CN112474065A - Method for selecting phosphorus from low-grade vanadium titano-magnetite tailings - Google Patents
Method for selecting phosphorus from low-grade vanadium titano-magnetite tailings Download PDFInfo
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- CN112474065A CN112474065A CN202011230321.2A CN202011230321A CN112474065A CN 112474065 A CN112474065 A CN 112474065A CN 202011230321 A CN202011230321 A CN 202011230321A CN 112474065 A CN112474065 A CN 112474065A
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- phosphorus
- low
- flotation
- vanadium titano
- grade vanadium
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- 239000011574 phosphorus Substances 0.000 title claims abstract description 69
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 69
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 38
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 26
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000005188 flotation Methods 0.000 claims abstract description 45
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 31
- 239000011707 mineral Substances 0.000 claims abstract description 31
- 239000003112 inhibitor Substances 0.000 claims abstract description 30
- 239000012141 concentrate Substances 0.000 claims abstract description 26
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 20
- 239000010452 phosphate Substances 0.000 claims abstract description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000007885 magnetic separation Methods 0.000 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 claims abstract description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 33
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 25
- 235000019353 potassium silicate Nutrition 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 20
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 14
- 238000007790 scraping Methods 0.000 claims description 14
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 13
- 239000006260 foam Substances 0.000 claims description 12
- 230000002000 scavenging effect Effects 0.000 claims description 11
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 6
- -1 2-carboxyphosphoryl acetic acid Chemical compound 0.000 claims description 5
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 5
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims 2
- 229940105329 carboxymethylcellulose Drugs 0.000 claims 2
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910021538 borax Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 21
- 238000011084 recovery Methods 0.000 abstract description 12
- 239000003814 drug Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000002367 phosphate rock Substances 0.000 abstract description 5
- 235000014113 dietary fatty acids Nutrition 0.000 abstract description 4
- 239000000194 fatty acid Substances 0.000 abstract description 4
- 229930195729 fatty acid Natural products 0.000 abstract description 4
- 150000004665 fatty acids Chemical class 0.000 abstract description 4
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010419 fine particle Substances 0.000 abstract description 2
- 229910052586 apatite Inorganic materials 0.000 description 23
- 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 23
- 239000010459 dolomite Substances 0.000 description 19
- 229910021532 Calcite Inorganic materials 0.000 description 18
- 229910000514 dolomite Inorganic materials 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 238000012360 testing method Methods 0.000 description 9
- 238000010408 sweeping Methods 0.000 description 7
- 239000011575 calcium Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 230000000994 depressogenic effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- ZQCUDFIHJAXGTP-UHFFFAOYSA-N [Na].C(CCCCCCCC=CCCCCCCCC)(=O)O Chemical compound [Na].C(CCCCCCCC=CCCCCCCCC)(=O)O ZQCUDFIHJAXGTP-UHFFFAOYSA-N 0.000 description 1
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical group [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 125000003010 ionic group Chemical group 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
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- 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
- 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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—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
- B03D2203/06—Phosphate ores
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for selecting phosphorus from low-grade vanadium titano-magnetite tailings, which comprises the following steps: carrying out low-intensity magnetic separation and tailing discarding on the low-grade vanadium-titanium magnetite tailings to obtain magnetic minerals and phosphorus flotation feed ores; the phosphorus flotation feeding is carried out the size mixing to obtain the ore pulp, and the regulator sodium carbonate and the gangue inhibitor HQ-P are added into the ore pulp in sequence1HQ-P as collector2And performing direct flotation phosphorus separation to obtain high-quality phosphate concentrate and phosphate separation tailings. The invention aims at the phosphorus separation of low-grade vanadium titano-magnetite tailings, and adopts low-intensity magnetic separation tailing discarding-magnetic separation tailings positive flotation in view of low phosphorus content of raw oresCompared with the full-flotation phosphorus separation process, the magnetic separation-flotation process has the advantages that the cost is reduced by 20-25% compared with the full-flotation process, and the economic benefit is improved. HQ-P inhibitor of the invention1With collector HQ-P2The combined use effectively avoids the problems of serious influence of argillized gangue, difficult fine particle floatation, poor selectivity of the fatty acid collecting agent, low recovery rate under low temperature and the like in phosphorite floatation, and obtains a high-phosphorus-grade phosphate concentrate product under the condition of low medicament dosage.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a method for selecting phosphorus from low-grade vanadium titano-magnetite tailings.
