CN108580023B - Multi-component recycling and beneficiation method for iron tailings associated with rare earth minerals - Google Patents
Multi-component recycling and beneficiation method for iron tailings associated with rare earth minerals Download PDFInfo
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Abstract
The invention relates to a multi-component recovery and beneficiation method for iron tailings associated with rare earth minerals, and belongs to the fields of mineral processing engineering and comprehensive resource recovery and utilization. The method comprises the following steps: carrying out mixed flotation on the rare earth minerals and fluorite minerals of the iron tailings associated with the rare earth minerals to obtain mixed flotation concentrate and mixed flotation tailings; performing strong magnetic separation on the bulk flotation concentrate at the magnetic field intensity of 0.4-1.0T to obtain strong magnetic separation concentrate and strong magnetic separation tailings; performing rare earth flotation on the strong magnetic separation concentrate to obtain rare earth flotation concentrate and rare earth flotation tailings; carrying out fluorite flotation on the strong magnetic separation tailings to obtain fluorite flotation concentrate and fluorite flotation tailings; and (3) dehydrating and drying the mixed flotation tailings, roasting in a reducing atmosphere, and performing low-intensity magnetic separation on the roasted minerals at 0.1-0.3T to obtain low-intensity magnetic concentrate and low-intensity magnetic tailings. The method of the invention is utilized to finally obtain three concentrates of rare earth concentrate, fluorite concentrate and iron concentrate and niobium-rich slag, thereby improving the comprehensive utilization rate of the iron tailings of associated rare earth minerals.
Description
Technical Field
The invention relates to a multi-component recovery and beneficiation method for iron tailings associated with rare earth minerals, and belongs to the fields of mineral processing engineering and comprehensive resource recovery and utilization.
Background
The iron ore associated with rare earth minerals is represented by bayan obo iron ore which is rich in rare earth, iron, niobium, fluorite and other minerals. The utilization of the bayan obo iron ore is limited to the recovery of iron and partial rare earth, so that useful minerals such as iron, rare earth, fluorite and the like with considerable reserves are still stored in a tailing pond, the recovery rate of the minerals such as iron, rare earth, fluorite and the like in the bayan obo ore dressing plant is not ideal at present, a large amount of useful minerals are continuously piled into the tailing pond, and thus, the waste of resources is more serious and the damage to the environment is further aggravated.
The rare earth ore content in the bayan obo tailing pond is about 7 percent, the iron mineral content is about 15 percent, the fluorite content is about 25 percent, the floatability and magnetism of the minerals are close to those of gangue minerals, and the minerals are difficult to separate by a conventional method, especially the iron minerals. The iron minerals in the tailings are mainly hematite, contain iron silicate and iron sulfide, and the minerals and the spodumene, the amphibole and the biotite in the gangue belong to weakly magnetic minerals, so that the minerals and the diopside, the amphibole and the biotite easily enter strong magnetic concentrates in strong magnetic operation, and the iron minerals are lost into the tailings and are not fully utilized. The fluorite in the tailings is complex in mineralization, the associated fluorite ore has fine embedded granularity, is mostly in a strip shape and a dip-dyeing shape, and has low fluorite grade and multiple associated mineral types. The fluorite entering the tailings is often wrapped with inclusions of other minerals, and most of the fluorite entering the concentrate of the conventional process exists in intergrowth and mainly intergrowth with lean ores of iron minerals, so that the grade of the iron concentrate is reduced, and the impurity content of the iron concentrate is increased. The rare earth minerals are similar to weakly magnetic minerals such as hematite and the like in magnetism, but similar to gangue minerals such as fluorite and the like in flotability, so that the rare earth minerals are difficult to efficiently select, and by combining the factors, the iron tailings similar to the associated rare earth minerals of the bayan obo tailings can be regarded as more difficultly-selected multi-metal associated iron ore resources, and the comprehensive utilization significance of the iron tailings is great.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a beneficiation method for recovering iron, rare earth, fluorite and niobium from iron tailings of associated rare earth minerals. The invention aims to solve the problem of comprehensive utilization of the iron tailings of the associated rare earth minerals, fully utilize the useful resources in the iron tailings of the associated rare earth minerals, improve the recovery rate of the useful minerals in the existing flow and provide a new path for comprehensive recovery of the valuable elements in the iron tailings of the associated rare earth minerals.
