CN114985113B - Method for strengthening separation of scheelite and calcium-containing mineral by using quinic acid and metal complex thereof as inhibitor - Google Patents
Method for strengthening separation of scheelite and calcium-containing mineral by using quinic acid and metal complex thereof as inhibitor Download PDFInfo
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- CN114985113B CN114985113B CN202210515634.5A CN202210515634A CN114985113B CN 114985113 B CN114985113 B CN 114985113B CN 202210515634 A CN202210515634 A CN 202210515634A CN 114985113 B CN114985113 B CN 114985113B
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- Prior art keywords
- scheelite
- quinic acid
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- calcium
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Links
- 239000003112 inhibitor Substances 0.000 title claims abstract description 58
- AAWZDTNXLSGCEK-LNVDRNJUSA-N (3r,5r)-1,3,4,5-tetrahydroxycyclohexane-1-carboxylic acid Chemical compound O[C@@H]1CC(O)(C(O)=O)C[C@@H](O)C1O AAWZDTNXLSGCEK-LNVDRNJUSA-N 0.000 title claims abstract description 57
- AAWZDTNXLSGCEK-UHFFFAOYSA-N Cordycepinsaeure Natural products OC1CC(O)(C(O)=O)CC(O)C1O AAWZDTNXLSGCEK-UHFFFAOYSA-N 0.000 title claims abstract description 57
- AAWZDTNXLSGCEK-ZHQZDSKASA-N Quinic acid Natural products O[C@H]1CC(O)(C(O)=O)C[C@H](O)C1O AAWZDTNXLSGCEK-ZHQZDSKASA-N 0.000 title claims abstract description 57
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 50
- 239000011707 mineral Substances 0.000 title claims abstract description 50
- 239000011575 calcium Substances 0.000 title claims abstract description 32
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 31
- 238000000926 separation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005728 strengthening Methods 0.000 title claims abstract description 10
- 150000004696 coordination complex Chemical class 0.000 title description 3
- 238000005188 flotation Methods 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 229910052751 metal Chemical class 0.000 claims abstract description 13
- 239000002184 metal Chemical class 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims description 29
- 229910021532 Calcite Inorganic materials 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000006260 foam Substances 0.000 claims description 13
- 238000007790 scraping Methods 0.000 claims description 10
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 8
- 239000010436 fluorite Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000004088 foaming agent Substances 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 5
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 3
- VDEUYMSGMPQMIK-UHFFFAOYSA-N benzhydroxamic acid Chemical compound ONC(=O)C1=CC=CC=C1 VDEUYMSGMPQMIK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 229940125507 complex inhibitor Drugs 0.000 claims description 2
- 239000002223 garnet Substances 0.000 claims description 2
- HBROZNQEVUILML-UHFFFAOYSA-N salicylhydroxamic acid Chemical compound ONC(=O)C1=CC=CC=C1O HBROZNQEVUILML-UHFFFAOYSA-N 0.000 claims description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000010665 pine oil Substances 0.000 claims 1
- 239000012141 concentrate Substances 0.000 abstract description 32
- 230000000694 effects Effects 0.000 abstract description 18
- 230000005764 inhibitory process Effects 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 235000010755 mineral Nutrition 0.000 description 32
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 22
- 229910052721 tungsten Inorganic materials 0.000 description 22
- 239000010937 tungsten Substances 0.000 description 22
- 239000003814 drug Substances 0.000 description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 6
- 235000019353 potassium silicate Nutrition 0.000 description 5
- NEAQRZUHTPSBBM-UHFFFAOYSA-N 2-hydroxy-3,3-dimethyl-7-nitro-4h-isoquinolin-1-one Chemical compound C1=C([N+]([O-])=O)C=C2C(=O)N(O)C(C)(C)CC2=C1 NEAQRZUHTPSBBM-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid group Chemical group C(C1=CC=CC=C1)(=O)O WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 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 description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 229910003641 H2SiO3 Inorganic materials 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
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000015424 sodium Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- 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
-
- 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
- B03D2203/04—Non-sulfide 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
Abstract
The invention discloses a method for strengthening and separating scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors, which comprises the following steps: step one: weighing a certain amount of mixed ore samples of scheelite and calcium-containing minerals, adding the mixed ore samples into a flotation tank, adding a proper amount of water, and stirring in a flotation machine; step two: adding a pH regulator to regulate the ore pulp to a certain pH value; step three: the hydrophilicity of the mineral surface is regulated by adding a certain amount of quinic acid or metal-quinic acid complex organic inhibitor solution. The invention strengthens the selective separation of scheelite and calcium-containing minerals by adopting quinic acid and metal-quinic acid complex as inhibitors, has wider dosage range of quinic acid, has very weak inhibition effect on scheelite even under the condition of dosage, and can effectively improve WO in concentrate 3 The process is environment-friendly, has remarkable environmental benefit and economic benefit, and is suitable for industrial production.
