein the magnetic field strength is 0.8-1.8T, and obtaining magnetic sand selection and non-magnetic substances; magnetic sand selection and +0.425mm material are mixed to be used as building materials, and-0.074 mm material is used as glass ingredients.
And (3) weighing a certain amount of non-magnetic matters, adding the non-magnetic matters into a 0.5L flotation tank of an XFD12 type flotation machine, wherein the concentration of flotation ore pulp is 30%, adding NaOH to adjust the pH of the ore pulp to be 10-11, stirring for 2 minutes, adding 800g/t of a novel Dan Yingyang ion collector, stirring for 1200r/min, stirring for 3 minutes, performing aerated flotation for 5 minutes, wherein a foam product is quartz rough concentrate, and a product in the tank is alkaline feldspar concentrate.
Feeding the quartz rough concentrate into a 0.5L flotation tank for reverse flotation of feldspar, wherein the concentration of flotation ore pulp is 20%, and adding H 2 SO 4 Regulating the pH value of ore pulp to 2-3, stirring for 2 minutes, adding 600g/t of novel feldspar anion-cation mixed collector, 100g/t of foaming agent, stirring at a speed of 1200r/min, stirring for 3 minutes, and floating for 3 minutes, wherein the foam product is acid feldspar concentrate, and the product in the tank is quartz concentrate. In order to ensure the grade of the flotation quartz concentrate, the step is performed for two more times, so that impurities such as feldspar and the like can be removed more thoroughly, and the tertiary feldspar concentrate is mixed to be used as the final acidic feldspar concentrate.
Washing the flotation quartz concentrate with ultrapure water for multiple times, drying, weighing 10 g of sample, and placing the sample into a high-pressure reaction kettle for heating and acid leaching test, wherein the mixed acid is HCl: HNO (HNO) 3 : HF=3:1:1, liquid-solid ratio 1:2, leaching temperature 70 ℃ and leaching time 24h, after the acid leaching is finished, flushing quartz concentrate into a quartz beaker by using ultrapure water, washing for a plurality of times to neutrality, drying, measuring 13 impurities by using ICP-MS, and obtaining high-purity quartz concentrate SiO after subtraction 2 The content is 99.98%.
TABLE 2 analysis results of high purity quartz concentrate
Element(s) | SiO 2 (%) | Fe | Mn | Cr | Ni | Cu | Mg |
Content mu g/g | 99.98 | 3.82 | 0.42 | 0.03 | 0.11 | 0.03 | 0.33 |
Element(s) | Ca | Al | Na | Li | K | Co | Ti |
Content mu g/g | 16.11 | 140.01 | 9.14 | 9.83 | 8.56 | 0.03 | 7.92 |
TABLE 3 analysis results of feldspar concentrates (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O |
Alkaline feldspar concentrate | 76.12 | 13.14 | 0.162 | 0.023 | 3.73 | 4.09 |
Acid feldspar concentrate | 68.82 | 16.81 | 0.184 | 0.021 | 4.83 | 4.93 |
TABLE 4 analysis results of building Material and glass batch products (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
+0.425mm grit | 78.65 | 10.03 | 1.799 | 0.024 | 3.48 | 2.25 | 0.828 | 0.253 |
Magnetic sand selection | 81.44 | 10.29 | 0.129 | 0.021 | 2.81 | 3.02 | 1.15 | 0.244 |
-0.074mm fine sand | 74.32 | 13.08 | 0.908 | 0.035 | 3.13 | 3.05 | 1.02 | 0.21 |
Examples
The ingredients of Jiangxi Yichun lepidolite mill tailings are shown in Table 5
TABLE 5 Multi-element analysis results of tailings (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
Content of | 79.86 | 11.83 | 0.081 | 0.007 | 2.69 | 4.35 | 0.51 | 0.03 |
Referring to FIG. 5, the tailings mainly comprise 40.61% of quartz mineral, 50.14% of feldspar mineral, 9.24% of mica mineral, 90.75% of quartz and feldspar mineral, 34.55% of tailings fineness of-0.074 mm and 65.16% of tailings fineness of-0.425+0.074 mm.