Background
The vanadium titano-magnetite is an important ferrous metal mineral resource in China, the storage capacity of the vanadium titano-magnetite in Chengdu area of Hebei exceeds 100 hundred million tons, the vanadium titano-magnetite is another large vanadium titano-magnetite except Panzhihua in China, and the titanium storage capacity is the second nationwide. The resource mineral has complex composition and many associated elements, and contains valuable elements such as phosphorus and the like besides iron. Magnetite is mostly recovered by adopting a magnetic separation process in a phosphosiderite separation plant, and low-grade phosphosiderite tailings have no mature flotation process and medicament system and can only be discarded as waste ores, so that the severe waste of phosphorus resources is caused. Therefore, in the face of the current situation that phosphorite resources are increasingly scarce, research on phosphorus separation of low-grade vanadium titano-magnetite tailings is carried out, and the method has important significance in the aspects of improving the comprehensive utilization rate of resources, reducing the transportation pressure of north China's phosphorus transportation, realizing sustainable development of phosphate fertilizer industry and agriculture in China and the like.
Flotation has always been considered the most efficient method for recovering phosphate rock. The flotation separation is difficult due to the fact that the main phosphorite apatite has extremely similar surface properties to carbonate gangue minerals (dolomite and calcite). In addition, because apatite and dolomite/calcite are mostly complex in embedding relationship, the embedding granularity is fine, the apatite and the dolomite/calcite belong to easily ground minerals, and the apatite and the dolomite/calcite are easily crushed in the crushing and grinding processes to cause serious argillization. The flotation after desliming causes large phosphorus loss, and the flotation concentrate grade and recovery rate are low. The water glass and the fatty acid collecting agent become the most commonly used inhibitor and collecting agent in the phosphorite flotation practice due to the advantages of wide sources, relatively low price and the like. However, the water glass is used as an inhibitor, and the inhibition force on the gangue is insufficient, the dosage of the required medicament is large, so that the gangue floats upwards and is seriously entrained, and the tailing wastewater is difficult to settle; in addition, the fatty acid medicament mainly containing oleic acid (sodium) is used as the collector, particularly in northern areas, the temperature is reduced, the dissolving and dispersing capacity of the fatty acid collector is obviously reduced, the medicament dosage is increased, the phosphorus recovery rate is reduced, and the waste of mineral resources is caused.
Therefore, how to obtain a high-grade phosphate concentrate product and ensure a high flotation recovery rate, a targeted gangue inhibitor and collector for low-grade phosphate ore separation are urgently needed to be developed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for efficiently floating and recovering phosphorus in low-grade vanadium titano-magnetite tailings, which can obtain a high-grade phosphorus concentrate product under the condition of not desliming and simultaneously ensure higher phosphorus flotation recovery rate.
The invention provides a phosphorus separation method of low-grade vanadium titano-magnetite tailings, which comprises the following steps:
1) magnetic separation: firstly, carrying out low-intensity magnetic separation and tailing discarding on low-grade vanadium-titanium magnetite tailings to obtain magnetic minerals and non-magnetic minerals (phosphorus flotation feeding);
2) flotation: mixing the nonmagnetic minerals obtained in the step 1) to obtain ore pulp, and sequentially adding a regulator sodium carbonate and a gangue inhibitor HQ-P into the ore pulp1HQ-P as collector2Performing direct flotation phosphorus separation to obtain high-quality phosphate concentrate and phosphate separation tailings;
wherein: HQ-P1Comprises 100 (10-15) parts by mass of 20-45 parts by mass of water glass and carboxymethylCellulose (CMC) and 2-carboxyphosphorylacetic acid (HPAA);
HQ-P2the anti-corrosion agent is composed of sodium oleate and polyethylene glycol monomethyl ether (MPEG-200) in a mass ratio of (80-95) to (5-20).
In the step 1), the magnetic field intensity of the low-intensity magnetic separation is 0.2-0.5T.