A multi-component recovery beneficiation method for iron tailings associated with rare earth minerals comprises the following steps: carrying out mixed flotation of rare earth minerals and fluorite minerals on iron tailings associated with the rare earth minerals to obtain mixed flotation concentrate and mixed flotation tailings; performing strong magnetic separation on the bulk flotation concentrate at the magnetic field intensity of 0.4-1.0T to obtain strong magnetic separation concentrate and strong magnetic separation tailings; performing rare earth flotation on the strong magnetic concentrate weak magnetic tailings to obtain rare earth flotation concentrates and rare earth flotation tailings; carrying out fluorite flotation on the strong magnetic separation tailings to obtain fluorite flotation concentrate and fluorite flotation tailings; dehydrating and drying the mixed flotation tailings, and roasting the mixed flotation tailings in a reducing atmosphere at the roasting temperature of 500-900 ℃ to ensure that the weakly magnetic hematite (limonite) undergoes a reduction reaction and is converted into strongly magnetic iron minerals; and carrying out low-intensity magnetic separation on the roasted minerals at 0.1-0.3T to obtain low-intensity magnetic concentrates and low-intensity magnetic tailings, wherein the low-intensity magnetic concentrates are iron concentrate products after dehydration.
The invention provides a multi-component recycling and beneficiation method for iron tailings associated with rare earth minerals, and particularly relates to a beneficiation method for recycling iron, rare earth, fluorite and niobium from the iron tailings associated with the rare earth minerals, wherein the iron tailings associated with the rare earth minerals are used as raw materials, the fluorite and the rare earth minerals are enriched through mixed flotation, then the obtained mixed flotation concentrate is subjected to strong magnetic separation to separate the rare earth minerals and the fluorite, and on the basis, flotation and concentration operations of the rare earth minerals and the fluorite are carried out to respectively obtain rare earth flotation concentrate (the grade of the rare earth concentrate is not less than 65%, the recovery rate of the rare earth is not less than 75%) and fluorite flotation concentrate (the grade of the fluorite concentrate is not less than 90%, and the recovery rate of the fluori. And roasting the mixed flotation tailings, wherein the reduction reaction of hematite and limonite can be converted into strong-magnetic iron minerals in the roasting process, and the obtained roasted ores are subjected to low-intensity magnetic separation to obtain low-intensity magnetic concentrates (the grade TFe of the iron concentrates is more than or equal to 62 percent, and the iron recovery rate is more than or equal to 70 percent) and low-intensity magnetic tailings, and the low-intensity magnetic tailings are used for further selecting niobium.
The ferromagnetic iron mineral is Fe3O4Or gamma-Fe2O3Or a mixture of both.
The iron tailings associated with the rare earth minerals are tailings obtained by iron selection of bayan obo iron ore or tailings of a bayan obo tailing pond, wherein the grade of iron (TFe) is 10 to20% fluorite (CaF)2) The grade is 20-35%, and the grade of Rare Earth (REO) is 5-10%.
The low-intensity magnetic separation of the present invention is carried out in commercially available low-intensity magnetic separators, such as wet permanent magnet drum separators.
The high-intensity magnetic separation is carried out in a commercially available strong magnetic separator, such as a vertical ring wet strong magnetic separator.
The invention relates to a method for classifying and grinding mixed flotation tailings after dehydration and drying.
The classification step may be carried out in a commercially available classification apparatus, such as one of a spiral classifier, a hydrocyclone; the milling can be carried out in commercially available mills, such as ball mills, stirred mills.
The roasting of the present invention is carried out in a commercially available fluidized roaster, such as one of a flash magnetic roaster, a circulating fluidized roaster, and a suspension magnetic roaster. The grinding is as follows: grinding the mixture of the weak magnetic pre-enriched concentrate and the strong magnetic pre-enriched concentrate until the particles with the particle size of-44 mu m account for 60-95 wt% of the total material.
The acid wash of the present invention is carried out in a commercially available reaction vessel, such as an autoclave.
The solid-liquid separation of the present invention is carried out in commercially available filters, such as ceramic filters.
According to the multi-component recovery beneficiation method for the iron tailings associated with the rare earth minerals, preferably, the reducing atmosphere is provided by a mixed gas of reducing gas and inert gas, wherein the volume ratio of the reducing gas to the inert gas is 1: 9-1: 1, the total gas flow is 3m3/h～10m3The reducing gas is CO and H2Or a mixture of the two in any proportion.
The multi-component recovery beneficiation method for the iron tailings associated with the rare earth minerals further comprises the step of selecting niobium, and specifically comprises the following steps: and (3) acid-washing the weak-magnetic tailings to obtain niobium-rich slag and acid-washed tailings.
According to the multi-component recovery beneficiation method for the iron tailings associated with the rare earth minerals, the acid washing is preferably as follows: acid washing is carried out on the weak magnetic tailings in a high-pressure reaction kettle by using 6-10 mol/L hydrochloric acid solution, and solid-liquid separation is carried out by using a filter, so that acid-leached residues, namely niobium-enriched residues and final tailings are obtained.
