NL2025809B1 - Fluorine-free extraction method for insoluble potassium ore - Google Patents
Fluorine-free extraction method for insoluble potassium ore Download PDFInfo
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- NL2025809B1 NL2025809B1 NL2025809A NL2025809A NL2025809B1 NL 2025809 B1 NL2025809 B1 NL 2025809B1 NL 2025809 A NL2025809 A NL 2025809A NL 2025809 A NL2025809 A NL 2025809A NL 2025809 B1 NL2025809 B1 NL 2025809B1
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- Prior art keywords
- ore slurry
- ore
- concentrate
- potassium feldspar
- coarse
- Prior art date
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- 238000000605 extraction Methods 0.000 title claims abstract description 25
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 21
- 239000011591 potassium Substances 0.000 title claims abstract description 21
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims abstract description 111
- 239000012141 concentrate Substances 0.000 claims abstract description 108
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000010445 mica Substances 0.000 claims abstract description 45
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 45
- 238000005188 flotation Methods 0.000 claims abstract description 39
- 239000010453 quartz Substances 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000002378 acidificating effect Effects 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 22
- 239000011707 mineral Substances 0.000 claims abstract description 22
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims abstract description 16
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims abstract description 16
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims abstract description 16
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims abstract description 12
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims description 203
- 239000002245 particle Substances 0.000 claims description 87
- 238000007885 magnetic separation Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003350 kerosene Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 7
- 238000010298 pulverizing process Methods 0.000 claims 6
- 238000003801 milling Methods 0.000 claims 2
- 238000007873 sieving Methods 0.000 claims 2
- 239000000725 suspension Substances 0.000 claims 2
- 238000000227 grinding Methods 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N hydrofluoric acid Substances F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 abstract 1
- 239000006260 foam Substances 0.000 description 18
- 239000010433 feldspar Substances 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 238000005273 aeration Methods 0.000 description 7
- -1 occurs in granite Chemical compound 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000011435 rock Substances 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 239000006148 magnetic separator Substances 0.000 description 4
- 229940049964 oleate Drugs 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 229910052570 clay Inorganic materials 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 229910052586 apatite Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 229940005740 hexametaphosphate Drugs 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052627 muscovite Inorganic materials 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 2
- 229910052655 plagioclase feldspar Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052626 biotite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000010438 granite Substances 0.000 description 1
- 229910052900 illite Inorganic materials 0.000 description 1
- 229910001608 iron mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052651 microcline Inorganic materials 0.000 description 1
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- 229910052652 orthoclase Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010435 syenite Substances 0.000 description 1
Classifications
-
- 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
- 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
- B03D1/02—Froth-flotation processes
- B03D1/025—Froth-flotation processes adapted for the flotation of fines
-
- 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
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/42—Micas ; Interstratified clay-mica products
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a fluorine—free extraction method for an insoluble potassium ore, and relates to the technical field of ore extraction. The extraction method includes a crushing process, a grinding process, a magnetic 5 separation process and a flotation process of a potassium feldspar ore. The present invention uses sodium hexametaphosphate and a sodium oleate/dodecylamine collector to float potassium feldspar under fluorine—free and weakly acidic conditions provided by a sulfuric acid. The present 10 invention increases the surface hydrophobicity of the potassium feldspar, so that the potassium feldspar is floated up and.selectedd Comparedxvith.hydrofluoric acid, the sulfuric acid is weaker in acidity and lower in corrosion and cost. Therefore, the extraction method provided by the present 15 invention reduces the corrosion<xfthe eguipment.andtflxeimpact onthehumanbodyandtheenvironmentandreducestheproduction cost. In addition, the extraction method realizes the extraction of high—quality potassium feldspar concentrate, mica concentrate and quartz concentrate and achieves the 20 comprehensive utilization of the mineral resources.
Description
TECHNICAL FIELD The present invention relates to the technical field of ore extraction, and in particular, to a fluorine-free extraction method for an insoluble potassium ore.