In the step 2), the modulus of the water glass is 2.5-3.0; the molecular formula of the 2-carboxyl phosphoryl acetic acid (HPAA) is C2H5O6P, the structural formula is as follows:
the molecular formula of the polyethanol monomethyl ether MPEG-200 is C23H48O12The structural formula is as follows:
preferably, the gangue inhibitor HQ-P1Respectively consists of water glass, carboxymethyl cellulose (CMC) and 2-carboxyl phosphoryl acetic acid (HPAA) with the mass ratio of 100:12: 36.
Preferably, the gangue inhibitor HQ-P1Respectively consists of water glass, carboxymethyl cellulose (CMC) and 2-carboxyl phosphoryl acetic acid (HPAA) with the mass ratio of 100:13: 39.
Preferably, the collector HQ-P2Respectively consists of sodium oleate and polyethanol monomethyl ether (MPEG-200) with the mass ratio of 90: 10.
Preferably, the collector HQ-P2Respectively consists of sodium oleate and polyethanol monomethyl ether (MPEG-200) with the mass ratio of 92: 8.
The direct flotation phosphorus separation operation is one coarse, one sweep and three fine.
The specific steps of the primary roughing operation are as follows: mixing the phosphorus flotation feed ore, adding 800-4000 g/t of sodium carbonate into the ore pulp, and stirring for 2-3 min; adding 200-600 g/t of gangue inhibitor HQ-P1Stirring 2-3 min; adding 100-500 g/t of collecting agent HQ-P2Stirring for 2-3 min; and (4) scraping and soaking for 4-6 min to obtain rough concentrate, wherein the product in the tank is scavenging feed ore.
The one-time scavenging operation comprises the following specific steps: adding 30-200 g/t of collecting agent HQ-P into scavenging feed ores2Stirring for 2-3 min, and scraping for 2-3 min to obtain scavenged foam product, returning the scavenged foam product to the roughing tank, wherein the product in the tank is the tailing product.
The third selection operation comprises the following specific steps: the first concentration, the second concentration and the third concentration are blank concentration, foam scraping is started after full stirring, the foam scraping time is 2-3 min, 1.5-2.5 min and 1.0-2 min respectively, and all middlings are returned to the previous flotation operation in sequence; and obtaining the final phosphate concentrate product.
The term "g/t" used in the present invention refers to the addition amount of the chemical agent relative to the phosphorus ore dressing, for example, the addition amount of the gangue depressant is 200g/t, which means that 200g of the gangue depressant is required to be added for treating 1 ton of phosphorus ore dressing.
The principle of the invention is as follows:
the water glass is an effective inhibitor of silicate gangue minerals and is also a good dispersant, so that the viscosity of the ore pulp is effectively reduced, and the entrainment of fine-grain gangue and mica minerals is reduced. Carboxymethyl cellulose (CMC) is an effective inhibitor and slime flocculant for calcium-containing, magnesium silicate, carbonate gangue minerals, argillaceous minerals, etc. The electrostatic attraction and chemical adsorption between the carboxyl in CMC molecule and calcium ion on the surface of the mollite/dolomite are the main reasons for selective adsorption of CMC on the surface of calcite/dolomite. Many other hydroxyl groups associate with water through hydrogen bonds, resulting in hydrophilic mineral surfaces. In addition, CMC can flocculate fine-grained calcite/dolomite, increasing the probability of action of calcite/dolomite with 2-carboxyphosphorylacetic acid (HPAA). HPAA has 1 phosphorus oxygen group (-PO) in its molecule3H2) And 2 carboxylic acid groups (-COOH), in the alkaline ore pulp, HPAA shows stronger anionic property and hydrophilicity due to ionization, and negatively charged oxygen ions are easy to generate electrostatic interaction with calcium ions on the surface of the calcium-containing mineral. Research shows that phosphorus oxy and carboxyl in HPAA molecules are negatively charged, the distance between the two functional groups is close to the Ca-Ca distance on the surface of calcite/dolomite, and the distance is far away from the Ca-Ca distanceSmaller than the Ca-Ca spacing of the apatite surface. Thus, HPAA adsorbs more readily on the calcite/dolomite surface than apatite, further inhibiting the adsorption of the collector, which is inhibited. In contrast, HPAA adsorbs poorly on apatite surfaces and does not affect apatite flotation. The combination of the three inhibitors can more strongly inhibit calcite/dolomite under the condition of reducing the viscosity of ore pulp, particularly selectively inhibit fine-fraction calcite/dolomite, and overcome the defects of large dosage, poor inhibition effect on fine-fraction gangue and the like of the traditional inhibitor. The combined inhibitor has weak action with the surface of the apatite, and basically does not influence the flotation of the apatite.