The invention discloses a multi-component recovery beneficiation method for iron tailings associated with rare earth minerals, which preferably comprises the following steps: mixing iron tailings associated with rare earth minerals into slurry, performing mixed flotation operation, adding an inhibitor, a collecting agent and an adjusting agent to respectively obtain mixed flotation concentrate and mixed flotation tailings,
wherein the inhibitor is water glass, and the dosage of the inhibitor is 0.20-0.80 kg/t; the collecting agent is sodium oleate, and the dosage of the collecting agent is 0.20-0.55 kg/t; the regulator is sodium carbonate, and the dosage of the regulator is 0.30-0.80 kg/t.
According to the multi-component recovery beneficiation method for the iron tailings associated with the rare earth minerals, the rare earth flotation is preferably as follows: concentrating the strongly-magnetic concentrate, then mixing the concentrated concentrate with pulp, feeding the concentrated concentrate into a flotation machine for rare earth concentration operation, adding an inhibitor, a rare earth mineral activating agent, a collecting agent and a foaming agent, adjusting the pH to 7-8, performing rare earth mineral flotation operation, and after rough concentration, performing concentration and scavenging for 1-3 times to obtain rare earth concentrate; finally obtaining rare earth flotation concentrate and rare earth flotation tailings,
wherein the inhibitor is oxalic acid, and the dosage of the inhibitor is 0.15-0.40 kg/t; the rare earth mineral activating agent is sodium fluosilicate, and the dosage of the sodium fluosilicate is 1.00-3.00 kg/t; the collecting agent is salicylhydroxamic acid or H316The dosage of the additive is 0.70-0.12 kg/t; the foaming agent is second oil, and the dosage of the second oil is 0.02-0.05 kg/t.
According to the multi-component recovery beneficiation method for the iron tailings associated with the rare earth minerals, the fluorite flotation is preferably as follows: concentrating the strong magnetic tailings, mixing the pulp, feeding the pulp into a flotation machine for fluorite flotation operation, adding an inhibitor and a collecting agent, floating fluorite, performing 1-3 times of fine concentration and scavenging after rough concentration to obtain fluorite concentrate,
wherein the inhibitor is water glass, and the dosage of the inhibitor is 0.15-0.40 kg/t; the collecting agent is sodium oleate, and the dosage of the collecting agent is 0.20-0.40 kg/t.
The invention relates to a multi-component recovery beneficiation method for iron tailings associated with rare earth minerals, which adopts a preferable technical scheme that: the method comprises the following process steps:
(1) and (3) mixed flotation: mixing iron tailings associated with rare earth minerals into slurry, performing mixed flotation operation of the rare earth minerals and fluorite minerals, and adding an inhibitor, a collecting agent and an adjusting agent to respectively obtain mixed flotation concentrate and mixed flotation tailings;
(2) strong magnetic separation: performing strong magnetic separation on the bulk flotation concentrate obtained in the step (1) at the magnetic field intensity of 0.4-1.0T to obtain strong magnetic separation concentrate and strong magnetic separation tailings;
(3) rare earth flotation: performing rare earth flotation on the strong magnetic concentrate weak magnetic tailings obtained in the step (2) to obtain rare earth flotation concentrates and rare earth flotation tailings;
(4) fluorite flotation: carrying out fluorite flotation on the strong magnetic separation tailings obtained in the step (2) to obtain fluorite flotation concentrate and fluorite flotation tailings;
(5) fluidized magnetic roasting: dehydrating and drying the mixed flotation tailings obtained in the step (1), dehydrating the obtained pre-enriched concentrate with qualified granularity, and then carrying out fluidized magnetic roasting in a reducing atmosphere, wherein the reducing atmosphere is provided by a mixed gas of a reducing gas and an inert gas, the volume ratio of the reducing gas to the inert gas is 1: 9-1: 1, and the total gas flow is 3m3/h～10m3The reducing gas is CO and H2Or mixing the two in any proportion, and roasting at the roasting temperature of 500-900 ℃ for 8-35 s to obtain roasted ore;
(6) performing low-intensity magnetic separation: carrying out low-intensity magnetic separation on the roasted minerals at 0.1-0.3T to obtain low-intensity magnetic concentrate and low-intensity magnetic tailings, wherein the low-intensity magnetic concentrate is an iron concentrate product after dehydration, and the low-intensity magnetic tailings can be used for selecting niobium through acid washing;
(7) acid washing: pickling the weak magnetic tailings obtained in the step (6) in a high-pressure reaction kettle with 6-10 mol/L hydrochloric acid solution, and performing solid-liquid separation by using a ceramic filter after pickling to obtain acid leaching residues, namely niobium-enriched residues and pickled tailings;