BACKGROUND Non-water-soluble (NWS) potassium-bearing rocks include feldspar clastic rocks {(potassium-containing sandstone, shale, glauconitic sandstone and illite clay rocks), hydromica clay rocks (mungite) and potassium feldspar ores, which have different potassium contents. Potassium feldspar mainly occurs in granite, granodiorite, monzonite, syenite, pegmatite and other rocks. China's rich potassium feldspar resources are used in the production of ceramic blanks, ceramic glazes, glass, electric porcelain, abrasive materials and potassium fertilizer, among which the glass and ceramic industries account for 80-90% of the total consumption of potassium feldspar. The production of China's glass and ceramic industries must be safeguarded to promote the healthy development of the national economy. To realize this purpose, it is necessary to strengthen the research of the beneficiation and purification techniques of potassium feldspar, rationally develop and utilize low- and medium-grade potassium feldspar ores, and realize the sustainable development of the potassium feldspar resources. The harmful impurities that affect the selection of potassium feldspar include clay, quartz, mica, apatite, zircon and iron minerals. Quartz is similar to potassium feldspar in physical properties, chemical composition and structure, and mainly distributed in the fractures of fractured potassium feldspar. Some quartz is filled with plagioclase and muscovite in the form of aggregates in the fractures of fractured potassium feldspar, and some embedded in the crystals of potassium feldspar. Therefore, it is difficult to separate potassium feldspar from quartz. At present, potassium feldspar is mainly beneficiated by desliming and iron removal. Among the quartz-potassium feldspar flotation separation processes, the most mature one is to use hydrofluoric acidto float feldspar under the pH of 2. In this process, the strongly acidic medium causes severe corrosion of the equipment, and the fluorine has a significant adverse impact on the human body and the environment.
SUMMARY In view of this, an objective of the present invention is to provide a fluorine-free extraction method for an insoluble potassium ore. The present invention floats potassium feldspar under fluorine-free and weakly acidic conditions, which achieves the comprehensive utilization of the mineral resources while reducing the corrosion of equipment and the impact on the human body and the environment, and reducing production costs.
To achieve the above purpose, the present invention provides the following technical solutions.
The present invention provides a fluorine-free extraction method for an insoluble potassium ore, including the following Steps: (1) providing potassium feldspar ore particles with a particle size of less than 1 mm; (2) slurrying the potassium feldspar ore particle with a particle size of less than 1 mm to obtain an ore slurry with a mass concentration of 60-65%; then grinding the ore slurry till ore particles with a particle size of less than 0.074 mm account for 65-70% total mass of ore particles, and adjusting the mass concentration of the ore slurry after grinding to
35-40%; (3) performing a wet strong magnetic separation on the ore slurry with a mass concentration of 35-40% to separate an iron-bearing mineral from a first intermediate ore slurry; (4) adding a sulfuric acid to the first intermediate ore slurry to adjust the pH to 5.0-5.5 to obtain a first weakly acidic ore slurry; mixing the first weakly acidic ore slurry with a first collector and a No. 2 oil in sequence, and then aerating for a first flotation to separate a coarse mica concentrate from a second intermediate ore slurry, where the first collector is kerosene;
(5) slurrying the coarse mica concentrate to obtain a coarse mica concentrate slurry; aerating the coarse mica concentrate slurry for a second flotation to separate a mica concentrate from a third intermediate ore slurry; returning to step (4) to mix the third intermediate ore slurry with the first intermediate ore slurry;
{6) adding the sulfuric acid to the second intermediate ore slurry to adjust the pH to 4.0-5.0 to obtain a second weakly acidic ore slurry; mixing the second weakly acidic ore slurry with sodium hexametaphosphate and a second collector in sequence, and then aerating for a third flotation to separate out a coarse potassium feldspar concentrate; filtering the remaining ore slurry, and then drying a residue to obtain a quartz concentrate, where the second collector is a mixture of sodium oleate and dodecylamine; and
(7) slurrying the coarse potassium feldspar concentrate to obtain a coarse potassium feldspar concentrate slurry; aerating the coarse potassium feldspar concentrate slurry for a fourth flotation to separate a potassium feldspar concentrate from a fourth intermediate ore slurry; returning to step (6)
to mix the fourth intermediate ore slurry with the second intermediate ore slurry. Preferably, the method for providing potassium feldspar ore particles with a particle size of less than 1 mm in step (1) is preferably: subjecting a potassium feldspar ore to coarse crushing, medium crushing, fine crushing and screening in sequence to obtain ore particles with a particle size of less than 1 mm. Preferably, the particle size of coarse ore particles obtained by the coarse crushing is less than 15 mm; the particle size of medium ore particles obtained by the medium crushing is less than 6 mm; the particle size of fine ore particles obtained by the fine crushing is less than 2 mm; the coarse crushing is performed by a coarse crushing jaw crusher, the medium crushing is performed by a medium crushing jaw crusher, and the fine crushing is performed by a roll crusher; the pore size of a sieve used for the screening is 1 mm.
