CN103468948B - Method for comprehensive recycling of metals from scandium-containing cobalt nickel hydroxide - Google Patents
Method for comprehensive recycling of metals from scandium-containing cobalt nickel hydroxide Download PDFInfo
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Abstract
Provided is a method for comprehensive recycling of metals from scandium-containing cobalt nickel hydroxide. The invention discloses a treatment method of the scandium-containing cobalt nickel hydroxide. The treatment method includes the steps: carrying out first leaching treatment of the cobalt nickel hydroxide precipitation by sulfuric acid, so as to obtain a nickel cobalt leaching solution; carrying out scandium extraction treatment of the nickel cobalt leaching solution by an organic extractant, so as to obtain a nickel-cobalt-containing solution and a scandium-containing organic phase; recycling nickel cobalt from the nickel-cobalt-containing solution; and recycling scandium from the scandium-containing organic phase. With the utilization of the method, scandium and nickel cobalt can be effectively extracted from the scandium-containing cobalt nickel hydroxide precipitation.
Description
Technical field
The present invention relates to field of metallurgy.Specifically, the present invention relates to the method containing scandium nickel hydroxide cobalt synthetical recovery metal.
Background technology
Containing a large amount of nickel cobalt metal elements in red soil nickel ore, because the nickel cobalt grade of domestic red soil nickel ore is lower, therefore China is for the production of the red soil nickel ore raw material of nickel cobalt mainly from external import, and its raw materials cost is higher.The domestic process to red soil nickel ore in the past is just confined to, to the extraction of wherein nickel cobalt, have ignored other a small amount of valuable metal elements contained in red soil nickel ore.To present invention finds in red soil nickel ore also containing a small amount of scandium element, but content is less, not easily extracts, the rate of recovery is low.The foreign matter contents such as the iron in red soil nickel ore, aluminium, manganese, magnesium, calcium are high, all far above the content of scandium, and the easily extraction of interference scandium.The technology of existing extraction scandium, production technique all also exist process compared with long, operation is complicated, yield poorly, raw and auxiliary material consumption is many, cost is high problem, be not suitable for red soil nickel ore and carry scandium.Therefore the present invention is based on above-mentioned discovery, emphatically the method extracting scandium from red soil nickel ore is studied, finally complete the present invention.The present invention is the utilization ratio improving red soil nickel ore further, reduces raw materials cost and opens new thinking, simultaneously for the extraction of scandium element provides new source.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or at least provides a kind of useful business to select.For this reason, one object of the present invention is a kind of method proposing effective process nickel hydroxide cobalt.
In one aspect of the invention, the present invention proposes a kind of nickel hydroxide cobalt treatment process, the method comprises: utilize sulfuric acid to carry out the first leaching process, to obtain nickel cobalt leach liquor to nickel hydroxide cobalt precipitation; Organic extractant is utilized to carry out scandium extraction treatment to described nickel cobalt leach liquor, to obtain nickel and cobalt containing solution and the organic phase containing scandium; Nickel cobalt is reclaimed from described nickel and cobalt containing solution; And reclaim scandium from the described organic phase containing scandium.Utilize aforesaid method can process red soil nickel ore, prepare nickel cobalt and scandium.
In addition, nickel hydroxide cobalt treatment process according to the above embodiment of the present invention can also have following additional technical characteristic:
According to embodiments of the invention, reclaim scandium from the described organic phase containing scandium and comprise further: utilize hydrochloric acid soln to strip, to obtain strip liquor to the described organic phase containing scandium; By described strip liquor and precipitant mix, to obtain the precipitation containing scandium; The described precipitation containing scandium is calcined, to obtain Scium trioxide.
According to embodiments of the invention, reclaim nickel cobalt from described nickel and cobalt containing solution and comprise further: described nickel and cobalt containing solution is carried out the process of heavy iron aluminium, to obtain iron aluminium slag and the nickel and cobalt containing solution through purification; Nickel and cobalt containing solution through purification is carried out wet-process refining, to reclaim nickel cobalt.
According to embodiments of the invention, comprise further and reclaim scandium from described iron aluminium slag through the following steps: utilize sulfuric acid to carry out the second leaching process to described iron aluminium slag, to obtain the second leach liquor, wherein, described second leach liquor contains iron, aluminium and scandium, organic extractant is utilized to carry out scandium extraction treatment to described second leach liquor, to obtain the organic phase containing scandium; Hydrochloric acid soln is utilized to strip, to obtain strip liquor to the described organic phase containing scandium; By described strip liquor and precipitant mix, to obtain the precipitation containing scandium; The described precipitation containing scandium is calcined, to obtain Scium trioxide.
