CN114054214B - Combined inhibitor for flotation separation of complex refractory copper-lead sulfide ore and application thereof - Google Patents
Combined inhibitor for flotation separation of complex refractory copper-lead sulfide ore and application thereof Download PDFInfo
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- CN114054214B CN114054214B CN202111406397.0A CN202111406397A CN114054214B CN 114054214 B CN114054214 B CN 114054214B CN 202111406397 A CN202111406397 A CN 202111406397A CN 114054214 B CN114054214 B CN 114054214B
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- 239000003112 inhibitor Substances 0.000 title claims abstract description 83
- 238000005188 flotation Methods 0.000 title claims abstract description 75
- 238000000926 separation method Methods 0.000 title claims abstract description 58
- FPIIKJRRXOPKIB-UHFFFAOYSA-N copper;sulfanylidenelead Chemical compound [Cu].[Pb]=S FPIIKJRRXOPKIB-UHFFFAOYSA-N 0.000 title claims abstract description 34
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 40
- 229960001922 sodium perborate Drugs 0.000 claims abstract description 35
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 claims abstract description 35
- 229920002472 Starch Polymers 0.000 claims abstract description 34
- 239000008107 starch Substances 0.000 claims abstract description 34
- 235000019698 starch Nutrition 0.000 claims abstract description 34
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 33
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 33
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 33
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 33
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 claims abstract description 31
- 239000010949 copper Substances 0.000 claims abstract description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000012141 concentrate Substances 0.000 claims description 42
- WIKSRXFQIZQFEH-UHFFFAOYSA-N [Cu].[Pb] Chemical compound [Cu].[Pb] WIKSRXFQIZQFEH-UHFFFAOYSA-N 0.000 claims description 32
- 230000002000 scavenging effect Effects 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 6
- PWZUZQNZVZKCBI-UHFFFAOYSA-N o-ethyl carbamothioate Chemical compound CCOC(N)=S PWZUZQNZVZKCBI-UHFFFAOYSA-N 0.000 claims description 5
- CMGLSTYFWSQNEC-UHFFFAOYSA-N o-ethyl n-ethylcarbamothioate Chemical compound CCNC(=S)OCC CMGLSTYFWSQNEC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- DSCFFEYYQKSRSV-UHFFFAOYSA-N 1L-O1-methyl-muco-inositol Natural products COC1C(O)C(O)C(O)C(O)C1O DSCFFEYYQKSRSV-UHFFFAOYSA-N 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 4
- VJXUJFAZXQOXMJ-UHFFFAOYSA-N D-1-O-Methyl-muco-inositol Natural products CC12C(OC)(C)OC(C)(C)C2CC(=O)C(C23OC2C(=O)O2)(C)C1CCC3(C)C2C=1C=COC=1 VJXUJFAZXQOXMJ-UHFFFAOYSA-N 0.000 claims description 4
- DSCFFEYYQKSRSV-KLJZZCKASA-N D-pinitol Chemical compound CO[C@@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@H]1O DSCFFEYYQKSRSV-KLJZZCKASA-N 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 239000004571 lime Substances 0.000 claims description 4
- 239000010665 pine oil Substances 0.000 claims description 4
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000001238 wet grinding Methods 0.000 claims description 2
- 230000000994 depressogenic effect Effects 0.000 claims 4
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 abstract description 40
- 229910052949 galena Inorganic materials 0.000 abstract description 39
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 18
- 239000011707 mineral Substances 0.000 abstract description 18
- 239000003814 drug Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 11
- 230000005764 inhibitory process Effects 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 230000002401 inhibitory effect Effects 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 231100000956 nontoxicity Toxicity 0.000 abstract description 5
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 28
- 235000010755 mineral Nutrition 0.000 description 17
- 238000003756 stirring Methods 0.000 description 10
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 6
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 6
- 229910052951 chalcopyrite Inorganic materials 0.000 description 5
- 229910052745 lead Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052950 sphalerite Inorganic materials 0.000 description 3
- 229910021532 Calcite Inorganic materials 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229940072033 potash Drugs 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229940116411 terpineol Drugs 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-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
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- -1 hydroxypropyl methyl Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- HRPSNEGMPFDHPH-UHFFFAOYSA-N potassium lead(2+) oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [K+].[Pb+2].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O HRPSNEGMPFDHPH-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001612 separation test Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Images
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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic 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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
-
- 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
-
- 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)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a combined inhibitor for flotation separation of complex refractory copper-lead sulphide ores, which comprises sodium perborate, quaternary ammonium starch ether and hydroxypropyl methyl cellulose. By combining the inorganic inhibitor and the organic inhibitor, the synergistic effect between the agents is fully exerted, the inhibition effect on galena is enhanced, the mutual content of copper and lead is reduced, and the copper and lead separation effect is good; by adding the sodium perborate solution, the oxidation sites on the surface of the galena are improved, more quaternary ammonium starch ether and hydroxypropyl methyl cellulose are adsorbed on the surface of the galena, and the inhibition effect on the galena is enhanced; the flotation step of mixing flotation and then flotation separation is adopted, so that non-target minerals can be removed to the maximum extent in the mixing flotation process, the workload of the subsequent flotation process is reduced, and the working efficiency of ore flotation is improved; compared with a single galena inhibitor and a traditional inhibitor dichromate, the inhibitor has the advantages of low medicament consumption, strong inhibiting capability, no toxicity and environmental protection.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a combined inhibitor for flotation separation of complex refractory copper-lead sulfide ores and application thereof.