Preferably, in step (3), the magnetic field strength of the wet strong magnetic separation is 11000-12000 Oe.
Preferably, in step (4), 350-450 g of sulfuric acid with a mass concentration of 3-5% is added per ton of first intermediate ore slurry; 130-150 g of first collector is added per ton of first intermediate ore slurry; 10-20 g of No. 2 oil is added per ton of first intermediate ore slurry.
Preferably, in step (6), 500-800 g of sulfuric acid with a mass concentration of 3-5% is added per ton of second intermediate ore slurry.
Preferably, in step (6), 200-250 gq of sodium hexametaphosphate is added per ton of second intermediate ore slurry.
Preferably, in step (6), 100-150 g of second collector is added per ton of second intermediate ore slurry, and the mass ratio of the sodium oleate to the dodecylamine is 1:4.
Preferably, before filtering, step (6) further includes continuing to mix the remaining ore slurry with the second collector, and aerating to separate out a coarse potassium feldspar concentrate.
5 Preferably, 50-70 g of second collector is added per ton of remaining ore slurry.
The present invention provides a fluorine-free extraction method for an insoluble potassium ore, including a crushing process, a grinding process, a magnetic separation process and a flotation process of the potassium feldspar ore. The present invention uses sodium hexametaphosphate and a sodium oleate/dodecylamine collector to float a potassium feldspar under fluorine-free and weakly acidic conditions provided by a sulfuric acid. Under the weakly acidic conditions, the surface of the potassium feldspar is negatively charged and the surface of quartz is not charged. A dodecylamine cation of the collector is first adsorbed on a negatively charged region on the surface of the potassium feldspar. An oleate anion and an adsorbed amine of the collector are complexed and co—adsorbed on the surface of the feldspar. A hexametaphosphate ion produced by the hydrolysis of the sodium hexametaphosphate added to an ore slurry desorbs the oleate with a low adsorption strength on the surface of the quartz, and prevents the adsorption of the dodecylamine cation. In this way, the method inhibits the quartz and increases the surface hydrophobicity of the potassium feldspar, so that the potassium feldspar is floated up and selected. The present invention creates the fluorine-free and weakly acidic conditions with the sulfuric acid to float the potassium feldspar. Compared with hydrofluoric acid, the sulfuric acid is weaker in acidity and lower in corrosion and cost. Therefore, the extraction method provided by the present invention reduces the corrosion of the equipment and the impact on the human body and the environment,
and reduces the production cost. In addition, the extraction method realizes the extraction of high-quality potassium feldspar concentrate and achieves the comprehensive utilization of the mineral resources.
The results of the examples show that the yield of the potassium feldspar concentrate extracted by the method of the present invention reaches 65-68%, and the potassium feldspar concentrate includes 11-13% of K;0 and 3-4% of Na20.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a flowchart of a fluorine-free extraction method for an insoluble potassium ore according to the present invention.
DETAILED DESCRIPTION The present invention provides a fluorine-free extraction method for an insoluble potassium ore, including the following Steps: (1) Provide potassium feldspar ore particles with a particle size of less than 1 mm. (2) Slurry the potassium feldspar ore particle with a particle size of less than 1 mm to obtain an ore slurry with a mass concentration of 60-65%; then grind the ore slurry till ore particles with a particle size of less than 0.074 mm account for 65-70% total mass of ore particles, and adjust the mass concentration of the ore slurry after grinding to 35-40%. (3) Perform a wet strong magnetic separation on the ore slurry with a mass concentration of 35-40% to separate an iron-bearing mineral from a first intermediate ore slurry. {4) Add a sulfuric acid to the first intermediate ore slurry to adjust the pH to 5.0-5.5 to obtain a first weakly acidic ore slurry; mix the first weakly acidic ore slurry with a first collector and a No. 2 oil in sequence, and then aerate for a first flotation to separate a coarse mica concentrate from a second intermediate ore slurry, where the first collector is kerosene.