the invention has the beneficial effects that: according to the method, the fluorite and the rare earth minerals are pre-enriched by adopting the mixed flotation, so that the subsequent roasted ore amount is reduced, the contents of fluorine and other harmful elements in the roasted ore are reduced, the pollution is reduced, the roasting furnace is protected, in addition, the energy consumption is reduced, and the concentrate quality is improved; the rare earth flotation difficulty can be reduced by pre-enriching the rare earth minerals by using strong magnetic separation; the iron ore is treated by a fluidized roasting method, so that the content of harmful impurities in the iron ore concentrate is reduced, the iron ore concentrate is uniform in product, and the grade and the recovery rate of the iron ore concentrate are increased while the iron ore concentrate is easy to select. The method is utilized to finally obtain three concentrates of rare earth concentrate, fluorite concentrate and iron concentrate and niobium-rich slag, so that the comprehensive utilization rate of the iron tailings of associated rare earth minerals is improved.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
In the example, tailings in a bayan obo tailing pond are used as raw materials, wherein the grade of iron (TFe) is 15.62%, and fluorite (CaF)2) The grade is 19.30 percent, and the grade of Rare Earth (REO) is 6.87 percent. The method of the invention is utilized to finally obtain the fluorite concentrate with the fluorite grade of 95.26% and the recovery rate of 82.23%; rare earth concentrate with rare earth grade of 66.54% and recovery rate of 83.12%; iron ore concentrate with iron grade of 64.89% and recovery rate of 87.65%; the method specifically comprises the following steps:
(1) after tailings in the bayan obo tailing pond are subjected to size mixing, mixed flotation operation is carried out, 0.50kg/t of water glass of an inhibitor, 0.35kg/t of sodium oleate of a collecting agent and 0.50kg/t of sodium carbonate of a regulator are added, and mixed flotation concentrate and mixed flotation tailings are obtained respectively.
(2) And (2) feeding the mixed flotation concentrate obtained in the step (1) into a strong magnetic separator, wherein the intensity of a strong magnetic field is 0.75T, and obtaining strong magnetic flotation concentrate and strong magnetic flotation tailings respectively.
(3) Concentrating the strong magnetic separation concentrate obtained in the step (2), then mixing the concentrated concentrate with slurry, feeding the concentrate into a flotation machine for rare earth flotation operation, adding 0.30kg/t oxalic acid as an inhibitor, 2.00kg/t sodium fluosilicate as an activator, 0.85kg/t salicylhydroxamic acid as a collector and 0.04kg/t second oil as a foaming agent, adjusting the pH to 7.5, performing rare earth mineral flotation operation, and performing 3 times of fine separation and 1 time of scavenging separation after rough separation to obtain rare earth concentrate; finally obtaining rare earth flotation concentrate and rare earth flotation tailings;
(4) concentrating the strong magnetic tailings in the step (2), mixing the concentrated strong magnetic tailings, feeding the concentrated strong magnetic tailings into a flotation machine for fluorite flotation operation, adding 0.25kg/t of sodium silicate of an inhibitor and 0.30kg/t of sodium oleate of a collecting agent, floating fluorite, and performing 2 times of fine concentration and 1 time of scavenging after rough concentration to obtain fluorite flotation concentrate and fluorite flotation tailings;
(5) dehydrating the mixed flotation tailings obtained in the step (1), and then using N with the volume ratio of 7:32The gas and CO gas are mixed and used as carrier gas, and the total gas flow is 5m3The roasted ore is obtained by roasting in a suspension magnetization roasting furnace for 25s at the reduction roasting temperature of 600 ℃;
(6) cooling the roasted ore obtained in the step (5), introducing a low-intensity magnetic separator with the magnetic field intensity of 0.25T for separation to respectively obtain low-intensity magnetic concentrate and low-intensity magnetic tailings, and dehydrating the low-intensity magnetic concentrate to obtain an iron concentrate product;
(7) and (4) carrying out acid washing on the weak magnetic tailings obtained in the step (6) in a high-pressure reaction kettle with 7.5mol/L hydrochloric acid solution, and carrying out solid-liquid separation by using a ceramic filter after acid washing to obtain acid-leached residues, namely niobium-enriched residues and acid-washed tailings.
Example 2
In the example, tailings in a bayan obo tailing pond are used as raw materials, wherein the grade of iron (TFe) is 13.47%, and fluorite (CaF)2) The grade is 22.45 percent, and the grade of Rare Earth (REO) is 6.56 percent. By utilizing the method, the fluorite concentrate with the fluorite grade of 96.46 percent and the recovery rate of 80.26 percent is finally obtained; rare earth concentrate with the rare earth grade of 63.58% and the recovery rate of 87.26%; iron ore concentrate with the iron grade of 63.69 percent and the recovery rate of 86.76 percent; the method specifically comprises the following steps:
(1) after tailings in the bayan obo tailing pond are subjected to size mixing, mixed flotation operation is carried out, 0.45kg/t of water glass of an inhibitor, 0.45kg/t of sodium oleate of a collecting agent and 0.40kg/t of sodium carbonate of a regulator are added, and mixed flotation concentrate and mixed flotation tailings are obtained respectively.