Background
Copper and lead are important non-ferrous metal mineral resources, are widely applied to various industries and are essential metal elements for economic development of China. The separation of copper-lead polymetallic sulphide ores is always one of the important subjects of the mineral separation world, and because the ores are generally compact and intergrowth and have fine embedded granularity, and galena and chalcopyrite have extremely similar floatability, the separation of the copper-lead polymetallic sulphide ores is difficult. In addition, along with the continuous development and utilization of the existing mineral resources, the rich ores which can be directly used in China are less and less, and the existing mineral resources also face the current situations of poverty, fineness and impurity. Therefore, the research on the high-efficiency separation of the copper-lead sulfide ore is of great significance.
In nature, the main source of lead is galena, often coexisting with sulphide minerals such as chalcopyrite, sphalerite and the like. In the separation of galena and other sulphide minerals, inhibitors of galena are mainly divided into two categories: inorganic inhibitors and organic inhibitors. The inorganic inhibitor is mainly dichromate, sulfite and the like, such as potassium dichromate, can effectively inhibit galena, but has certain harm to the environment; the organic inhibitor is mainly macromolecular medicaments such as carboxymethyl cellulose, sodium humate and the like, but the macromolecular medicaments are easily embedded in the copper-lead ore with extremely fine granularity, so that the inhibition effect on the square-lead ore is not obvious. In the prior art, the above problems are solved by using a combination inhibitor. However, the combined inhibitors of the prior art are generally environmentally hazardous and have limited inhibitory effect on the ore.
In the prior art, the invention patent application with publication number CN 104772218A discloses a flotation separation process of copper-lead bulk concentrates, which is to add lime and sodium sulfide into copper-lead bulk concentrates separated from raw ores, stir for 2-4 min, dehydrate and remove drugs through a thickener, add a combined inhibitor and a collecting agent, roughen to obtain copper rough ores and lead rough ores, and finely select the copper rough ores to obtain copper concentrates; scavenging lead rough ores to obtain lead concentrate; the combined inhibitor is a combination of sulfuric acid, sodium sulfite and humic acid. However, sodium sulfite which is harmful to the environment exists in the combined inhibitor adopted in the technical scheme, and the requirements of no toxicity and environmental protection cannot be met.
In view of the above, there is a need for an improved non-toxic environment-friendly combined inhibitor with good inhibition effect for flotation separation of complex refractory copper-lead sulfide ores, so as to solve the above problems.
Disclosure of Invention
The invention aims to provide a non-toxic environment-friendly composite inhibitor with good inhibition effect for flotation separation of complex refractory copper-lead sulfide ores.
In order to achieve the purpose, the invention provides a combined inhibitor for flotation separation of complex refractory copper-lead sulfide ores, which comprises a sodium perborate aqueous solution, a quaternary ammonium starch ether aqueous solution and a hydroxypropyl methyl cellulose aqueous solution, wherein the addition ratio of the sodium perborate aqueous solution to the quaternary ammonium starch ether aqueous solution to the hydroxypropyl methyl cellulose aqueous solution is (1-2): (1.5-3): (2-4); the mass percent of the sodium perborate aqueous solution is 5-10%, the mass percent of the quaternary ammonium starch ether aqueous solution is 0.5-1%, and the mass percent of the hydroxypropyl methyl fiber aqueous solution is 0.5-1%.