(5) Slurry the coarse mica concentrate to obtain a coarse mica concentrate slurry; aerate the coarse mica concentrate slurry for a second flotation to separate a mica concentrate from a third intermediate ore slurry; return to step (4) to mix the third intermediate ore slurry with the first intermediate ore slurry.
{6) Add the sulfuric acid to the second intermediate ore slurry to adjust the pH to 4.0-5.0 to obtain a second weakly acidic ore slurry; mix the second weakly acidic ore slurry with sodium hexametaphosphate and a second collector in sequence, and then aerate for a third flotation to separate out a coarse potassium feldspar concentrate; filter the remaining ore slurry, and then dry a residue to obtain a quartz concentrate, where the second collector is a mixture of sodium oleate and dodecylamine.
(7) Slurry the coarse potassium feldspar concentrate to obtain a coarse potassium feldspar concentrate slurry; aerate the coarse potassium feldspar concentrate slurry for a fourth flotation to separate a potassium feldspar concentrate from a fourth intermediate ore slurry; return to step (6) to mix the fourth intermediate ore slurry with the second intermediate ore slurry.
The present invention provides potassium feldspar ore particles with a particle size of less than 1 mm. In the present invention, the method for providing potassium feldspar ore particles with a particle size of less than 1 mm is preferably to subject a potassium feldspar ore to coarse crushing, medium crushing, fine crushing and screening in sequence to obtain ore particles with a particle size of less than 1 mm. In the present invention, the particle size of coarse ore particles obtained by the coarse crushing is less than 15 mm; the particle size of medium ore particles obtained by the medium crushing is less than 6 mm; the particle size of fine ore particles obtained by the fine crushing is less than 2 mm.
The coarse crushing is performed by a coarse crushing jaw crusher, the medium crushing is performed by a medium crushing jaw crusher, and the fine crushing is performed by a roll crusher.
The pore size of a sieve used for the screening is 1 mm.
After the screening ends, ore particles with a particle size of greater than 1 mm are returned to the roll crusher for further crushing.
The present invention has no special requirement for the coarse crushing jaw crusher, the medium crushing jaw crusher and the roll crusher, and a crusher well known to those skilled in the art can be used.
In a specific example of the present invention, the model of the coarse crushing jaw crusher is RK400*300, and the model of the medium crushing jaw crusher is RK330*%200. After the potassium feldspar ore particle with a particle size of less than 1 mm is obtained, the present invention slurries the potassium feldspar particle to obtain an ore slurry with a mass concentration of 60-65%. Then the present invention grinds the ore slurry till ore particles with a particle size of less than 0.074 mm account for 65-70% total mass of ore particles, and adjusts the mass concentration of the ore slurry after grinding to 35-40%. The present invention has no special requirement for the ore slurrying method, and a slurrying method well known to those skilled in the art can be used.
In the present invention, the grinding is performed by a bar grinder.
The present invention has no special requirement for the bar grinder, and a bar grinder well known to those skilled in the art can be used.
After the grinding, the ore particle with a particle size of less than 0.074 mm in the ground ore slurry preferably accounts for 66-68% total mass of ore particles.
After the grinding, the present invention adjusts the mass concentration of the ore slurry to 35-40%, which is appropriate for a subsequent separation by a magnetic separator. After the ore slurry with a mass concentration of 35-40% is obtained, the present invention performs a wet strong magnetic separation on the ore slurry with a mass concentration of 35-40% to separate an iron-bearing mineral from a first intermediate ore slurry. In the present invention, the magnetic field strength of the wet strong magnetic separation is preferably 11000-12000 Oe, and more preferably 11500 Oe. In the present invention, the wet magnetic separation is preferably performed in a strong magnetic separator. In a specific example of the present invention, the model of the strong magnetic separator is RK/XCSQ-50*70.