According to embodiments of the invention, described organic extractant is be selected from least one in organo phosphoric extractant, neutral phosphorus-dased extractant, organic carboxyl acid extraction agent, organic amine extraction agent, organic chelated extraction agent.Can further improve scandium percentage extraction thus.
According to embodiments of the invention, described organo phosphoric extractant is at least one of P204 or CYANEX272, and described neutral phosphorus-dased extractant is TBP, and described organic carboxyl acid extraction agent is at least one of naphthenic acid or CA12, described organic amine extraction agent is N235, and described organic chelated extraction agent is N503.Can further improve scandium percentage extraction thus.
According to embodiments of the invention, the concentration of described hydrochloric acid soln is 0.01mol/L ~ 5mol/L.Can further improve scandium percentage extraction thus.
According to embodiments of the invention, described precipitation agent is at least one being selected from NaOH, ammoniacal liquor, sodium carbonate, sodium bicarbonate, oxalic acid, and the concentration of described precipitant solution is 0.1mol/L ~ 5mol/L.Can further improve scandium percentage extraction thus.
According to embodiments of the invention, the described precipitation containing scandium is carried out calcining be temperature lower calcination 1 ~ 6 hour at 700 ~ 900 degrees Celsius and complete.The yield of Scium trioxide can be improved thus further.
According to embodiments of the invention, utilizing before sulfuric acid carries out the first leaching process to described nickel hydroxide cobalt precipitation, slurrying process is carried out to described nickel hydroxide cobalt precipitation, to obtain nickel hydroxide cobalt slurries, and described first leaching process is carried out to described nickel hydroxide cobalt slurries.Leaching efficiency can be improved further thus, to improve the processing efficiency of red soil nickel ore further.
According to embodiments of the invention, the solid-to-liquid ratio of described nickel hydroxide cobalt slurries is (1:20) ~ (1:1).So that carry out extraction process to it, the yield of nickel cobalt and scandium can be improved further thus.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the schematic flow sheet of nickel hydroxide cobalt treatment process according to an embodiment of the invention.
Fig. 2 is the schematic flow sheet of nickel hydroxide cobalt treatment process in accordance with another embodiment of the present invention.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise one or more these features.In describing the invention, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
S100: extract scandium from nickel hydroxide cobalt precipitation
In one aspect of the invention, the present invention proposes a kind for the treatment of process of nickel hydroxide cobalt, according to one embodiment of present invention, the method comprises: utilize sulfuric acid to carry out leaching process, to obtain nickel cobalt leach liquor to nickel hydroxide cobalt precipitation; Organic extractant is utilized to carry out scandium extraction treatment to nickel cobalt leach liquor, to obtain nickel and cobalt containing solution and the organic phase containing scandium; Nickel cobalt is reclaimed from nickel and cobalt containing solution; And reclaim scandium from the organic phase containing scandium.
According to a particular embodiment of the invention, the type that organic extractant can adopt also is not particularly limited, according to concrete example of the present invention, organic extractant can adopt at least one being selected from organo phosphoric extractant, neutral phosphorus-dased extractant, organic carboxyl acid extraction agent, organic amine extraction agent, organic chelated extraction agent.The extraction yield of scandium can be improved thus further.Contriver finds at least one of P204 or CYANEX272 in organo phosphoric extractant by test of many times, TBP in neutral phosphorus-dased extractant, naphthenic acid in organic carboxyl acid extraction agent or CA12, N235 in organic amine extraction agent, N503 in organic chelated extraction agent all has good extraction to scandium, P204 effect of extracting wherein in organo phosphoric extractant is better, and is better than the effect of extracting of same kind of extractants P507.
According to one embodiment of present invention, as shown in Figure 1, following method can be utilized to reclaim scandium from containing the organic phase of scandium: utilize hydrochloric acid soln to strip to the organic phase containing scandium, to obtain strip liquor; Strip liquor is mixed with precipitant solution, to obtain the precipitation containing scandium; Precipitation containing scandium is calcined, to obtain Scium trioxide.Utilize the method can scandium element effectively in organic phase thus.According to a particular embodiment of the invention, the concentration of described hydrochloric acid is also not particularly limited, and according to a particular embodiment of the invention, the concentration of hydrochloric acid is specifically as follows 0.01mol/L ~ 5mol/L.The add-on that simultaneously can control hydrochloric acid is often liter is that the hydrochloric acid 0.1 of 1mol/L rises to 10 liters containing adding concentration in the organic phase of scandium.The extraction rate of scandium can be improved thus further.According to one embodiment of present invention, precipitation agent can be adopted to be precipitated by strip liquor, according to a particular embodiment of the invention, precipitation agent is at least one being selected from NaOH, ammoniacal liquor, sodium carbonate, sodium bicarbonate, oxalic acid, can improve deposition efficiency further thus.According to a particular embodiment of the invention, oxalic acid is utilized to precipitate strip liquor further, obtain containing scandium precipitation, the concentration of its mesoxalic acid is also not particularly limited, according to concrete example of the present invention, concentration can be adopted to be that the oxalic acid of 0.1mol/L ~ 5mol/L precipitates, and the volume of the oxalic acid added can control according to concrete concentration, such as, the oxalic acid 1.5 liters that concentration is 2mol/L can be added in often liter of strip liquor.Scandium extraction rate can be improved further thus.According to one embodiment of present invention, further the precipitation containing scandium obtained is calcined, to obtain Scium trioxide.Utilize the method for calcining effectively can remove other impurity in precipitation thus, the purity of scandium can be improved thus further.