Description
Technical Field
The invention relates to a method for separating scheelite and calcium-containing minerals, in particular to a method for strengthening and separating scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors, belonging to the technical field of separation science.
Background
Scheelite inhibitors are largely divided into two main classes, inorganic inhibitors and organic inhibitors. In order to enhance the selective inhibition of gangue minerals by inhibitors, researchers have conducted extensive research into novel high-potency inhibitors as well as combination inhibitors. Silicate and phosphate are commonly used scheelite inorganic inhibitors, the application of water glass in silicate is the most widely, practice proves that the optimal modulus (SiO 2/Na 2O) of the water glass is 2.4-2.8, and it is generally considered that HSiO 3-and H2SiO3 generated by water glass hydrolysis are adsorbed on the surface of scheelite, so that the water glass is hydrophilic and plays a role in inhibition; it is also known that colloidal SiO2 in water glass can also play a role in inhibition in addition to HSiO 3-and H2SiO 3. She Xue by uniformly roughing scheelite with Na2CO3+ Na2SiO3 as regulator, adding a large amount of Na2SiO3 for normal temperature concentration, and obtaining scheelite concentrate with WO3 grade of 69.84% and recovery rate of 70.76% from raw ore with WO3 grade of 0.22%. Besides the water glass series medicaments, phosphate inhibitors are also widely applied in scheelite flotation practice. In research such as the ocean, the selective inhibition effect of sodium hexametaphosphate on calcium-containing gangue minerals is found to be that the Ca-X intensity of the mineral surface is weak, and Ca < 2+ > on the mineral surface is easy to act with sodium hexametaphosphate to be masked in a liquid phase, so that the active particles on the mineral surface, which act with a collector, are reduced.
The organic inhibitor is also a commonly used inhibitor in scheelite flotation, has the advantages of multiple types, wide raw materials, environmental protection, capability of designing functional groups and molecular weight according to requirements, and the like, and can be divided into a small molecular inhibitor and a large molecular inhibitor according to the molecular weight. The commonly used small molecule inhibitors in scheelite flotation mainly comprise oxalic acid, citric acid, tartaric acid, lactic acid and the like, and the macromolecular organic inhibitors mainly comprise tannin, starch, gelatin copying, carboxymethyl cellulose, dextrin, sodium humate and the like. Zhang Ying and the like show that water molecules and minerals on the surface of the sodium polyacrylate discharged mineral in ore pulp are adsorbed, the adsorption energy is negative, and the inhibition strength of sodium polyacrylate on 3 kinds of minerals under the natural pH condition is fluorite > calcite > scheelite. The macromolecular organic inhibitor has the characteristics of low dosage and high efficiency, and the selectivity of inhibition can be improved by modifying the macromolecular inhibitor. The combined inhibitor is an important component of mixed medicines, and the combined use of medicines is an important development direction in the field of flotation medicines. Compared with single inhibitor, the mixed use of the inhibitor can obviously enhance the selective inhibition on gangue minerals, improve foam mineralization, reduce the cyclic load of middlings, improve the flotation index of scheelite, and has wide application prospect.
From the research of scheelite flotation in recent years, the development of new medicaments, the modification of medicaments and the combined use of different types of medicaments are the research trend of scheelite flotation medicaments. The macromolecular organic inhibitor has a good effect on the flotation separation of scheelite and gangue, and is a promising flotation reagent for scheelite. The combined use of the medicaments can exert the synergistic effect among the medicaments and has positive effect on scheelite flotation. Although the research and development of scheelite medicaments are advanced, the scheelite medicaments have the problems of high price, serious environmental pollution and the like, and the inhibitor has the defects of insufficient selectivity, narrow dosage range, easy inhibition effect on scheelite and serious resource loss. It is difficult to meet the requirements of many concentrating mills. Therefore, development and search of scheelite agents with good flotation effect, low cost and environmental friendliness are efforts of mineral dressing workers.