After the first intermediate ore slurry is separated, the present invention adds a sulfuric acid to the first intermediate ore slurry to adjust the pH to 5.0-5.5 to obtain a first weakly acidic ore slurry. The present invention mixes the first weakly acidic ore slurry with a first collector and a No. 2 oil in sequence, and then aerates for a first flotation to separate a coarse mica concentrate from a second intermediate ore slurry. The first collector is kerosene. In the present invention, the first flotation is preferably performed in a flotation machine. In the present invention, preferably 350-450 g, more preferably 380-400 g of sulfuric acid with a mass concentration of preferably 3-5% is added per ton of first intermediate ore slurry. In the present invention, the pH of the first weakly acidic ore slurry is 5.0, 5.1, 5.2,
5.3, 5.4 and 5.5. After the sulfuric acid is added, the present invention preferably stirs the obtained first weakly acidic ore slurry for 3-5 min before adding the first collector. In the present invention, preferably 130-150 g, more preferably 135-145 g of first collector is added per ton of first intermediate ore slurry. After the collector is added, the present invention preferably stirs the ore slurry with the collector added for 3-5 min, then adds a No. 2 oil, continues to stir for 1-2 min, and aerates the ore slurry (with air). In this way, the first collector fully reacts with the mineral particles in the ore slurry to expand the difference in floatability between the mineral particles. In the present invention, the No. 2 oil is terpenic oil, which serves as a foaming agent, and the aeration rate is preferably 160-200 M3 per liter of first intermediate ore slurry. In the present invention, under the weakly acidic conditions with the pH of
5.0-5.5, kerosene easily forms a hydrophobic layer on the surface of a mica mineral. A hydrophobic mica particle floats with a bubble to the surface of the ore slurry to form a foam layer, and the foam layer is scraped off by a scraper to obtain the coarse mica concentrate. Other particles that cannot float, including potassium feldspar, quartz and other impurity minerals, are left in the ore slurry to form the second intermediate ore slurry.
After the coarse mica concentrate is obtained, the present invention slurries the coarse mica concentrate to obtain a coarse mica concentrate slurry, and then aerates the coarse mica concentrate slurry for a second flotation to separate a mica concentrate from a third intermediate ore slurry. In the present invention, the mass concentration of the coarse mica concentrate slurry is preferably 28-33%. In the present invention, during the second flotation, no collector is added, and the aeration rate is preferably 160-200 M® per liter of coarse mica concentrate slurry. In the present invention, due to the good floatability, the mica particle floats with the bubble to the surface of the ore slurry to form a foam layer, and the foam layer is scraped off by a scraper. The foam layer is preferably filtered and dried in sequence to obtain a mica concentrate. Other minerals that cannot float up are left in the ore slurry to form the third intermediate ore slurry. The third intermediate ore slurry is mixed with the first intermediate ore slurry in the step of the flotation of the coarse mica concentrate in the above solution.