Further, the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose are both high molecular organic compounds, the molecular weight of the quaternary ammonium starch ether is 5-8 ten thousand, the molecular weight of the hydroxypropyl methyl cellulose is 8-12 ten thousand, and the purity of the sodium perborate is 60-90%.
The invention also provides an application method of the combined inhibitor for flotation separation of the complex refractory copper-lead sulphide ore for copper-lead separation of the copper-lead sulphide ore, which comprises the following steps:
s1, crushing the adopted copper-lead sulphide ore raw ore, and then carrying out wet grinding to obtain raw ore pulp;
s2, placing the raw ore pulp obtained in the step S1 into a flotation machine for a first roughing test, performing two times of concentration on flotation foams obtained by roughing, returning the concentrated tailings to the previous operation in sequence, performing two times of scavenging on the tailings obtained by roughing, returning the scavenged concentrates to the previous level in sequence to form a closed cycle, obtaining copper-lead bulk concentrates after two times of concentration, and obtaining final tailings after two times of scavenging;
s3, placing the copper-lead bulk concentrate obtained in the step S2 into a flotation machine for a second roughing test, carrying out tertiary concentration on flotation foam obtained by roughing, adding a required amount of the combined inhibitor in the concentration process according to the requirement of each concentration, wherein the active components of the combined inhibitor comprise sodium perborate, quaternary ammonium starch ether and hydroxypropyl methyl cellulose, and the adding proportion of the sodium perborate, the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose is (1-2): (1.5-3): (2-4), returning the tailings obtained by fine concentration to the previous stage in sequence, performing primary scavenging on the tailings obtained by rough concentration, returning scavenged concentrate to the previous stage in sequence to form closed cycle, obtaining copper concentrate after three times of fine concentration, and obtaining lead concentrate after primary scavenging.
Further, in step S3, 1500-5000 g/t of activated carbon and 500-1000 g/t of combined inhibitor are added in the rough concentration process, 200-300 g/t of combined inhibitor is added in the first concentration, 100-200 g/t of combined inhibitor is added in the second concentration, and 50-100 g/t of combined inhibitor is added in the third concentration.
Further, in step S2, roughly selecting and adding 800-1200 g/t of water glass, 20-50 g/t of ethyl thionocarbamate and 20-30 g/t of pine oil; 10-20 g/t of ethyl thiourethane and 10-15 g/t of pinitol oil are added in the first scavenging; and adding 5-10 g/t of ethyl thionocarbamate and 5-10 g/t of pine oil in the second scavenging.
Further, in step S1, the pH value of the ore pulp is adjusted to 8-9 by lime.
Further, in step S1, the content of the ground ore with the fineness of-0.074 mm accounts for 70-80%.
Further, in step S1, water is added to the pulp concentration of 30-40%.
Further, in step S2, the concentration process does not add any agent, and in step S3, the sweep process does not add any agent.
The invention has the beneficial effects that:
the invention provides a combined inhibitor for flotation separation of complex refractory copper-lead sulfide ores, which comprises sodium perborate, quaternary ammonium starch ether and hydroxypropyl methyl cellulose; the method comprises the following steps of combining an inorganic inhibitor and an organic inhibitor by adopting a drug adding mode of a combined medicament, wherein the adding proportion of sodium perborate, quaternary ammonium starch ether and hydroxypropyl methyl cellulose is (1-2): (1.5-3): (2-4), when the copper-lead sulfide ore flotation agent is used for ore flotation, the synergistic effect among agents is fully exerted, the effective inhibition on galena is enhanced, the mutual content of copper and lead is reduced, and the separation effect of the copper-lead sulfide ore is good; by adding the sodium perborate solution into the pulp solution, the oxidation sites on the surface of the galena are improved, so that more macromolecular organic compound quaternary ammonium starch ether and hydroxypropyl methyl cellulose are adsorbed on the surface of the galena, and the inhibiting effect on the galena is enhanced; the flotation step of mixing flotation and then flotation separation is adopted, so that non-target minerals can be removed to the maximum extent in the mixing flotation process, the workload of the subsequent flotation process is reduced, and the working efficiency of ore flotation is improved; compared with a single galena inhibitor and a traditional inhibitor, namely dichromate, the inhibitor has the advantages of low medicament consumption, strong inhibiting capability, no toxicity and environmental protection, and has good industrial application prospect.