(2) And (2) feeding the mixed flotation concentrate obtained in the step (1) into a strong magnetic separator, wherein the intensity of a strong magnetic field is 0.80T, and obtaining strong magnetic flotation concentrate and strong magnetic flotation tailings respectively.
(3) Concentrating the strong magnetic separation concentrate in the step (2), mixing the concentrated concentrate with slurry, feeding the concentrate into a flotation machine for rare earth flotation operation, and adding 0.30kg/t oxalic acid of an inhibitor, 1.80kg/t sodium fluosilicate of an activator and 0.95kg/t H of a collector316Adjusting the pH of No. two oil with 0.04kg/t of rare earth flotation foaming agent to 7.8, performing flotation operation on rare earth minerals, and performing 2 times of fine concentration and 1 time of scavenging after rough concentration to obtain rare earth concentrates; finally obtaining rare earth flotation concentrate and rare earth flotation tailings;
(4) concentrating the strong magnetic tailings in the step (2), mixing the concentrated strong magnetic tailings, feeding the concentrated strong magnetic tailings into a flotation machine for fluorite flotation operation, adding 0.25kg/t of water glass of an inhibitor and 0.3kg/t of sodium oleate of a collecting agent, floating fluorite, and performing 2 times of fine concentration and 1 time of scavenging after rough concentration to obtain fluorite flotation concentrate and fluorite flotation tailings;
(5) dehydrating the mixed flotation tailings obtained in the step (1), and then using N with the volume ratio of 7:32The gas and CO gas are mixed and used as carrier gas, and the total gas flow is 6m3Roasting for 30s in a flash magnetic roasting furnace at the reduction roasting temperature of 650 ℃ to obtain roasted ore;
(6) cooling the roasted ore obtained in the step (5), introducing a low-intensity magnetic separator with the magnetic field intensity of 0.25T for separation to respectively obtain low-intensity magnetic concentrate and low-intensity magnetic tailings, and dehydrating the low-intensity magnetic concentrate to obtain an iron concentrate product;
(7) and (4) carrying out acid washing on the weak magnetic tailings obtained in the step (6) in a high-pressure reaction kettle with 8.5mol/L hydrochloric acid solution, and carrying out solid-liquid separation by using a ceramic filter after acid washing to obtain acid-leached residues, namely niobium-enriched residues and acid-washed tailings.
Example 3
In the example, tailings in a bayan obo tailing pond are used as raw materials, wherein the grade of iron (TFe) is 15.62%, and fluorite (CaF)2) The grade is 19.30 percent, and the grade of Rare Earth (REO) is 6.87 percent. The fluorite grade finally obtained by the method is 95.26 percent, and the recovery rate is 82.23 percentThe fluorite concentrate; rare earth concentrate with rare earth grade of 66.54% and recovery rate of 83.12%; iron ore concentrate with iron grade of 64.89% and recovery rate of 87.65%; the method specifically comprises the following steps:
(1) after tailings in the bayan obo tailing pond are subjected to size mixing, mixed flotation operation is carried out, 0.50kg/t of water glass of an inhibitor, 0.35kg/t of sodium oleate of a collecting agent and 0.50kg/t of sodium carbonate of an adjusting agent are added, and mixed flotation concentrate and mixed flotation tailings are obtained respectively.
(2) And (2) feeding the mixed flotation concentrate obtained in the step (1) into a strong magnetic separator, wherein the intensity of a strong magnetic field is 0.75T, and obtaining strong magnetic flotation concentrate and strong magnetic flotation tailings respectively.