Disclosure of Invention
The invention aims to provide a method for strengthening and separating scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors, so as to solve the problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions: the method comprises the following steps:
step one: weighing a certain amount of mixed ore samples of scheelite and calcium-containing minerals, adding the mixed ore samples into a flotation tank, adding a proper amount of water, and stirring in a flotation machine;
step two: adding a pH regulator to regulate the ore pulp to a certain pH value;
step three: adding a certain amount of quinic acid or metal-quinic acid complex organic inhibitor solution to regulate the hydrophilicity of the mineral surface;
step four: adding a certain amount of active agent to regulate the ore pulp;
step five: adding a certain amount of collector solution to regulate the hydrophobicity of the mineral surface;
step six: adding a certain amount of foaming agent to regulate the ore pulp;
step seven: aerating, and performing flotation and foam scraping operation;
step eight: for foam productionThe product is dried and weighed, and tested in WO 3 Is calculated WO 3 Is a recovery rate of (2).
As a preferable technical scheme of the invention, the mixed sample of scheelite and calcium-containing mineral in the step one, wherein the calcium-containing mineral is one or more of calcite, fluorite and garnet, and the content of the calcium-containing mineral is 30-95% and the content of the scheelite is 5-60%.
As a preferable technical scheme of the invention, the pH adjuster in the second step is: one or more of sodium carbonate, sodium hydroxide and hydrochloric acid, and the pH value is 2.0-12.0.
As a preferred technical scheme of the invention, the step three certain amount of quinic acid solution is as follows: the dosage is 0.01X10 -4 mol/L-30×10 -4 The mol/L metal ion in the metal-quinic acid complex is Al 3+ 、Fe 3+ 、Ni 2+ 、Er 3+ 、La 3+ 、Y 3+ 、Ti 4+ 、Zn 2+ The molar ratio of the metal ions to quinic acid is 0.1:1-15:1; the dosage of the metal-quinic acid complex inhibitor is 0.005×10 -4 mol/L-30×10 -4 mol/L。
As a preferable technical scheme of the invention, the activating agent in the fourth step is lead nitrate and aluminum sulfate, and the dosage of the activating agent is as follows: 0-50×10 -4 mol/L。
As a preferable technical scheme of the invention, the types and the amounts of the collecting agents in the fifth step are as follows: sodium oleate (amount of 0.1X10) -4 mol/L-0×10 -4 mol/L), cetyltrimethyl sodium bromide (amount: 0.05X10 g -4 mol/L-80×10 -4 mol/L), benzoic hydroxamic acid (amount: 0.01X10 -4 mol/L-30×10 -4 mol/L), salicylic hydroxamic acid (amount: 0.01X10 -4 mol/L-30×10 -4 mol/L), naphthenic acid (amount: 0.1X10 times -4 mol/L-100×10 -4 mol/L), sodium oleate + benzohydroxamic acid (amount: 0.01X10 -4 mol/-30×10 -4 mol/L; the molar ratio is as follows: 0.1:1-10:1).
As a preferable technical scheme of the invention, the foaming agent in the step six is pinitolOne or more of oil and methyl isobutyl carbinol (MIBC), and foaming agent in an amount of 0-30X10 × -4 mg/L。
As a preferable technical scheme of the invention, the flotation scraping time in the step seven is 0.5-8min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to a method for strengthening and separating scheelite and calcium-containing mineral by using quinic acid and metal complex thereof as inhibitor, which strengthens the selective separation of scheelite and calcium-containing mineral by using quinic acid and metal-quinic acid complex as inhibitor, has wider dosage range of quinic acid, has very weak inhibition effect on scheelite even under the condition of dosage, and can effectively improve WO in concentrate 3 The process is environment-friendly, has remarkable environmental benefit and economic benefit, and is suitable for industrial production.
2. According to the method for strengthening and separating scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors, disclosed by the invention, quinic acid or metal-quinic acid complexes are used as inhibitors, the working procedure is simple, the cost is low, the quinic acid sources are wide, and the quinic acid can be extracted from plants.
3. The invention relates to a method for strengthening and separating scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors.