Drawings
FIG. 1 is a schematic process flow diagram of the combined inhibitor for flotation separation of complex refractory copper-lead sulphide ores for flotation separation of copper-lead sulphide ores.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the aspects of the present invention are shown in the drawings, and other details not closely related to the present invention are omitted.
In addition, it is also to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Example 1
Taking a certain copper-lead polymetallic sulphide ore in Yunnan as an object, wherein the raw ore contains 0.28 percent of Cu and 2.98 percent of Pb, the main ore minerals are chalcopyrite, galena and sphalerite, and the main gangue minerals are calcite, quartz, potash feldspar and the like;
in this embodiment, the galena combination inhibitor is added together with a 5% sodium perborate solution, a 0.5% quaternary ammonium starch ether solution, and a 0.5% hydroxypropyl methylcellulose solution at a ratio of 1: 1.5: 2.5;
referring to fig. 1, a combined inhibitor for flotation separation of complex refractory copper-lead sulfide ore is used for flotation separation of copper-lead sulfide ore, and comprises the following steps:
s1, crushing the collected raw ore to-2 mm, then grinding the crushed ore finely until the particle fineness of ore particles is-0.074 mm and accounts for 75%, adding water for size mixing until the concentration of ore pulp is 33%; then, adjusting the pH value of the ore pulp to 8 by using lime to provide a good reaction environment for the interaction of a subsequent medicament and ore;
s2, performing a mixed flotation test on the ore pulp obtained in the step S1, wherein the flotation test comprises the following steps: 1 roughing, 2 concentrating and 2 scavenging to obtain copper-lead bulk concentrate and tailings;
a roughing process: adding 850g/t of silicate inhibitor water glass, 30g/t of collecting agent ethyl thionocarbamate and 20g/t of foaming agent terpineol oil into the ore pulp obtained in the step S1, stirring for 3min, and then performing rough concentration for 3min to obtain rough copper lead concentrate and rough tailings;
a scavenging process: during the first scavenging, 10g/t of ethyl thiourethane and 10g/t of pinitol oil are added into the rough tailings, scavenging is carried out after stirring for 3min, scavenging is carried out for 2min, during the second scavenging, 5g/t of ethyl thiourethane and 5g/t of pinitol oil are added, scavenging is carried out after stirring for 3min, scavenging time is 2min, and the concentrates subjected to the two scavenging are sequentially returned to the previous stage to form closed cycle, so that tailings are finally obtained;
a selection process: the process does not add any medicament, and directly stirs the rough copper-lead concentrate obtained in the rough concentration process for 3min and then carries out fine concentration for 2min to obtain copper-lead bulk concentrate I; then stirring the copper-lead bulk concentrate I for 3min, wherein the concentration time is 2min, finally obtaining copper-lead bulk concentrate II, and the middlings of the copper-lead bulk concentrate II repeatedly return to the concentration process to form closed cycle;
s3, performing flotation separation test on the copper-lead bulk concentrate obtained in the step S2, wherein the flotation test comprises the following steps: 1 roughing, 3 concentrating and 1 scavenging to obtain copper concentrate and lead concentrate;
the roughing process comprises the following steps: adding 2000g/t of activated carbon into the copper-lead bulk concentrate II, stirring for 3min, removing a medicament residual on the surface of the mineral, adding 500g/t of a combined inhibitor, stirring for 3min, and then performing roughing, wherein the roughing time is 3min, so as to obtain copper rough concentrate and lead rough concentrate;
a scavenging process: the process does not add any reagent, lead rough concentrate obtained in the roughing process is directly stirred for 3min and then scavenged, scavenging time is 2min, lead concentrate is obtained, middlings of the lead concentrate are returned to the previous stage, and closed cycle is formed;
a selection process: adding 200g/t of combined inhibitor into the copper rough concentrate obtained in the rough concentration process, stirring for 3min, and then carrying out first fine concentration for 2 min; then, adding 100g/t of combined inhibitor, stirring for 3min, and then carrying out secondary selection, wherein the selection time is 2 min; then, 50g/t of combined inhibitor is added, the mixture is stirred for 3min and then is subjected to third concentration for 2min, finally copper concentrate is obtained, the concentrate obtained by the second and third concentration is returned to the previous stage in sequence to form closed cycle, and the flotation separation result is shown in table 1.