(3) Concentrating the strong magnetic separation concentrate obtained in the step (2), mixing the concentrated strong magnetic separation concentrate with slurry, feeding the concentrated strong magnetic separation concentrate into a flotation machine for rare earth flotation, adding 0.30kg/t oxalic acid as an inhibitor, 2.10kg/t sodium fluosilicate as an activator, 0.85kg/t salicylhydroxamic acid as a collector and 0.04kg/t second oil as a rare earth flotation foaming agent, adjusting the pH to 7.5, performing flotation of rare earth minerals, and performing 3 times of fine separation and 1 time of scavenging separation after rough separation to obtain rare earth concentrate; finally obtaining rare earth flotation concentrate and rare earth flotation tailings;
(4) concentrating the strong magnetic tailings in the step (2), mixing the concentrated strong magnetic tailings, feeding the concentrated strong magnetic tailings into a flotation machine for fluorite flotation operation, adding 0.25kg/t water glass of an inhibitor and 0.30kg/t sodium oleate of a collecting agent, floating fluorite, and performing 2 times of fine concentration and 1 time of scavenging after roughing to obtain fluorite flotation concentrate and fluorite flotation tailings;
(5) dehydrating the mixed flotation tailings obtained in the step (1), and then using N with the volume ratio of 8:22Gas and H2The gas mixture is used as carrier gas, and the total gas flow is 7m3Roasting for 20s in a circulating fluidized roasting furnace at the roasting temperature of 650 ℃ to obtain roasted ore;
(6) cooling the roasted ore obtained in the step (5), introducing a low-intensity magnetic separator with the magnetic field intensity of 0.25T for separation to respectively obtain low-intensity magnetic concentrate and low-intensity magnetic tailings, and dehydrating the low-intensity magnetic concentrate to obtain an iron concentrate product;
(7) and (4) carrying out acid washing on the weak magnetic tailings obtained in the step (6) in a high-pressure reaction kettle with 7.5mol/L hydrochloric acid solution, and carrying out solid-liquid separation by using a ceramic filter after acid washing to obtain acid-leached residues, namely niobium-enriched residues and acid-washed tailings.
Example 4
In the example, the site iron tailings in the Baiyunebo selection plant are used as raw materials, wherein the grade of iron (TFe) is 9.87%, and fluorite (CaF)2) The grade is 18.20%, and the grade of Rare Earth (REO) is 5.93%. By utilizing the method, the fluorite concentrate with the fluorite grade of 95.43 percent and the recovery rate of 80.09 percent is finally obtained; rare earth concentrate with rare earth grade of 65.76% and recovery rate of 80.32%; iron ore concentrate with the iron grade of 65.74 percent and the recovery rate of 85.21 percent; the method specifically comprises the following steps:
(1) mixing the bayan obo iron tailings, performing mixed flotation, adding 0.60kg/t of water glass as an inhibitor, 0.40kg/t of sodium oleate as a collecting agent and 0.45kg/t of sodium carbonate as an adjusting agent to obtain mixed flotation concentrate and mixed flotation tailings respectively.
(2) And (2) feeding the mixed flotation concentrate obtained in the step (1) into a strong magnetic separator, wherein the intensity of a strong magnetic field is 0.80T, and obtaining strong magnetic flotation concentrate and strong magnetic flotation tailings respectively.
(3) Concentrating the strong magnetic separation concentrate in the step (2), then mixing the concentrated concentrate with slurry, feeding the concentrate into a flotation machine for rare earth flotation operation, adding 0.35kg/t oxalic acid as an inhibitor, 2.00kg/t sodium fluosilicate as an activator, 0.85kg/t salicylhydroxamic acid as a collector and 0.04kg/t second oil as a rare earth flotation foaming agent, adjusting the pH to 7.6, performing flotation operation on rare earth minerals, and performing 3 times of fine separation and 2 times of scavenging after rough separation to obtain rare earth concentrate; finally obtaining rare earth flotation concentrate and rare earth flotation tailings;
(4) concentrating the strong magnetic tailings in the step (2), mixing the concentrated strong magnetic tailings, feeding the concentrated strong magnetic tailings into a flotation machine for fluorite flotation operation, adding 0.30kg/t of sodium silicate of an inhibitor and 0.35kg/t of sodium oleate of a collecting agent, floating fluorite, and performing 3 times of fine concentration and 2 times of scavenging after rough concentration to obtain fluorite flotation concentrate and fluorite flotation tailings;
(5) dehydrating the mixed flotation tailings obtained in the step (1), and then using N with the volume ratio of 7:32The gas and CO gas are mixed and used as carrier gas, and the total gas flow is 7m3The mixture is roasted for 18s in a suspension magnetization roasting furnace at the reduction roasting temperature of 700 ℃ to obtain roasted ore;
(6) cooling the roasted ore obtained in the step (5), introducing a low-intensity magnetic separator with the magnetic field intensity of 0.25T for separation to respectively obtain low-intensity magnetic concentrate and low-intensity magnetic tailings, and dehydrating the low-intensity magnetic concentrate to obtain an iron concentrate product;
(7) and (4) carrying out acid washing on the weak magnetic tailings obtained in the step (6) in a high-pressure reaction kettle with 6.5mol/L hydrochloric acid solution, and carrying out solid-liquid separation by using a ceramic filter after acid washing to obtain acid-leached residues, namely niobium-enriched residues and acid-washed tailings.