Key equipment: a sieving machine, a standard sleeve sieve, a wet type strong magnetic separator, an XFD12 flotation machine, an electrothermal oven and a high-pressure reaction kettle.
The test flow is as in FIG. 1, and tailings are subjected to screening classification to obtain +0.425mm material, -0.425+0.074mm material and-0.074 mm material. Carrying out two-stage strong magnetic separation on a material with the thickness of-0.425+0.074mm to remove mica and iron, wherein the magnetic field strength of the first stage is 1.2T, and the magnetic field strength of the second stage is 1.6T, so as to obtain magnetic sand and nonmagnetic substances; magnetic sand selection and +0.425mm material are mixed to be used as building materials, and-0.074 mm material is used as glass ingredients.
And (3) weighing a certain amount of non-magnetic matters, adding the non-magnetic matters into a 0.5L flotation tank of an XFD12 type flotation machine, wherein the concentration of flotation ore pulp is 30%, adding NaOH to adjust the pH of the ore pulp to be 10-11, stirring for 2 minutes, adding 300g/t of novel Dan Yingyang ion collector, stirring for 1200r/min, stirring for 3 minutes, performing aerated flotation for 5 minutes, wherein a foam product is quartz rough concentrate, and a product in the tank is alkaline feldspar concentrate.
Feeding the quartz rough concentrate into a 0.5L flotation tank for reverse flotation of feldspar, wherein the concentration of flotation ore pulp is 20%, and adding H 2 SO 4 Regulating the pH value of ore pulp to 2-3, stirring for 2 minutes, adding 200g/t of novel feldspar anion-cation mixed collector, 60g/t of foaming agent, stirring at a speed of 1200r/min, stirring for 3 minutes, and floating for 3 minutes, wherein the foam product is acid feldspar concentrate, and the product in the tank is quartz concentrate. In order to ensure the grade of the flotation quartz concentrate, the step is performed for two more times, so that impurities such as feldspar and the like can be removed more thoroughly, and the tertiary feldspar concentrate is mixed to be used as the final acidic feldspar concentrate.
Washing the flotation quartz concentrate with ultrapure water for multiple times, drying, weighing 10 g of sample, and placing the sample into a high-pressure reaction kettle for heating and acid leaching test, wherein the mixed acid is HCl: HNO (HNO) 3 : HF=3:1:1, liquid-solid ratio 1:2, leaching temperature 80 ℃, leaching time 24h, flushing quartz concentrate into a quartz beaker with ultrapure water after the acid leaching is finished, washing for a plurality of times to neutrality, drying, measuring 13 impurities by ICP-MS, and obtaining high-purity quartz concentrate SiO after subtraction 2 The content is 99.95 percent.
TABLE 6 analysis results of high purity quartz concentrate
Element(s) | SiO 2 (%) | Fe | Mn | Cr | Ni | Cu | Mg |
Content mu g/g | 99.95 | 11.64 | 0.17 | - | 0.13 | 0.18 | 1.9 |
Element(s) | Ca | Al | Na | B | K | Ba | Ti |
Content mu g/g | - | 383.21 | 55.46 | 1.62 | 34.80 | 0.01 | 5.25 |
TABLE 7 analysis results of feldspar concentrates (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
Alkaline feldspar concentrate | 71.38 | 16.16 | 0.056 | 0.004 | 4.18 | 5.22 | 0.60 | 0.046 |
Acid feldspar concentrate | 70.68 | 14.57 | 0.13 | 0.006 | 4.20 | 5.49 | 0.62 | 0.026 |
TABLE 8 analysis results of building materials and glass batch products (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
+0.425mm grit | 76.00 | 12.85 | 2.00 | 0.02 | 4.48 | 2.278 | 0.47 | 0.053 |
Magnetic sand selection | 78.34 | 11.91 | 0.71 | 0.048 | 3.052 | 3.859 | 0.84 | 0.127 |
-0.074mm fine sand | 77.26 | 12.86 | 0.071 | 0.009 | 2.457 | 5.015 | 0.64 | 0.033 |
Examples
The composition of lepidolite mill tailings in Ganzhou is shown in table 9.