Comparative example 1
Comparative example 1 differs from example 1 only in that: the potassium dichromate is used as an inhibitor, other steps are basically the same as those of the example 1, the details are not repeated, and the flotation separation result is shown in the table 1.
Table 1 flotation separation results of copper-lead bulk concentrate in example 1 and comparative example
From the test results in table 1, it can be seen that the copper-lead separation can be achieved well by using the combined inhibitor of the present invention, and the mutual content in the copper-lead concentrate is low. Compared with the traditional potassium dichromate lead-inhibiting copper flotation, the separation method in the technical scheme has the same effect as the separation of copper and lead by potassium dichromate, and the combined inhibitor used in the invention has the advantages of no toxicity and environmental protection.
Example 2
Taking a certain copper-lead metal sulfide ore in Sichuan as an object, wherein the raw ore contains 0.45 percent of Cu and 3.24 percent of Pb, the copper mainly exists in a chalcopyrite form, the lead mainly exists in a galena form, and the embedding granularity is fine;
in this example, the galena combination inhibitor is added together with a 5% sodium perborate solution, a 0.5% quaternary ammonium starch ether solution, and a 0.5% hydroxypropyl methylcellulose solution at a ratio of 1.5: 2: 2.5; compared with the embodiment 1, the difference is only that: the dosage of the combined inhibitor in the roughing process in the step S3 is 600g/t, other steps are basically the same as those in the example 1, the description is omitted, and the flotation separation result is shown in Table 2.
Table 2 flotation separation results of copper-lead bulk concentrate in example 2
As can be seen from the test results in Table 2, the combined inhibitor of the invention can well realize the separation of copper and lead, and has lower mutual content of copper and lead and higher recovery rate.
Example 3
Taking a copper-lead metal sulfide ore in certain Hunan as an object, wherein a raw ore contains 0.19 percent of Cu and 2.37 percent of Pb, copper mainly exists in chalcopyrite, and lead mainly exists in galena;
in this example, the galena combination inhibitor is a sodium perborate solution with a mass concentration of 5%, a quaternary ammonium starch ether solution of 0.5% and a hydroxypropyl methylcellulose solution of 0.5% added together in a ratio of 1: 2: 3; compared with the embodiment 1, the difference is only that: 1200g/t of water glass is added in the roughing process in the step S2, 3000g/t of activated carbon and 800g/t of combined inhibitor are added in the roughing process in the step S3, 250g/t of combined inhibitor is added in the first concentrating, 150g/t of combined inhibitor is added in the second concentrating, other steps are basically the same as those in the example 1, repeated description is omitted, and the flotation separation result is shown in Table 3.
Table 3 flotation separation of copper-lead bulk concentrate in example 3
As can be seen from the test results in Table 3, the combined inhibitor of the invention can well realize the separation of copper and lead, and has lower mutual content of copper and lead and higher recovery rate.
Example 4 to example 7
Taking a certain copper-lead polymetallic sulphide ore in Yunnan as an object, wherein the raw ore contains 0.28 percent of Cu and 2.98 percent of Pb, the main ore minerals are chalcopyrite, galena and sphalerite, and the main gangue minerals are calcite, quartz, potash feldspar and the like; in this example, the galena combination inhibitor is added together with a 5% sodium perborate solution, a 0.5% quaternary ammonium starch ether solution, and a 0.5% hydroxypropyl methylcellulose solution by mass concentration; compared with the embodiment 1, the difference is only that: the mass ratios of the sodium perborate solution, the quaternary ammonium starch ether solution and the hydroxypropyl methylcellulose solution are different, other steps are basically the same as those in example 1, and are not repeated herein, and the flotation separation results are shown in table 4.
TABLE 4 addition mass ratio of sodium perborate solution, quaternary ammonium starch ether solution and hydroxypropyl methylcellulose solution in examples 1-7 and copper recovery rate under the same conditions
From the test results in table 4, it can be seen that when the sodium perborate, the quaternary ammonium starch ether and the hydroxypropyl methylcellulose are added in the mass ratio of (1-2): (1.5-3): (2-4), the combined inhibitor formed by combining the three components has the best inhibiting effect on galena in the copper-lead sulfide ores, and the best copper-lead separation effect.