Drawings
FIG. 1 is a flow chart of a flotation separation process of scheelite and calcium-containing minerals according to the present invention;
FIG. 2 is a chart showing the effect of quinic acid as an inhibitor on scheelite separation from calcite according to the present invention;
FIG. 3 is a chart showing the effect of quinic acid as an inhibitor on scheelite separation from fluorite according to the present invention;
FIG. 4 is a chart showing the effect of quinic acid to Fe3+ mole ratio on scheelite to calcite separation in accordance with the present invention;
FIG. 5 is a chart showing the effect of the metal-quinic acid complex of the invention as an inhibitor on scheelite separation from calcite.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-5, the present invention provides a technical scheme of a method for strengthening separation of scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors:
according to the figures 1-5, the method comprises the following steps:
step one: weighing a certain amount of mixed ore samples of scheelite and calcium-containing minerals, adding the mixed ore samples into a flotation tank, adding a proper amount of water, and stirring in a flotation machine;
step two: adding a pH regulator to regulate the ore pulp to a certain pH value;
step three: adding a certain amount of quinic acid or metal-quinic acid complex organic inhibitor solution to regulate the hydrophilicity of the mineral surface;
step four: adding a certain amount of active agent to regulate the ore pulp;
step five: adding a certain amount of collector solution to regulate the hydrophobicity of the mineral surface;
step six: adding a certain amount of foaming agent to regulate the ore pulp;
step seven: aerating, and performing flotation and foam scraping operation;
step eight: drying and weighing the foam product, and testing WO 3 Is calculated WO 3 Is a recovery rate of (2).
Example 1
In the test, weighing a mixed mineral sample with the mass of 4g, wherein the proportion of scheelite to calcite in the mixed mineral sample is 1:1, adding the mixed mineral sample and a proper amount of water into a flotation tank with the volume of 40mL, stirring for 3min, sequentially adding sodium hydroxide to adjust the pH value of ore pulp to 8.5, and stirring for 3min; adding a certain amount of quinic acid solution with concentration of 0.5X10 -4 mol/L-3×10 -4 mol/L, stirring for 3min; adding lead nitrate solution with concentration of 1.5X10 -4 mol/L, stirring for 3min; adding a benzoic hydroxamic acid solution with a concentration of 1.5X10 -4 mol/L, stirring for 3min; adding MIBC solution with concentration of 0.5X10 -4 mol/L, stirring for 3min, performing flotation and foam scraping operation for 3min to obtain tungsten concentrate K and tailings X, respectively oven drying, weighing, and assaying WO in the concentrate 3 And calculates the recovery rate, and compares the difference between the grade of tungsten concentrate and the recovery rate under different quinic acid concentration conditions.
FIG. 2 shows the effect of quinic acid as inhibitor on the separation of scheelite from calcite in this example, and shows that the concentration of quinic acid increases, the grade of tungsten concentrate increases significantly, the recovery rate decreases slowly, and the concentration is 1.5X10 -4 In the mol/L process, the grade of concentrate K is 64.98 percent at most, the recovery rate is 91.02 percent, the grade of tungsten concentrate is kept stable along with the continuous increase of the concentration of quinic acid, the recovery rate is slightly reduced, and the recovery rate is more than 80 percent, so that quinic acid does not have a strong inhibitor effect on scheelite under the condition of high concentration and only has a strong selective inhibition effect on calcite, and therefore, a tungsten concentrate product with high grade and high recovery rate can be obtained in the separation of scheelite and calcite by using quinic acid as an inhibitor.
Example 2
In the test, weighing 4g of mixed ore sample, wherein the proportion of scheelite to fluorite in the mixed ore sample is 1:1, adding the mixed ore sample and a proper amount of water into a flotation tank with the volume of 40mL, stirring for 3min, sequentially adding sodium hydroxide to adjust the pH value of ore pulp to 8.5, and stirring for 3min; adding a certain amount of quinic acid solution with concentration of 0.5X10 -4 mol/L-3×10 -4 mol/L, stirring for 3min; adding sodium oleate solution with concentration of 3.0X10 -4 mol/L, and stirring for 3min. Finally, carrying out flotation foam scraping operation, wherein the foam scraping time is 3min, obtaining tungsten concentrate K and tailings X, respectively drying and weighing, and testing WO in the concentrate 3 And calculates the recovery rate, and compares the difference between the grade of tungsten concentrate and the recovery rate under the condition of different concentrations of quinic acid.
FIG. 3 is the present embodimentIn the examples, the effect of quinic acid as inhibitor on the separation of scheelite and fluorite is shown by the graph that the concentration of quinic acid increases, the grade of tungsten concentrate obviously increases, the recovery rate decreases slowly and the concentration is 2.0X10 -4 When the mol/L concentration is increased, the grade of concentrate K is 67.46% at most, the recovery rate is 88.15%, the grade of scheelite is stable along with the continuous increase of the concentration of quinic acid, the recovery rate is slightly reduced, and the recovery rate is higher than 85%, so that quinic acid does not have a strong inhibitor effect on scheelite under the condition of high concentration and only has a strong selective inhibition effect on fluorite, and therefore, a tungsten concentrate product with high grade and high recovery rate can be obtained in the separation of scheelite and fluorite by using quinic acid as an inhibitor.