The polyethanol monomethyl ether (MPEG-200) is a high-surface-activity green environment-friendly nonionic surfactant, and has no collecting property on apatite. After the sodium oleate and the polyethanol monomethyl ether are compounded, the surface activity of a compounded system is higher than that of a single sodium oleate system, and the critical micelle concentration is lower than that of the single polyethanol monomethyl ether and the single sodium oleate. Therefore, the collecting performance of the sodium oleate on the apatite is obviously improved under the low-temperature condition. Sodium oleate and polyethanol monomethyl ether are subjected to co-adsorption on the surface of apatite, due to the interaction of hydrophobic chains and the reduction of electrostatic repulsion among ionic groups, the adsorption effect of the sodium oleate is enhanced by the existence of MPEG-200, and particularly under the condition of low concentration, the adsorption of the compound collector on the surface of the apatite is stronger than that of single sodium oleate. Compared with the single sodium oleate serving as the collecting agent, the composite collecting agent has denser flotation foam, large foam ore carrying capacity and strong collecting performance on fine-grained apatite, and is more favorable for improving the flotation recovery rate of the apatite.
The combined inhibitor can effectively and selectively inhibit dolomite/calcite, reduce mechanical entrainment of fine-grain gangue and mica minerals, is matched with a compounded collecting agent for use, and can simultaneously ensure the phosphorus grade and the phosphorus recovery rate in phosphate concentrate under the low-temperature condition.
The invention has the beneficial effects that:
(1) aiming at the phosphorus separation of the low-grade vanadium-titanium magnetite tailings, in view of low phosphorus content of raw ores, the process of low-intensity magnetic separation tailing discarding in advance and magnetic separation tailing direct flotation phosphorus separation is adopted, and compared with full flotation phosphorus separation, the magnetic separation-flotation process has the advantages that the cost is reduced by 20-25% compared with the full flotation process, and the economic benefit is improved;
(2) based on the principle of mixed application, HQ-P inhibitor with good effect of inhibiting calcium-containing gangue such as calcite/dolomite1The phosphorus-containing water glass is combined with water glass according to a certain weight proportion, so that argillaceous gangue can be effectively inhibited, and a high-grade phosphate concentrate product is obtained;
(3) by compounding sodium oleate and polyethanol monomethyl ether, the apatite collecting agent has stronger apatite collecting capability under the conditions of low temperature and low dosage. The purpose of selective separation can be achieved under the condition of no mud removal through the matching use of the combined inhibitor and the compound collector. The raw materials of the medicament have wide sources, are easy to prepare and easy to implement industrial operation;
(4) after the phosphorus separation method and the reagent system provided by the invention are adopted, when the low-grade phosphorus-containing vanadium titano-magnetite tailings are treated, the tailings contain 0.8-2.5% of phosphorus, the phosphorus grade in the phosphorus concentrate is more than 35%, and the phosphorus flotation operation recovery rate is more than 77%.
Drawings
FIG. 1 is a flow chart of a sorting process of example 1 and comparative examples 1 to 5;
FIG. 2 is a flow chart of a sorting process of comparative example 6;
FIG. 3 is a flow chart of the sorting process of example 2 and comparative example 7;
Detailed Description
Example 1
The mineral dressing tailings of a certain vanadium titano-magnetite in Hebei river have low phosphorus content and P content2O5The content of the mineral is 1.63%, the relative content of the apatite is about 6%, the main gangue minerals are calcite and dolomite, the relative content of the minerals is up to 12.5%, and the mineral also contains gangue such as mica, quartz and the like. The argillization is serious, the content of minus 38 mu m reaches 40 percent, the particle size distribution range of apatite and calcite/dolomite is 10 to 150 mu m, the thickness distribution is not uniform, and the apatite separation index is not ideal.