TABLE 9 Multi-element analysis results of tailings (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
Content of | 80.54 | 11.36 | 0.18 | 0.034 | 4.00 | 3.28 | 0.34 | 0.046 |
Referring to FIG. 5, the tailings mainly comprise 46.61% of quartz mineral, 46.5% of feldspar mineral, 6.89% of mica mineral, 93.11% of the sum of quartz and feldspar mineral, 30.74% of tailings fineness of-0.074 mm and 69.16% of tailings fineness of-0.425+0.074 mm.
Key equipment: a sieving machine, a standard sleeve sieve, a wet type strong magnetic separator, an XFD12 flotation machine, an electrothermal oven and a high-pressure reaction kettle.
The test flow is as in FIG. 1, and tailings are subjected to screening classification to obtain +0.425mm material, -0.425+0.074mm material and-0.074 mm material. Carrying out two-stage strong magnetic separation on a material with the thickness of-0.425+0.074mm to remove mica and iron, wherein the magnetic field strength of the first stage is 1.2T, and the magnetic field strength of the second stage is 1.6T, so as to obtain magnetic sand and nonmagnetic substances; magnetic sand selection and +0.425mm material are mixed to be used as building materials, and-0.074 mm material is used as glass ingredients.
And (3) weighing a certain amount of non-magnetic matters, adding the non-magnetic matters into a 0.5L flotation tank of an XFD12 type flotation machine, wherein the concentration of flotation ore pulp is 30%, adding NaOH to adjust the pH of the ore pulp to be 10-11, stirring for 2 minutes, adding 400g/t of novel Dan Yingyang ion collector, stirring for 1200r/min, stirring for 3 minutes, performing aerated flotation for 5 minutes, wherein a foam product is quartz rough concentrate, and a product in the tank is alkaline feldspar concentrate.
Feeding the quartz rough concentrate into a 0.5L flotation tank for reverse flotation of feldspar, wherein the concentration of flotation ore pulp is 20%, and adding H 2 SO 4 Regulating the pH value of the ore pulp to 2-3, stirring for 2 minutes, and adding novel feldspar yin and yang250g/t of ion mixed collector, 60g/t of foaming agent, stirring speed of 1200r/min, stirring for 3 minutes and flotation time of 3 minutes, wherein the foam product is acid feldspar concentrate, and the product in the tank is quartz concentrate. In order to ensure the grade of the flotation quartz concentrate, the scavenging is carried out twice according to the step, so that impurities such as feldspar and the like can be removed more thoroughly, and the three times of scavenging feldspar foam are mixed to be used as the final acidic feldspar concentrate.
Washing the flotation quartz concentrate with ultrapure water for multiple times, drying, weighing 10 g of sample, and placing the sample into a high-pressure reaction kettle for heating and acid leaching test, wherein the mixed acid is HCl: HNO (HNO) 3 : HF=3:1:1, liquid-solid ratio 1:2, leaching temperature 80 ℃, leaching time 24h, flushing quartz concentrate into a quartz beaker with ultrapure water after the acid leaching is finished, washing for a plurality of times to neutral, drying, measuring 13 impurities by ICP-MS, and obtaining high-purity quartz concentrate SiO after subtraction 2 The content is 99.97%.