According to one embodiment of present invention, leach taking a step forward for the treatment of step second and comprise slurrying process, be specially utilize sulfuric acid to nickel hydroxide cobalt precipitation carry out the second leaching process before, slurrying process is carried out to nickel hydroxide cobalt precipitation, to obtain nickel hydroxide cobalt slurries, and described second leaching process is carried out to described nickel hydroxide cobalt slurries, metallic element in being convenient to utilize sulfuric acid to be precipitated by nickel hydroxide cobalt thus leaches, and then can improve the efficiency of the second leaching process and the rate of recovery of nickel cobalt and scandium further.
According to a particular embodiment of the invention, the solid-to-liquid ratio of nickel hydroxide cobalt slurries that above-mentioned slurrying process obtains is (1:20) ~ (1:1).Can improve further thus and leach the efficiency of process and the rate of recovery of nickel cobalt and scandium.
According to one embodiment of present invention, conveniently understand, below the source of the nickel hydroxide cobalt of above-mentioned process is described in detail, according to a particular embodiment of the invention, above-mentioned nickel hydroxide cobalt can from the leach liquor of red soil nickel ore, according to a particular embodiment of the invention, below the method preparing nickel hydroxide nickel cobalt from red soil nickel ore is described in detail.
According to embodiments of the invention, sulfuric acid is utilized to carry out leaching process, to obtain red soil nickel ore leaching liquid to red soil nickel ore; The process of heavy iron aluminium and the process of heavy nickel cobalt are carried out to red soil nickel ore leaching liquid, to obtain iron aluminium slag and nickel hydroxide cobalt precipitation respectively.According to a particular embodiment of the invention, sulfuric acid is utilized first to leach red soil nickel ore, most iron aluminium slag will be removed, be further advanced by the pH value regulating leach liquor, residue iron aluminium element in removing leach liquor, therefore containing a large amount of nickel cobalts and scandium element in the leach liquor obtained, and then the pending nickel hydroxide cobalt precipitation of the present invention is obtained.
According to a particular embodiment of the invention, first utilize sulfuric acid to carry out pressure leaching process to red soil nickel ore in aforesaid method, valuable metal scandium, nickel, cobalt major part enter in high pressure pickling liquor; And most of impurity iron rule enters leached tailings with stable rhombohedral iron ore form, make most of iron be separated removing as impurity, in high pressure pickling liquor, concentration of iron is less than 1g/L.After pressurized acid leaching process is carried out to red soil nickel ore, most iron aluminium slag is separated thus.
Further, the process of heavy iron aluminium and the process of heavy nickel cobalt are carried out to above-mentioned red soil nickel ore leaching liquid, be specially and first adopt NaOH to regulate pH to 3.0 ~ 4.0 of above-mentioned red soil nickel ore leaching liquid, generate iron aluminium slag precipitation, filtered, with the process of heavy iron aluminium, the most of iron aluminium impurity in red soil nickel ore leaching liquid is separated removing by acidleach process thus.
Carry out the process of heavy nickel cobalt to the rear leach liquor of above-mentioned heavy iron aluminium further, particularly, continue in leach liquor, add NaOH and regulate pH to 7.0 ~ 9.0, generation precipitation, filtration obtain scandium hydroxide nickel cobalt precipitation.Scandium content in scandium hydroxide nickel cobalt precipitation is 0.01% ~ 5%, makes scandium be able to enrichment thus.
Therefore, according to a particular embodiment of the invention, sulfuric acid is utilized to carry out leaching process, to obtain nickel cobalt leach liquor to nickel hydroxide cobalt precipitation further; Organic extractant is utilized to carry out scandium extraction treatment to nickel cobalt leach liquor, to obtain nickel and cobalt containing solution and the organic phase containing scandium; Nickel cobalt is reclaimed from nickel and cobalt containing solution; And reclaim scandium from the organic phase containing scandium.