Example 3
In the test, 6 groups of scheelite and calcite mixed ore samples with the mass of 4g are weighed, the ratio of scheelite to calcite in the mixed ore samples is 1:1, the scheelite and the calcite mixed ore samples are separated and added into a flotation tank with the volume of 40mL for stirring for 3min, sodium hydroxide is sequentially added to adjust the pH value of ore pulp to 8.5, and stirring is carried out for 3min; respectively adding quinic acid and Fe 3+ The molar ratio of the Fe-quinic acid complex solution is 1:0, 1:1/4, 1:1/2, 1:1, 1:2 and 1:4, the concentration is 1.5X10-4 mol/L, and the mixture is stirred for 3min; adding lead nitrate solution with concentration of 1.5X10 -4 mol/L, stirring for 3min; adding a benzoic hydroxamic acid solution with a concentration of 1.5X10 -4 mol/L, stirring for 3min; adding MIBC solution with concentration of 0.5X10-4 mol/L, stirring for 3min, and performing flotation and foam scraping operation for 3min to obtain tungsten concentrate K and tailings X, respectively oven drying, weighing, and assaying WO in the concentrate 3 And calculate the recovery rate, compare quinic acid with Fe 3+ The influence of Fe-quinic acid complex inhibitors formed in different molar ratios on the grade and recovery rate of tungsten concentrate.
FIG. 4 shows quinic acid and Fe in this example 3+ The effect of the molar ratio on the separation of scheelite from calcite, as can be seen, with Fe 3+ The grade of tungsten concentrate is gradually increased, the recovery rate is slightly reduced, and when quinic acid and Fe are mixed 3+ When the molar ratio of the tungsten concentrate to the tungsten concentrate is more than 1:2, the grade K of the tungsten concentrate is recoveredThe yield was drastically lowered, and it was found that a small amount of Fe was added to the quinic acid solution 3+ The Fe quinic acid complex can effectively improve the grade of tungsten concentrate, has no influence on the recovery rate, and can obtain tungsten concentrate products with high grade and high recovery rate in the separation of scheelite and calcite.
Example 4
In the test, 6 groups of scheelite and calcite mixed ore samples with the mass of 4g are weighed, the ratio of scheelite to calcite in the mixed ore samples is 1:1, the scheelite and the calcite mixed ore samples are separated and added into a flotation tank with the volume of 40mL for stirring for 3min, sodium hydroxide is sequentially added to adjust the pH value of ore pulp to 8.5, and stirring is carried out for 3min; respectively adding quinic acid, al-quinic acid, fe-quinic acid, er-quinic acid, zn-quinic acid, and La-quinic acid solution (the molar ratio of metal ion to quinic acid is 1:2), wherein the quinic acid concentration is 1.5X10 -4 mol/L, stirring for 3min; adding lead nitrate solution with concentration of 1.5X10 -4 mol/L, stirring for 3min; adding a benzoic hydroxamic acid solution with a concentration of 1.5X10 -4 mol/L, stirring for 3min; adding MIBC solution with concentration of 0.5X10-4 mol/L, stirring for 3min, and performing flotation and foam scraping operation for 3min to obtain tungsten concentrate K and tailings X, respectively oven drying, weighing, and assaying WO in the concentrate 3 And calculates the recovery rate, and compares the difference of the grade and the recovery rate of the tungsten concentrate under the condition of different metal-quinic acid complex inhibitors.
Fig. 5 shows the effect of using metal-quinic acid complex as inhibitor on separating scheelite from calcite in this example, and shows that when using metal-quinic acid complex as inhibitor, the grade of tungsten concentrate is obviously improved compared with that of quinic acid alone, the recovery rate is only slightly reduced, the grade of concentrate K is higher than 68%, and the recovery rate is higher than 86%, so that using metal-quinic acid complex as inhibitor can effectively improve the grade of tungsten concentrate, and has no influence on recovery rate basically, and the tungsten concentrate product with high grade and high recovery rate can be obtained in separating scheelite from calcite.