After the second intermediate ore slurry is obtained, the present invention adds the sulfuric acid to the second intermediate ore slurry to adjust the pH to 4.0-5.0 to obtain a second weakly acidic ore slurry. The present invention mixes the second weakly acidic ore slurry with sodium hexametaphosphate and a second collector in sequence, and then aerates for a third flotation to separate a coarse potassium feldspar concentrate. The present invention filters the remaining ore slurry, and then dries a residue to obtain a quartz concentrate. The second collector is a mixture of sodium oleate and dodecylamine. In the present invention, preferably 500-800 g, and more preferably 600-700 g of sulfuric acid with a mass concentration of preferably 3-5% is added per ton of second intermediate ore slurry. In the present invention, the pH of the second weakly acidic ore slurry is specifically 4.0, 4.5 and 5.0. After the sulfuric acid is added, the present invention preferably stirs the second weakly acidic ore slurry for 3-5 min before adding the sodium hexametaphosphate. In the present invention, preferably 200-250 g, more preferably 220-230 g of sodium hexametaphosphate is added per ton of second intermediate ore slurry. The present invention preferably stirs the ore slurry with the sodium hexametaphosphate added for 3-5 min before adding the second collector. In the present invention, preferably 100-150 g, more preferably 120 g of second collector is added per ton of second intermediate ore slurry. The mass ratio of the sodium oleate to the dodecylamine in the second collector is preferably 1:4. Under the weakly acidic conditions with the pH of 4.0-5.0, the surface of the potassium feldspar is negatively charged and the surface of quartz is not charged. A dodecylamine cation of the collector is first adsorbed on a negatively charged region on the surface of the potassium feldspar. An oleate anion and an adsorbed amine of the collector are complexed and co-adsorbed on the surface of feldspar. A hexametaphosphate ion produced by the hydrolysis of the sodium hexametaphosphate added to the ore slurry desorbs the oleate with a low adsorption strength on the surface of the quartz, and prevents the adsorption of the dodecylamine cation. In this way, the method inhibits the quartz and increases the surface hydrophobicity of the potassium feldspar, so that the potassium feldspar floats up with the bubble to the surface of the ore slurry to form a foam layer. The foam layer is scraped off by a scraper to separate out the coarse potassium feldspar concentrate (first coarse potassium feldspar concentrate).
Before the remaining ore slurry is filtered, the present invention preferably continues to mix the remaining ore slurry with the second collector for aeration. Preferably 50-70 g, more preferably 60 g of second collector is added per ton of remaining ore slurry. In the present invention, the remaining ore slurry is continuously mixed with the second collector for aeration, so that the coarse potassium feldspar concentrate (second coarse potassium feldspar concentrate) is separated out from the remaining ore slurry. Other minerals that cannot float up, mainly quartz, are left in the ore slurry, and filtered and dried in sequence to obtain a quartz concentrate. The present invention preferably combines the first coarse potassium feldspar concentrate and the second coarse potassium feldspar concentrate that are separated out.
After the coarse potassium feldspar concentrate is separated out, the present invention slurries the coarse potassium feldspar concentrate to obtain a coarse potassium feldspar concentrate slurry. The present invention aerates the coarse potassium feldspar concentrate slurry for a fourth flotation to separate a potassium feldspar concentrate from a fourth intermediate ore slurry. In the present invention, the mass concentration of the coarse potassium feldspar concentrate slurry is preferably 27-30%. In the present invention, during the fourth flotation, no collector is added, and the aeration rate is preferably 160-200 M3 per liter of coarse potassium feldspar concentrate slurry. In the present invention, the aeration is preferably performed while stirring at preferably 1850-2090 r/min. After the aeration, a potassium feldspar particle floats with a bubble to the surface of the ore slurry to form a foam layer, and the foam layer is scraped off by a scraper. The foam layer is preferably filtered and dried in sequence to obtain a potassium feldspar concentrate. Other minerals that cannot float up are left in the ore slurry to form the fourth intermediate ore slurry. The fourth intermediate ore slurry is mixed with the second intermediate ore slurry in the step of the flotation of the coarse potassium feldspar concentrate in the above solution.
The present invention floats the potassium feldspar under fluorine-free and weakly acidic conditions provided by the sulfuric acid. Compared with hydrofluoric acid, the sulfuric acid is weaker in acidity and lower in corrosion and cost.
Therefore, the extraction method provided by the present invention reduces the corrosion of the equipment and the impact on the human body and the environment and reduces the production cost. In addition, the extraction method realizes the extraction of high-quality potassium feldspar concentrate, mica concentrate and guartz concentrate and achieves the comprehensive utilization of the mineral resources.
The fluorine-free extraction method for an insoluble potassium ore provided by the present invention is described in detail below with reference to the examples, but the examples should not be construed as a limitation to the protection scope of the present invention.
Example 1 In this example, the raw potassium feldspar ore was mined from Qinghai, which included the minerals such as potassium feldspar (microcline feldspar, orthoclase and perthite), quartz, and a small amount of muscovite, biotite, apatite, zircon and metal minerals (such as ferrous materials). An analysis of the raw ore showed that the ore included 74.5wt.4 of potassium feldspar, 9.17wt.% of plagioclase, 9.75wt.% of quartz and 5.67wt.% of mica.