Table 10 analysis results of high purity quartz concentrate
Element(s) | SiO 2 (%) | Fe | Mn | Cr | Ni | Cu | Mg |
Content mu g/g | 99.96 | 10.43 | 0.32 | - | 0.05 | 0.11 | - |
Element(s) | Ca | Al | Na | B | K | Ba | Ti |
Content mu g/g | - | 302.23 | 4.88 | 0.49 | 27.54 | 0.01 | 21.8 |
TABLE 11 analysis results of feldspar concentrates (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
Alkaline feldspar concentrate | 73.94 | 15.17 | 0.11 | 0.017 | 5.56 | 4.81 | 0.33 | 0.049 |
Acid feldspar concentrate | 72.40 | 15.23 | 0.17 | 0.025 | 6.04 | 5.18 | 0.49 | 0.061 |
TABLE 12 analysis results of building materials and glass batch products (%)
Composition of the components | SiO 2 | Al 2 O 3 | Fe 2 O 3 | TiO 2 | K 2 O | Na 2 O | CaO | MgO |
+0.425mm grit | 77.55 | 12.44 | 0.877 | 0.094 | 4.38 | 2.04 | 0.15 | 0.16 |
Magnetic sand selection | 76.08 | 12.56 | 2.53 | 0.278 | 3.95 | 3.06 | 0.65 | 0.479 |
-0.074mm fine sand | 77.04 | 12.63 | 0.22 | 0.054 | 4.08 | 4.47 | 0.39 | 0.044 |
Quartz and feldspar are separated by the conventional reagent, namely dodecyl amine, and the obtained flotation quartz concentrate is compared with the flotation quartz concentrate obtained by the novel reagent in the method under a microscope, as shown in figures 2-4:
yellow and black impurities are visible to naked eyes and under a microscope, and the impurities are poor in selectivity, and although feldspar is reversely floated for multiple times, the impurities are not thoroughly separated, the selectivity of a new reagent is strong, quartz and feldspar can be better separated in a short process, so that high-grade flotation concentrate is obtained, and the low-iron high-purity quartz concentrate is produced for next hot-pressure acid leaching to serve as a bedding, so that the economic benefit of the quartz and the feldspar is increased.
The low-iron high-purity quartz concentrate, feldspar concentrate, building material and glass batching products obtained by the implementation have respective purposes, really realize tail-free production of mines, accord with the green development concept, have wide application range and have wide application market and application prospect.
The foregoing description is only illustrative of the preferred embodiment of the present invention, and is not to be construed as limiting the invention, but is to be construed as limiting the invention to any and all simple modifications, equivalent variations and adaptations of the embodiments described above, which are within the scope of the invention, may be made by those skilled in the art without departing from the scope of the invention.
Claims (9)
1. A method for extracting quartz and feldspar from granite pegmatite tailings, which is characterized by comprising the following steps:
step (1) screening and classifying: taking granite peganite tailings as an input raw ore, and screening and grading to obtain a +0.425mm material, -0.425+0.074mm material and-0.074 mm material;
and (2) carrying out strong magnetic separation: carrying out two-stage strong magnetic separation tests on the materials with the diameters of between (1) and (0.425+0.074 mm) to obtain magnetic sand and nonmagnetic substances;
and (3) quartz forward flotation: regulating the pH value of the ore pulp of the non-magnetic matters in the step (2) to 10-11 by using alkali, and then adding a quartz cation collector DS-01 to perform a quartz forward flotation test to obtain quartz rough concentrate and alkaline feldspar concentrate; meanwhile, combining the materials of 0.425mm and the magnetic separation sand of 0.425mm in the step (1) and the step (2) to be used as building materials;
and (4) reverse flotation and roughing of feldspar: adjusting the pH value of ore pulp to 2-3 by using acid in the quartz coarse concentrate in the step (3), then adding a feldspar anion-cation collector XK-02 and a foaming agent KW-03, and performing a reverse flotation coarse flotation feldspar test to obtain quartz coarse concentrate and feldspar concentrate 1;
and (5) reverse flotation and scavenging 1: adding acid into the quartz rough concentrate obtained in the step (4) to adjust the pH value of the ore pulp to 2-3, then adding feldspar anion-cation collector XK-02 and foaming agent KW-03, and performing a reverse flotation scavenging 1 test to obtain quartz rough concentrate and feldspar concentrate 2;
and (6) reverse flotation and scavenging 2: adding acid into the quartz rough concentrate in the step (5) to adjust the pH value of the ore pulp to 2-3, then adding feldspar anion-cation collector XK-02 and foaming agent KW-03, and performing a reverse flotation scavenging 2 test to obtain flotation quartz concentrate and feldspar concentrate 3;
and (7) hot-pressing acid leaching: combining the feldspar concentrate 1 in the step (4), the feldspar concentrate 2 in the step (5) and the feldspar concentrate 3 in the step (6) to be used as acid feldspar concentrate; carrying out hot-pressing acid leaching, washing and drying on the flotation quartz concentrate in the step (6) to obtain quartz concentrate;
wherein Dan Yingzheng flotation collector DS-01 is a polymer of alkaline earth metal cations and alkyl sulfonate; the feldspar negative and positive ion collector XK-02 is a mixture of compound amine, fatty acid and silicate inhibitor; the foaming agent KW-03 is a mixture of hydrocarbon oil and pine oil.