The process flow of this example is shown in fig. 1, and the specific sorting process and the pharmaceutical system are as follows:
(1) firstly, carrying out low-intensity magnetic separation and tailing discarding on the tailings, wherein the magnetic field intensity is 0.4T, and obtaining nonmagnetic minerals (phosphorus flotation feeding);
(2) roughing operation: mixing the phosphorus flotation feed ore, and stirring for 1 min; sequentially adding 1250g/t of sodium carbonate, stirring for 2min, adding 300g/t of gangue inhibitor HQ-P1Stirring for 2min, and adding 400g/t of collecting agent HQ-P2Stirring for 2min, and scraping and soaking for 5min to obtain rougher concentrate and scavenging feed;
(3) primary scavenging operation: adding 90g/t of collecting agent HQ-P into scavenging feed ore2Stirring for 2min, and scraping and soaking for 3min to obtain final tailings;
(4) and (3) performing tertiary concentrate operation: and (3) blank concentration is carried out on the first concentration, the second concentration and the third concentration, and the foam scraping time is respectively 2min, 2min and 1.5min, so that the final phosphate concentrate is obtained.
The gangue inhibitor HQ-P1Respectively consists of water glass, carboxymethyl cellulose (CMC) and 2-carboxyl phosphoryl acetic acid (HPAA) with the mass ratio of 100:12: 36.
The collector HQ-P2Consists of sodium oleate and polyethanol monomethyl ether (MPEG-200) with the mass ratio of 90: 10.
Wherein sodium carbonate is prepared into 5% water solution, and added with gangue inhibitor HQ-P1Preparing into 2% aqueous solution, adding collecting agent HQ-P2Prepared into 2 percent aqueous solution for adding. The test results are shown in table 1# 1.
Comparative example 1
The process flow was the same as in example 1 except that a single water glass was used as the gangue depressant. The flotation results are shown in figure 2 #.
Roughing: 300g/t water glass, 400g/t HQ-P2;
Sweeping: 90g/t HQ-P2;
Comparative example 2
The process flow was the same as in example 1 except that the collector was sodium oleate alone. The flotation results are shown in # 3 in table 1.
Roughing: 300g/t HQ-P1400g/t sodium oleate;
sweeping: 90g/t sodium oleate;
comparative example 3
The process flow was the same as in example 1 except that the gangue depressants used were single water glass and the collector used was single sodium oleate. The flotation results are shown in # 4 in table 1.
Roughing: 300g/t of water glass and 400g/t of sodium oleate
Sweeping: 90g/t of sodium oleate
Comparative example 4
The process flow is the same as in example 1, except that the gangue inhibitor HQ-P1Respectively consists of water glass, carboxymethyl cellulose (CMC) and 2-carboxyl phosphoryl acetic acid (HPAA) with the mass ratio of 100:25: 30. The test results are shown in table 1 as # 5.
Roughing: 300g/t HQ-P1HQ-P of 400g/t2;
Sweeping: 90g/t HQ-P2;
Comparative example 5
The process flow is identical to that of example 1, except that the collector HQ-P2The test result is shown in 6# in Table 1, which is composed of sodium oleate and polyethanol monomethyl ether (MPEG-200) with a mass ratio of 100: 20.
Roughing: 300g/t HQ-P1HQ-P of 400g/t2;
Sweeping: 90g/t HQ-P2;
Comparative example 6
The phosphorus-selecting feed ore is completely screened out by materials with a granularity of-400 meshes (-0.038mm), then the flotation test is carried out, the test flow is shown in figure 2, and the test result is shown in 7# in table 1. Wherein the gangue inhibitor adopts single water glass, and the collecting agent adopts single sodium oleate.