The raw potassium feldspar ore was extracted as follows: (1) First, the raw potassium feldspar ore was crushed with a coarse crushing jaw crusher (model: RK400*300) to a particle size of less than 15 mm.
Ore particles with a particle size of less than 15 mm was put into a medium crushing jaw crusher (model: RK330*200) to be crushed to a particle size of less than 6 mm.
Ore particles with a particle size of less than 6 mm was crushed with a roll crusher.
After the crushing, an ore particle was screened with a sieve with a diameter of 1 mm.
An ore particle with a diameter of more than 1 mm was returned to the roll crusher for further crushing.
The above operation was repeated till the particle size of all ore particles was less than 1 mm. (2) Ore particles with a particle size of less than 1 mm were slurried to obtain an ore slurry with a mass concentration of 65%. The ore slurry was ground till ore particles with a particle size of less than 0.074 mm in the ore slurry accounted for 68% total mass of ore particles.
Then the mass concentration of the ore slurry was adjusted to 38%. {3) The obtained ore slurry was subjected to a wet strong magnetic separation by a strong magnetic separator under the magnetic field strength of 11000 Oe to separate an iron-bearing mineral from a first intermediate ore slurry.
(4) The first intermediate ore slurry obtained by the magnetic separation was put into a flotation machine.
(4.1) Coarse flotation of mica: 350 g of sulfuric acid with a mass concentration of 5% was added per ton of first intermediate ore slurry. The pH of the ore slurry was adjusted to 5.5, and the ore slurry was stirred for 3 min. Then 130 g of kerosene collector was added per ton of first intermediate ore slurry, and the ore slurry was stirred for 3 min. Then 15 g of No. 2 oil (foaming agent) was added per ton of first intermediate ore slurry, and the ore slurry was stirred for 1 min. The ore slurry was aerated and a foam formed was scraped off by a scraper to yield a coarse mica concentrate. Other minerals that could not float up were left in the ore slurry to form a second intermediate ore slurry.
(4.2) Fine flotation of mica: The coarse mica concentrate was slurried and stirred for 3 min without adding a collector. Then the coarse mica concentrate was aerated, and a foam formed was scraped off by a scraper. The foam was filtered and dried to yield a fine mica concentrate. Other minerals that could not float up were left in the ore slurry to form a third intermediate ore slurry, which was mixed with the first intermediate ore slurry.
(4.3) Coarse flotation of potassium feldspar: 550 g of sulfuric acid with a mass concentration of 5% was added per ton of second intermediate ore slurry. The pH of the ore slurry was adjusted to 5.0, and the ore slurry was stirred for 3 min. 200 g of sodium hexametaphosphate was added per ton of second intermediate ore slurry, and the ore slurry was stirred for 33min. 120 g of collector composed of sodium oleate dodecylamine with amass ratio of 1:4 was added per ton of second intermediate ore slurry, and the ore slurry was aerated for a first-stage coarse flotation of potassium feldspar. A potassium feldspar particle floated with a bubble to the surface of the ore slurry to forma foam layer. The foam layer was scraped off by a scraper to yield a first coarse potassium feldspar concentrate. 60 g of collector composed of sodium oleate and dodecylamine with a mass ratio of 1:4 was added per ton of remaining ore slurry, and the ore slurry was stirred and aerated for a second-stage coarse flotation of potassium feldspar. A potassium feldspar particle floated with a bubble to the surface of the ore slurry to form a foam layer, and the foam layer was scraped off by a scraper to yield a second coarse potassium feldspar concentrate. Other minerals that could not float up, mainly quartz, were left in the ore slurry, and filtered and dried to form a quartz concentrate.
(4.4) Fine flotation of coarse potassium feldspar concentrate: The first coarse potassium feldspar concentrate and the second coarse potassium feldspar concentrate were combined, stirred and aerated without adding a collector. A foam formed was scraped off by a scraper, and filtered and dried to yield a potassium feldspar concentrate. Other minerals that could not float up were left in the ore slurry to form a fourth intermediate ore slurry, which was mixed with the second intermediate ore slurry.