The technical personnel in the field should understand that the mass percent of the sodium perborate solution related to the invention can also be 6%, 7% or 10%, the mass percent of the quaternary ammonium starch ether solution can also be 0.6%, 0.7% or 1%, and the mass percent of the hydroxypropyl methyl cellulose solution can also be 0.6%, 0.7% or 1%, which is not limited herein, and only needs to be added in a proper amount according to the actual needs.
The technical principle of the present invention is explained as follows:
according to the invention, the copper-lead sulfide ore is subjected to flotation by adopting the flotation steps of mixing flotation and then separation, and the water glass, the collecting agent ethyl thiourethane and the terpineol oil are added in the mixing flotation process to separate target minerals from non-target minerals to the greatest extent, so that the treatment capacity of subsequent operation is reduced, and the copper-lead bulk concentrate is obtained. And then, carrying out flotation separation on the copper-lead bulk concentrate by using the combined inhibitor provided by the invention. In the flotation separation, the addition proportion of the sodium perborate solution, the quaternary ammonium starch ether solution and the hydroxypropyl methyl cellulose solution is (1-2) in mass ratio: (1.5-3): (2-4), the mixed solution of the three acts on the surface of the ore together to inhibit the deleading ore, so that the flotation of the copper-lead sulfide ore is realized. As the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose are used as the inhibitor of the galena, in a flotation environment, the surface of the galena is slightly oxidized by dissolved oxygen or hydrogen peroxide in ore pulp, a small amount of oxidation sites are generated on the surface of ore particles, and the inhibitor is adsorbed on the oxidation sites, but the adsorption amount of the inhibitor is very small, the adsorption of a collecting agent on the surface of the galena cannot be prevented, and the inhibiting effect of the inhibitor on the galena is not obvious. The sodium perborate in the combined inhibitor is used as an oxidation auxiliary agent, when the sodium perborate exists, the oxidation sites on the surface of ore particles can be increased, so that the inhibitor is adsorbed on more oxidation sites, and meanwhile, a hydrophilic film is formed on the surface of the ore by long chains of the inhibitor, so that the collecting agent is prevented from being adsorbed on the surface of galena. The experimental result shows that when the sodium perborate, the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose are added according to the proportion, the effective inhibition on galena can be realized, the lead in the copper-lead sulfide ore can be selected favorably, and the floating of copper is not influenced. When the content of the sodium perborate in the combined inhibitor is too low, the oxidation sites on the surface of the galena are too few, the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose adsorbed on the surface of the galena are limited, and the inhibiting effect on the galena is not obvious. When the content of the sodium perborate in the combined inhibitor is too high, the oxidation sites on the surface of the galena are too many, the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose adsorbed on the surface of the galena are too excessive, and the floatability of the mineral is too low, so that the flotation work is not facilitated; meanwhile, excessive sodium perborate influences the pH value of ore pulp, and further influences the flotation environment; in addition, the inhibition effect of the sodium perborate on galena is not obvious, which is not beneficial to the separation of copper and lead and can affect the recovery rate and grade of copper.
In conclusion, the combined inhibitor comprising sodium perborate, quaternary ammonium starch ether and hydroxypropyl methyl cellulose and used for flotation separation of complex refractory copper-lead sulfide ores, provided by the invention, combines an inorganic inhibitor and an organic inhibitor and is used for ore flotation according to a certain addition ratio, so that the synergistic effect among the agents is fully exerted, the effective inhibition on the square lead ores is enhanced, the mutual content of copper and lead is reduced, and the copper-lead separation effect is good; by adding the sodium perborate solution, the oxidation sites on the surface of the galena are improved, so that more macromolecular organic compounds, namely quaternary ammonium starch ether and hydroxypropyl methyl cellulose, are adsorbed to the surface of the galena, and the inhibiting effect on the galena is enhanced; the flotation step of mixing flotation and then flotation separation is adopted, so that non-target minerals can be removed to the maximum extent in the mixing flotation process, the workload of the subsequent flotation process is reduced, and the working efficiency of ore flotation is improved; compared with a single galena inhibitor and a traditional inhibitor dichromate, the inhibitor has the advantages of low medicament consumption, strong inhibition capability, no toxicity and environmental protection.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (9)
1. A combined inhibitor for flotation separation of complex refractory copper-lead sulfide ores is characterized by comprising a sodium perborate aqueous solution, a quaternary ammonium starch ether aqueous solution and a hydroxypropyl methyl cellulose aqueous solution, wherein the addition ratio of the sodium perborate aqueous solution to the quaternary ammonium starch ether aqueous solution to the hydroxypropyl methyl cellulose aqueous solution is (1-2): (1.5-3): (2-4); the mass percent of the sodium perborate aqueous solution is 5-10%, the mass percent of the quaternary ammonium starch ether aqueous solution is 0.5-1%, and the mass percent of the hydroxypropyl methyl cellulose aqueous solution is 0.5-1%.