Roughing: 300g/t of water glass and 400g/t of sodium oleate
Sweeping: 90g/t of sodium oleate
TABLE 1 TEST 1# -7 # FULL FLOW CLOSED CIRCUIT COMPARATIVE TEST RESULTS/% (amended)
As can be seen from Table 1, the amount of gangue depressants and collectors was compared with that of water glass and collector under the same dosage conditionsAgent HQ-P2Combination (2 # in Table 1), inhibitor HQ-P1Combined with sodium oleate (No. 3 in Table 1), water glass and sodium oleate (No. 4 in Table 1), HQ-P1With HQ-P2The combination (1 # in Table 1) enables higher P2O5Grade and P2O5And (4) recovering rate. Changing HQ-P1When the phosphorus phase in the phosphate concentrate is obtained, the phosphorus recovery rate is reduced by 6.53 percent according to the mass ratio of the medium active components (5 # in table 1) and the comparative example 1 (1 # in table 1); changing HQ-P2When the phosphorus recovery rate in the phosphorus concentrate is comparable to that obtained in comparative example 1 (No. 1 in Table 1), the weight ratio of the medium active components (No. 6 in Table 1), and the phosphorus recovery rate are reduced by 4.13%, which shows that HQ-P used in example 11And HQ-P2The mass ratio of the active components is more suitable for selecting the low-grade vanadium titano-magnetite. In comparative example 6 (7#), the material with minus 0.038mm removed has the effect of improving the grade of the phosphate concentrate compared with comparative example 3(4#), but the phosphate grade of the phosphate concentrate is still lower than 35%, and the phosphorus content in the deslimed mud product is 38.73%, so that the loss is too large, and the problem of low grade of the phosphate concentrate cannot be solved by desliming. HQ-P described above1And HQ-P2The combination is an excellent phosphorus flotation medicament.
Example 2
Certain low grade vanadium titano-magnetite tailings, P, of Panzhihua2O5At 1.82% mineral content, the mineral composition is relatively complex, the main gangue minerals being quartz, calcite, dolomite and mica, with a relative mineral content of apatite of about 7% and calcite/dolomite of up to 16%. The fineness of the tailings is-74 mu m and accounts for 75%, and apatite and calcite/dolomite belong to fine particle embedded cloth and belong to low-grade refractory phosphorus-containing iron tailings.
The process flow of this example is shown in fig. 2, and the specific sorting process and the pharmaceutical system are as follows:
(1) firstly, carrying out low-intensity magnetic separation and tailing discarding on the tailings, wherein the magnetic field intensity is 0.35T, and obtaining nonmagnetic minerals (phosphorus flotation feeding);
(2) roughing operation: mixing the phosphorus flotation tailings, and stirring for 1 min; sequentially adding 3000g/t sodium carbonate, stirring for 2min, and adding 400g/t gangue inhibitor HQ-P1Stirring for 2min, and adding 300g/t of collecting agent HQ-P2Stirring for 2min, and scraping and soaking for 5.5min to obtain roughed concentrate and scavenging feed ore;
(3) primary scavenging operation: adding 100g/t of collecting agent HQ-P into scavenging feed ore2Stirring for 2min, and scraping and soaking for 2.5min to obtain final tailings;
(4) and (3) performing tertiary concentrate operation: and (3) blank concentration is carried out on the first concentration, the second concentration and the third concentration, and the foam scraping time is respectively 2.5min, 2min and 1.5min, so that the final phosphate concentrate is obtained.
The gangue inhibitor HQ-P1Respectively consists of water glass, carboxymethyl cellulose (CMC) and 2-carboxyl phosphoryl acetic acid (HPAA) with the mass ratio of 100:13: 39.
The collector HQ-P2Consists of sodium oleate and polyethanol monomethyl ether (MPEG-200) with the mass ratio of 92: 8.
The collector is prepared into 2.5% aqueous solution, and the gangue inhibitor is added into the aqueous solution with the mass concentration of 5%. The test results are shown in table 2 as # 8.
Comparative example 7
The process flow was the same as in example 2 except that the gangue depressants used were single water glass and the collector used was single sodium oleate. The flotation results are shown in table 2# 9.
Roughing: 400g/t of water glass and 300g/t of sodium oleate
Sweeping: 100g/t of sodium oleate
TABLE 2 results of the 8# to 9# full-run closed-circuit comparative experiments%
As shown in Table 2, HQ-P was used as a collector, compared with the conventional sodium silicate used as an inhibitor and sodium oleate used as a collector (9 # in Table 2)1And HQ-P2Combined action (8 # in Table 2), phosphorus concentrate P was obtained2O5The content is improved by 7.55 percent, and the phosphorus recovery rate is improved by 9.34 percent. The above results demonstrate HQ-P1And HQ-P2The combination is superiorGood phosphorus flotation agent.