Claims (7)
1. A multi-component recovery beneficiation method for iron tailings associated with rare earth minerals is characterized by comprising the following steps: the method comprises the following steps: carrying out mixed flotation of rare earth minerals and fluorite minerals on iron tailings associated with the rare earth minerals to obtain mixed flotation concentrate and mixed flotation tailings; carrying out strong magnetic separation on the bulk flotation concentrate under the condition that the magnetic field intensity is 0.4-1.0T to obtain strong magnetic separation concentrate and strong magnetic separation tailings; performing rare earth flotation on the strong magnetic separation concentrate to obtain rare earth flotation concentrate and rare earth flotation tailings; carrying out fluorite flotation on the strong magnetic separation tailings to obtain fluorite flotation concentrate and fluorite flotation tailings; dehydrating and drying the mixed flotation tailings, and roasting the mixed flotation tailings in a reducing atmosphere at the roasting temperature of 500-900 ℃ to enable the weakly magnetic hematite and limonite to undergo a reduction reaction and be converted into strongly magnetic iron minerals; carrying out low-intensity magnetic separation on the roasted minerals at 0.1-0.3T to obtain low-intensity magnetic concentrates and low-intensity magnetic tailings, wherein the low-intensity magnetic concentrates are iron concentrate products after dehydration; and (3) acid-washing the weak-magnetic tailings to obtain niobium-rich slag and acid-washed tailings.
2. The method of claim 1, wherein: the mixed flotation comprises the following steps: and (3) mixing the iron tailings associated with the rare earth minerals into slurry, performing mixed flotation operation of the rare earth minerals and the fluorite minerals, and adding an inhibitor, a collecting agent and an adjusting agent to respectively obtain mixed flotation concentrate and mixed flotation tailings.
Wherein the inhibitor is water glass, and the dosage of the inhibitor is 0.20-0.80 kg/t; the collecting agent is sodium oleate, and the dosage of the collecting agent is 0.20-0.55 kg/t; the regulator is sodium carbonate, and the dosage of the regulator is 0.30-0.80 kg/t.
3. The method of claim 1, wherein: the rare earth flotation comprises the following steps: concentrating the strongly-magnetic concentrate, then mixing the concentrated concentrate with pulp, feeding the concentrated concentrate into a flotation machine for rare earth concentration operation, adding a gangue mineral inhibitor, a rare earth mineral activating agent, a collecting agent and a foaming agent, adjusting the pH value to 7-8, performing rare earth mineral flotation operation, and after rough concentration, performing concentration and scavenging for 1-3 times to obtain rare earth concentrate; finally obtaining rare earth flotation concentrate and rare earth flotation tailings,
wherein the gangue mineral inhibitor is oxalic acid, and the dosage of the oxalic acid is 0.15-0.40 kg/t; the rare earth mineral activating agent is sodium fluosilicate, and the dosage of the sodium fluosilicate is 1.00-3.00 kg/t; the collecting agent is salicylhydroxamic acid or H316The dosage of the additive is 0.70-1.20 kg/t; the foaming agent is second oil, and the dosage of the second oil is 0.02-0.05 kg/t.
4. The method of claim 1, wherein: the reducing atmosphere is provided by a mixed gas of a reducing gas and an inert gas, wherein the volume ratio of the reducing gas to the inert gas is 1: 9-1: 1, and the total gas flow is 3m3/h～10m3The reducing gas is CO and H2Or a mixture of the two in any proportion.
5. The method of claim 1, wherein: the fluorite flotation comprises the following steps: concentrating the strong magnetic tailings, mixing the pulp, feeding the pulp into a flotation machine for fluorite flotation operation, adding gangue mineral inhibitor and collecting agent, floating fluorite, performing 1-3 times of fine concentration and scavenging after rough concentration to obtain fluorite concentrate,
wherein the inhibitor is water glass, and the dosage of the inhibitor is 0.15-0.40 kg/t; the collecting agent is sodium oleate, and the dosage of the collecting agent is 0.20-0.40 kg/t.
6. The method of claim 1, wherein: the acid washing comprises the following steps: acid washing is carried out on the weak magnetic tailings and 6-10 mol/L hydrochloric acid solution in a high-pressure reaction kettle, solid-liquid separation is carried out by using a ceramic filter, and acid-leaching residues, namely niobium-enriched residues and acid-washing tailings, are obtained.