2. The combined inhibitor for flotation separation of complex refractory copper-lead sulfide ores according to claim 1, wherein the quaternary ammonium starch ether and the hydroxypropyl methylcellulose are both high molecular weight organic compounds, the molecular weight of the quaternary ammonium starch ether is 5-8 ten thousand, the molecular weight of the hydroxypropyl methylcellulose is 8-12 ten thousand, and the purity of the sodium perborate is 60-90%.
3. The use of the combined depressant for the flotation separation of the complex refractory copper-lead sulphide ore in any one of claims 1 to 2, which is used for the copper-lead separation of the complex refractory copper-lead sulphide ore, comprises the following steps:
s1, crushing the adopted copper-lead sulphide ore raw ore, and then carrying out wet grinding to obtain raw ore pulp;
s2, placing the raw ore pulp obtained in the step S1 into a flotation machine for a first roughing test, carrying out two times of fine separation on flotation foams obtained by the roughing, returning the fine tailings to the previous operation in sequence, carrying out two times of scavenging on the tailings obtained by the roughing, returning the scavenged concentrates to the previous level in sequence to form closed cycle, obtaining copper-lead bulk concentrates after the two times of fine separation, and obtaining final tailings after the two times of scavenging;
s3, placing the copper-lead bulk concentrate obtained in the step S2 into a flotation machine for a second roughing test, carrying out tertiary concentration on flotation foam obtained by roughing, adding a required amount of a combined inhibitor in the concentration process according to the requirement of each concentration, wherein the active components of the combined inhibitor comprise sodium perborate, quaternary ammonium starch ether and hydroxypropyl methyl cellulose, and the adding proportion of the sodium perborate, the quaternary ammonium starch ether and the hydroxypropyl methyl cellulose is (1-2): (1.5-3): (2-4), returning the tailings obtained by fine concentration to the previous stage in sequence, performing primary scavenging on the tailings obtained by rough concentration, returning scavenged concentrate to the previous stage in sequence to form closed cycle, obtaining copper concentrate after three times of fine concentration, and obtaining lead concentrate after primary scavenging.
4. The application of the combined inhibitor for flotation separation of complex refractory copper-lead sulphide ores according to claim 3, wherein in the step S3, 1500-5000 g/t of activated carbon and 500-1000 g/t of combined inhibitor are added in the roughing process, 200-300 g/t of combined inhibitor is added in the first concentrating process, 100-200 g/t of combined inhibitor is added in the second concentrating process, and 50-100 g/t of combined inhibitor is added in the third concentrating process.
5. The application of the combined inhibitor for flotation separation of the complex refractory copper-lead sulphide ore according to claim 3, wherein in the step S2, 800-1200 g/t of water glass, 20-50 g/t of ethyl thionocarbamate and 20-30 g/t of pine oil are added in a roughing mode; 10-20 g/t of ethyl thiourethane and 10-15 g/t of pinitol oil are added in the first scavenging; and adding 5-10 g/t of ethyl thionocarbamate and 5-10 g/t of pine oil in the second scavenging.
6. The use of the combined depressant for the flotation separation of complex refractory copper-lead sulphide ores according to claim 3, wherein in step S1, the pH value of the ore pulp is adjusted to 8-9 by using lime.
7. The application of the combined inhibitor for flotation separation of complex refractory copper-lead sulphide ores according to claim 3, wherein in the step S1, the content of ore grinding fineness of-0.074 mm accounts for 70-80%.
8. The use of the combined depressant for flotation separation of complex refractory copper-lead sulphide ores according to claim 3, wherein in step S1, water is added to the ore pulp with a concentration of 30-40%.
9. The use of the combined depressant for flotation separation of complex refractory copper-lead sulphide ores according to claim 3, wherein in step S2 the concentration process does not add any agent and in step S3 the scavenging process does not add any agent.
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