Claims (10)
1. A method for selecting phosphorus from low-grade vanadium titano-magnetite tailings comprises the following steps:
1) magnetic separation: firstly, carrying out low-intensity magnetic separation and tailing discarding on low-grade vanadium-titanium magnetite tailings to obtain magnetic minerals and non-magnetic minerals;
2) flotation: mixing the nonmagnetic minerals obtained in the step 1) to obtain ore pulp, and sequentially adding a regulator sodium carbonate and a gangue inhibitor HQ-P into the ore pulp1HQ-P as collector2Performing direct flotation phosphorus separation to obtain high-quality phosphate concentrate and phosphate separation tailings;
wherein: HQ-P1The high-performance sodium silicate-sodium borate composite material is composed of water glass, carboxymethyl cellulose (CMC) and 2-carboxyl phosphoryl acetic acid (HPAA) in a mass ratio of 100 (10-15) to 20-45;
HQ-P2consists of 80-95 wt% and 5-20 wt% of sodium oleate and MPEG-200.
2. The method for separating phosphorus from low-grade vanadium titano-magnetite tailings according to claim 1, wherein in the step 1), the magnetic field strength of the low-intensity magnetic separation is 0.2-0.5T; in the step 2), the modulus of the water glass is 2.5-3.0; the molecular formula of the 2-carboxyl phosphoryl acetic acid HPAA is C2H5O6P, the structural formula is as follows:
the molecular formula of the polyethanol monomethyl ether MPEG-200 is C23H48O12The structural formula is as follows:
3. the method for selecting phosphorus from low-grade vanadium titano-magnetite tailings according to claim 1 or 2, characterized in that the gangue inhibitionAgent HQ-P1The high-performance sodium carboxymethyl cellulose sodium silicate-sodium carboxymethyl cellulose (CMC) and 2-carboxyphosphoryl acetic acid (HPAA) in a mass ratio of 100:12: 36.
4. The method for selecting phosphorus from low-grade vanadium titano-magnetite tailings according to claim 1 or 2, wherein the gangue inhibitor HQ-P1The high-performance sodium carboxymethyl cellulose sodium silicate-sodium carboxymethyl cellulose (CMC) and 2-carboxyphosphoryl acetic acid (HPAA) in a mass ratio of 100:13: 39.
5. The method for separating phosphorus from low-grade vanadium titano-magnetite tailings according to claim 1 or 2, wherein the collector HQ-P2Consists of sodium oleate and polyethanol monomethyl ether MPEG-200 with the mass ratio of 90: 10.
6. The method for separating phosphorus from low-grade vanadium titano-magnetite tailings according to claim 1 or 2, wherein the collector HQ-P2Consists of sodium oleate and polyethanol monomethyl ether MPEG-200 with the mass ratio of 92: 8.
7. The method for selecting phosphorus from low-grade vanadium titano-magnetite tailings according to claim 1 or 2, wherein the positive flotation phosphorus selection operation is one rough and three fine.
8. The method for selecting phosphorus from low-grade vanadium titano-magnetite tailings according to claim 7, wherein the primary roughing operation comprises the following specific steps: mixing the phosphorus flotation feed ore, adding 800-4000 g/t of sodium carbonate into the ore pulp, and stirring for 2-3 min; adding 200-600 g/t of gangue inhibitor HQ-P1Stirring for 2-3 min; adding 100-500 g/t of collecting agent HQ-P2Stirring for 2-3 min; and (4) scraping and soaking for 4-6 min to obtain rough concentrate, wherein the product in the tank is scavenging feed ore.
9. The method for selecting phosphorus from low-grade vanadium titano-magnetite tailings according to claim 7, wherein the specific steps of the primary scavenging operation are as follows: adding 30-200 g/t of collecting agent HQ-P2Stirring for 2-3 min, and scraping for 2-3 min to obtain scavenged foam product, returning the scavenged foam product to the roughing tank, wherein the product in the tank is the tailing product.
10. The method for selecting phosphorus from low-grade vanadium titano-magnetite tailings according to claim 7, wherein the three selection operations comprise the following specific steps: the first concentration, the second concentration and the third concentration are blank concentration, foam scraping is started after full stirring, the foam scraping time is 2-3 min, 1.5-2.5 min and 1.0-2 min respectively, and all middlings are returned to the previous flotation operation in sequence; and obtaining the final phosphate concentrate product.
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CN114453139A (en) * | 2022-02-28 | 2022-05-10 | 矿冶科技集团有限公司 | Beneficiation method for recycling extremely low-grade phosphorus minerals from iron dressing tailings of gangue minerals and application of beneficiation method |
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