Example 2 Example 2 was different from Example 1 in that: {4.3) Coarse flotation of potassium feldspar: 650 g of sulfuric acid with a mass concentration of 5% was added per ton of second intermediate ore slurry, and the pH of the ore slurry was adjusted to 4.5. Others were the same as those in Example 1.
Example 3 Example 3 was different from Example 1 in that: (4.3) Coarse flotation of potassium feldspar: 800 g of sulfuric acid with a mass concentration of 5% was added per ton of second intermediate ore slurry, and the pH of the ore slurry was adjusted to 4.0. Others were the same as those in Example 1. Example 4 Example 4 was different from Example 1 in that: {4.3) Coarse flotation of potassium feldspar: 650 g of sulfuric acid with a mass concentration of 5% was added per ton of second intermediate ore slurry. The pH of the ore slurry was adjusted to 4.5, and the ore slurry was stirred for 3 min. Then 250 g of sodium hexametaphosphate was added per ton of second intermediate ore slurry. Others were the same as those in Example 1.
Example 5 Example 5 was different from Example 1 in that: (4.3) Coarse flotation of potassium feldspar: 650 g of sulfuric acid with a mass concentration of 5% was added per ton of second intermediate ore slurry. The pH of the ore slurry was adjusted to 4.5, and the ore slurry was stirred for 3 min.
Then 200 g of sodium hexametaphosphate was added per ton of second intermediate ore slurry, and the ore slurry was stirred for 3 min. 150 g of collector composed of sodium oleate and dodecylamine with amass ratio of 1:4 was added per ton of second intermediate ore slurry, and the ore slurry was aerated for a first-stage coarse flotation of potassium feldspar. Others were the same as those in Example 1.
The composition of the potassium feldspar concentrate, the mica concentrate and the quartz concentrate extracted by Examples 1 to 5 was tested. The test results are shown in Table
1.
Table 1 Composition of potassium feldspar concentrate, mica concentrate and quartz concentrate extracted by Examples 1 to 5
Test Yield K.0 Na-,O Fe, 04 510; Product name No. (%) (wt. 2) | (wt. 2) | (Wwh.%) | (wt .&) Potassium 66.86 Example feldspar 11.89 3.12 0.05 65.26 1 concentrate Mica 13.59
10.25 2.73 0.62 61.28 concentrate Quartz 14.34
1.35 0.47 0.05 92.85 concentrate Potassium 67.10 Example feldspar 12.10 3.51 0.05 64.25 2 concentrate Mica 13.21
10.32 2.66 0.63 61.27 concentrate Quartz 13.28
1.22 0.41 0.05 93.38 concentrate Potassium 06.45 Example feldspar 12.25 3.43 0.05 64.98 3 concentrate Mica 13.67
10.41 2.56 0.68 61.02 concentrate Quartz 14.10
1.24 0.34 93.93 concentrate Potassium 66.22 Example feldspar 12.05 3.17 0.03 65.16 4 concentrate cone [mn] enen fe
10.32 2.42 0.62 61.22 concentrate cy | [vn [enn
1.52 0.42 0.05 93.88 concentrate Potassium 65.85 Example feldspar 12.45 3.23 0.05 64.42 concentrate i EE EY
10.10 2.55 0.66 61.36 concentrate tty [oe [en [en [en
1.46 0.38 0.05 92.58 concentrate As can be seen from Table 1 that the present invention uses a raw ore magnetic separation-fluorine-free weak acid flotation process to perform the beneficiation and 5 purification of the potassium feldspar ore to obtain high-quality potassium/sodium feldspar concentrate, mica concentrate and quartz concentrate. On the premise of ensuring the comprehensive utilization of resources, the present invention reduces the impact on the equipment and environment, and reduces the production cost, which effectively illustrates the superiority of the magnetic separation-fluorine-free weak acid flotation process of the present invention. The above descriptions are merely preferred implementations of the present invention. It should be noted that a person of ordinary skill in the art may further make several improvements and modifications without departing from the principle of the present invention, but such improvements and modifications should be deemed as falling within the protection scope of the present invention.
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