In the description of the present invention, it should be understood that the orientation or positional relationship indicated is based on the orientation or positional relationship shown in the drawings, and is merely for convenience in describing the present invention and simplifying the description, and does not indicate or imply that the apparatus or element referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and defined otherwise, for example, it may be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intermediaries, or in communication with each other or in interaction with each other, unless explicitly defined otherwise, the meaning of the terms described above in this application will be understood by those of ordinary skill in the art in view of the specific circumstances.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The method for strengthening and separating scheelite and calcium-containing minerals by using quinic acid and metal complexes thereof as inhibitors is characterized by comprising the following steps:
step one: weighing a certain amount of mixed ore samples of scheelite and calcium-containing minerals, adding the mixed ore samples into a flotation tank, adding a proper amount of water, and stirring in a flotation machine;
step two: adding a pH regulator to regulate the ore pulp to a certain pH value;
step three: adding a certain amount of quinic acid or metal-quinic acid complex organic inhibitor solution to adjust the hydrophilicity of the mineral surface, wherein the certain amount of quinic acid solution is as follows: the dosage is 0.01X10 -4 mol/L-30×10 -4 The mol/L metal ion in the metal-quinic acid complex is Al 3+ 、Fe 3+ 、Ni 2+ 、Er 3+ 、La 3+ 、Y 3+ 、Ti 4+ 、Zn 2+ Molar coordination of metal ions with quinic acidThe ratio is 0.1:1-15:1; the dosage of the metal-quinic acid complex inhibitor is 0.005×10 -4 mol/L-30×10 - 4 mol/L；
Step four: adding a certain amount of active agent to regulate the ore pulp;
step five: adding a certain amount of collector solution to regulate the hydrophobicity of the mineral surface;
step six: adding a certain amount of foaming agent to regulate the ore pulp;
step seven: aerating, and performing flotation and foam scraping operation;
step eight: drying and weighing the foam product, and testing WO 3 Is calculated WO 3 Is a recovery rate of (2).
2. The method for the enhanced separation of scheelite and calcium-containing minerals using quinic acid and its metal complexes as inhibitors according to claim 1, wherein: the mixed sample of scheelite and calcium-containing mineral in the first step, wherein the calcium-containing mineral is one or more of calcite, fluorite and garnet, and the content of the calcium-containing mineral is 30-95% and the content of scheelite is 5-60%.
3. The method for the enhanced separation of scheelite and calcium-containing minerals using quinic acid and its metal complexes as inhibitors according to claim 1, wherein: the pH regulator in the second step is as follows: one or more of sodium carbonate, sodium hydroxide and hydrochloric acid, and the pH value is 2.0-12.0.
4. The method for the enhanced separation of scheelite and calcium-containing minerals using quinic acid and its metal complexes as inhibitors according to claim 1, wherein: the activating agent in the fourth step is lead nitrate and aluminum sulfate, and the using amount of the activating agent is as follows: 0-50×10 -4 mol/L。
5. The method for the enhanced separation of scheelite and calcium-containing minerals using quinic acid and its metal complexes as inhibitors according to claim 1, wherein: capturing in the fifth stepThe types and the dosage of the collecting agent are as follows: the dosage of sodium oleate is as follows: 0.1X10 times -4 mol/L-0×10 -4 The mol/L and the dosage of the hexadecyl trimethyl sodium bromide are as follows: 0.05X10 g -4 mol/L-80×10 -4 The mol/L and the using amount of the benzohydroxamic acid are as follows: 0.01X10 -4 mol/L-30×10 -4 The mol/L and the salicylic hydroxamic acid consumption are as follows: 0.01X10 -4 mol/L-30×10 -4 The mol/L and naphthenic acid consumption are as follows: 0.1X10 times -4 mol/L-100×10 -4 The mol/L and the dosage of sodium oleate and the benzohydroxamic acid are as follows: 0.01X10 -4 mol/-30×10 -4 mol/L; the molar ratio is as follows: 0.1:1-10:1.
6. The method for the enhanced separation of scheelite and calcium-containing minerals using quinic acid and its metal complexes as inhibitors according to claim 1, wherein: the foaming agent in the step six is one or more of pine oil and methyl isobutyl carbinol, and the dosage of the foaming agent is 0-30 multiplied by 10 -4 mg/L。
7. The method for the enhanced separation of scheelite and calcium-containing minerals using quinic acid and its metal complexes as inhibitors according to claim 1, wherein: the flotation foam scraping time in the step seven is 0.5-8min.
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