2. The method for extracting quartz and feldspar from granite pegmatite tailings according to claim 1, wherein in the step (1), the screening equipment is a standard screen for laboratory, and the standard screen meets the requirement of quartz granularity of 0.425mm and 0.074mm.
3. The method for extracting quartz and feldspar from granite pegmatite tailings according to claim 1, wherein in the step (2), the high-intensity magnetic separation is high-gradient magnetic separation, the magnetic separation operation comprises first-stage magnetic separation and second-stage magnetic separation, and non-magnetic matters subjected to the first-stage magnetic separation enter the second-stage magnetic separation, and the magnetic field strength is 0.8-1.8T.
4. The method for extracting quartz and feldspar from granite pegmatite tailings of mineral separation according to claim 1, wherein in the step (3), dan Yingzheng flotation is aerated flotation, and the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding alkali to adjust the pH of ore pulp to 10-11, wherein the alkali is one or a mixture of sodium hydroxide and sodium carbonate, the concentration of quartz positive flotation ore pulp is 20-35%, the dosage of Dan Yingyang ion collector is 300-800 g/t, the stirring speed is 800-1200 r/min, and the flotation time is 2-5 min.
5. The method for extracting quartz and feldspar from granite pegmatite tailings of mineral separation according to claim 1, wherein in the step (4), the reverse flotation and roughing of the feldspar are aerated flotation, and the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: and adding acid to adjust the pH of the ore pulp to 2-3, wherein the acid is one or a mixture of sulfuric acid, oxalic acid, nitric acid and hydrochloric acid, the concentration of quartz rough concentrate reverse flotation feldspar ore pulp is 15-30%, the consumption of feldspar anion-cation mixed collector is 400-600 g/t, the consumption of foaming agent is 50-100 g/t, the stirring rate is 800-1200 r/min, and the flotation time is 2-5 min.
6. The method for extracting quartz and feldspar from granite pegmatite tailings of mineral separation according to claim 1, wherein in the step (5), the reverse flotation and scavenging 1 is aerated flotation, the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding a small amount of acid to adjust the pH of ore pulp to 2-3, wherein the acid is one or a mixture of sulfuric acid, oxalic acid, nitric acid and hydrochloric acid, the concentration of the ore pulp in reverse flotation scavenging 1 is 15-25%, the consumption of feldspar anion-cation mixed collector is 100-300 g/t, the consumption of foaming agent is 30-50g/t, the stirring rate is 800-1200 r/min, and the flotation time is 2-3 min.
7. The method for extracting quartz and feldspar from granite pegmatite tailings of mineral separation according to claim 1, wherein in the step (6), the reverse flotation and scavenging 2 is aerated flotation, the flotation machine is an XFD12 type multi-tank, and the process conditions are as follows: adding a small amount of acid to adjust the pH of ore pulp to 2-3, wherein the acid is one or a mixture of sulfuric acid, oxalic acid, nitric acid and hydrochloric acid, the concentration of the reverse flotation 2 ore pulp is 10-25%, the consumption of the feldspar anion-cation mixed collector is 60-150 g/t, the consumption of the foaming agent is 20-40 g/t, the stirring rate is 800-1200 r/min, and the flotation time is 1-2 min.
8. The method for extracting quartz and feldspar from granite pegmatite tailings of mineral separation according to claim 1, wherein in the step (7), the acid leaching process is as follows: at least one of ultrasonic acid leaching, stirring acid leaching and heating acid leaching, wherein the acid is mixed acid, and the mixed acid is two or more of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid and oxalic acid, and the leaching time is 4-24 h.
9. The method for extracting quartz and feldspar from granite pegmatite tailings of mineral separation as claimed in claim 1, wherein the step (7) is carried out by pickling the quartz concentrate to obtain SiO 2 ≥99.95%、Fe≤10μg/g。
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