7. The method of claim 1, wherein: the method comprises the following process steps:
(1) and (3) mixed flotation: mixing iron tailings associated with rare earth minerals into slurry, performing mixed flotation, and adding an inhibitor, a collecting agent and an adjusting agent to respectively obtain mixed flotation concentrate and mixed flotation tailings;
(2) strong magnetic separation: performing strong magnetic separation on the bulk flotation concentrate obtained in the step (1) at the magnetic field intensity of 0.4-1.0T to obtain strong magnetic separation concentrate and strong magnetic separation tailings;
(3) rare earth flotation: performing rare earth flotation on the strong magnetic separation concentrate obtained in the step (2) to obtain rare earth flotation concentrate and rare earth flotation tailings;
(4) fluorite flotation: carrying out fluorite flotation on the strong magnetic separation tailings obtained in the step (2) to obtain fluorite flotation concentrate and fluorite flotation tailings;
(5) fluidized magnetic roasting: dehydrating and drying the mixed flotation tailings obtained in the step (1), and then carrying out fluidized magnetic roasting in a reducing atmosphere, wherein the reducing atmosphere is provided by a mixed gas of a reducing gas and an inert gas, the volume ratio of the reducing gas to the inert gas is 1: 9-1: 1, and the total gas flow is 3m3/h～10m3The reducing gas is CO and H2Or mixing the two in any proportion, and roasting at the roasting temperature of 500-900 ℃ for 8-35 s to obtain roasted ore;
(6) performing low-intensity magnetic separation: carrying out low-intensity magnetic separation on the roasted minerals at 0.1-0.3T to obtain low-intensity magnetic concentrates and low-intensity magnetic tailings, wherein the low-intensity magnetic concentrates are iron concentrate products after dehydration;
(7) acid washing: and (4) carrying out acid washing on the weak magnetic tailings obtained in the step (6) in a high-pressure reaction kettle with 6-10 mol/L hydrochloric acid solution, and carrying out solid-liquid separation by using a ceramic filter after acid washing to obtain acid-leached residues, namely niobium-enriched residues and acid-washed tailings.
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| CN114570531A (en) * | 2022-01-25 | 2022-06-03 | 贵州省新材料研究开发基地 | Flotation separation method for low-grade carbonate fluorite ore |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60238173A (en) * | 1984-05-12 | 1985-11-27 | Kobe Steel Ltd | Flotation of rare earth mineral |
| CN101348860A (en) * | 2008-09-01 | 2009-01-21 | 武汉理工大学 | Production method of porous active magnetite |
| CN102168173A (en) * | 2011-03-29 | 2011-08-31 | 内蒙古科技大学 | Method for extracting niobium from tailings |
| CN102994738A (en) * | 2012-12-06 | 2013-03-27 | 内蒙古科技大学 | Method for preparing niobium-enriched ore by employing X-fluorescence sorting-microwave carbon thermal reduction |
| CN103394408A (en) * | 2013-07-26 | 2013-11-20 | 北京科技大学 | Method for comprehensively recycling valuable minerals in rare-earth tailings |
| CN103831173A (en) * | 2014-03-17 | 2014-06-04 | 内蒙古包钢钢联股份有限公司 | Technique of improving rare earth recovery rate and fluorite grade in tailings |
| CN106636614A (en) * | 2017-01-17 | 2017-05-10 | 东北大学 | Method for leaching niobium, scandium and rare earth elements from tailings |
| CN107282288A (en) * | 2017-05-26 | 2017-10-24 | 内蒙古科技大学 | A kind of beneficiation method of synthetical recovery weak magnetism, rare earth and fluorite |
| CN107523662A (en) * | 2017-08-16 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of method that metallic iron in rich iron tailings is reclaimed in fluidization |
-
2018
- 2018-04-19 CN CN201810355216.8A patent/CN108580023B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60238173A (en) * | 1984-05-12 | 1985-11-27 | Kobe Steel Ltd | Flotation of rare earth mineral |
| CN101348860A (en) * | 2008-09-01 | 2009-01-21 | 武汉理工大学 | Production method of porous active magnetite |
| CN102168173A (en) * | 2011-03-29 | 2011-08-31 | 内蒙古科技大学 | Method for extracting niobium from tailings |
| CN102994738A (en) * | 2012-12-06 | 2013-03-27 | 内蒙古科技大学 | Method for preparing niobium-enriched ore by employing X-fluorescence sorting-microwave carbon thermal reduction |
| CN103394408A (en) * | 2013-07-26 | 2013-11-20 | 北京科技大学 | Method for comprehensively recycling valuable minerals in rare-earth tailings |
| CN103831173A (en) * | 2014-03-17 | 2014-06-04 | 内蒙古包钢钢联股份有限公司 | Technique of improving rare earth recovery rate and fluorite grade in tailings |
| CN106636614A (en) * | 2017-01-17 | 2017-05-10 | 东北大学 | Method for leaching niobium, scandium and rare earth elements from tailings |
| CN107282288A (en) * | 2017-05-26 | 2017-10-24 | 内蒙古科技大学 | A kind of beneficiation method of synthetical recovery weak magnetism, rare earth and fluorite |
| CN107523662A (en) * | 2017-08-16 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of method that metallic iron in rich iron tailings is reclaimed in fluidization |
Non-Patent Citations (1)
| Title |
|---|
| 白云鄂博稀土尾矿多组分综合回收工艺及耦合关系研究;张悦;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20170731;第46-49页 * |
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