Utilize aforesaid method can process red soil nickel ore, can extract containing a large amount of nickel cobalt elements and a small amount of scandium element in red soil nickel ore, prepare the product of nickel cobalt and scandium.Especially can the scandium element in red soil nickel ore effectively be extracted.In order to improve the extraction yield of a small amount of scandium element in red soil nickel ore further, contriver finds first red soil nickel ore repeatedly to be leached process and the process of heavy iron aluminium and scandium extraction treatment, obtain iron aluminium slag and the organic phase containing scandium respectively, finally extract scandium from containing the organic phase of scandium.Therefore utilize the method for above-mentioned process nickel hydroxide cobalt of the present invention, effectively can improve the extraction yield of scandium.
According to one embodiment of present invention, by processing nickel hydroxide cobalt precipitation, obtain other nickel and cobalt containing solution intermediate product, according to a particular embodiment of the invention, contriver finds, further extraction process can be carried out to the solution containing nickel cobalt further, can reclaim and obtain nickel cobalt and scandium element, the rate of recovery and the nickel cobalt productive rate of scandium can be further increased thus.According to a particular embodiment of the invention, contain to product between therefrom the method reclaiming nickel cobalt and scandium in the solution of nickel cobalt to be below described in detail.
S200: reclaim nickel cobalt from nickel and cobalt containing solution
According to one embodiment of present invention, first from above-mentioned nickel hydroxide cobalt precipitation, nickel and cobalt containing solution is obtained, following method is utilized to reclaim nickel cobalt from nickel and cobalt containing solution further: nickel and cobalt containing solution to be carried out the process of heavy iron aluminium, to obtain iron aluminium slag and the nickel and cobalt containing solution through purification; Nickel and cobalt containing solution through purification is carried out wet-process refining, to reclaim nickel cobalt.The method can be utilized thus the nickel cobalt contained in red soil nickel ore effectively can be extracted.
According to one embodiment of present invention, method of the present invention comprises repeatedly carries out the process of heavy iron aluminium, first be that the red soil nickel ore leaching liquid that red soil nickel ore obtains after first leaches process is carried out the first heavy iron aluminium process, obtain iron aluminium slag, next is that nickel and cobalt containing solution is carried out the process of heavy iron aluminium, obtains iron aluminium slag.Therefore, a large amount of iron aluminium slag that utilized the method for process red soil nickel ore of the present invention to prepare.
S300: reclaim scandium from iron aluminium slag
According to one embodiment of present invention, can carry out extracting scandium the iron aluminium that the process of heavy iron aluminium obtains to nickel and cobalt containing solution from above-mentioned.As shown in Figure 1-2, according to a particular embodiment of the invention, the method reclaiming scandium from iron aluminium slag can comprise: first, and utilize sulfuric acid to carry out leaching process to iron aluminium slag, to obtain leach liquor, wherein, leach liquor contains iron, aluminium and scandium.Further, organic extractant is utilized to carry out scandium extraction treatment to leach liquor, to obtain the organic phase containing scandium.According to a particular embodiment of the invention, this organic extractant can be identical with organic extractant nickel cobalt leach liquor being carried out to scandium extraction treatment, according to example of the present invention, the type that organic extractant can adopt also is not particularly limited, according to concrete example of the present invention, organic extractant can adopt at least one being selected from organo phosphoric extractant (as P204, CYANEX272, P507), neutral phosphorus-dased extractant (as TBP), organic carboxyl acid extraction agent (as naphthenic acid, CA12), organic amine extraction agent (as N235), organic chelated extraction agent (as N503).The extraction yield of scandium can be improved thus further.
According to a particular embodiment of the invention, hydrochloric acid soln is utilized to strip, to obtain strip liquor to the organic phase containing scandium that above-mentioned extraction obtains.According to a particular embodiment of the invention, the concentration of described hydrochloric acid is also not particularly limited, and according to a particular embodiment of the invention, the concentration of hydrochloric acid is specifically as follows 0.01mol/L ~ 5mol/L.The add-on that simultaneously can control hydrochloric acid is often liter is that the hydrochloric acid 0.1 of 1mol/L rises to 10 liters containing adding concentration in the organic phase of scandium.The extraction rate of scandium can be improved thus further.According to a particular embodiment of the invention, oxalic acid is utilized to precipitate strip liquor further, obtain containing scandium precipitation, the concentration of its mesoxalic acid is also not particularly limited, according to concrete example of the present invention, concentration can be adopted to be that the oxalic acid of 0.1mol/L ~ 5mol/L precipitates, and the volume of the oxalic acid added can control according to concrete concentration, such as, the oxalic acid 1.5 liters that concentration is 2mol/L can be added in often liter of strip liquor.Scandium extraction rate can be improved further thus.
According to one embodiment of present invention, further the precipitation containing scandium obtained is calcined, to obtain Scium trioxide.Utilize the method for calcining effectively can remove other impurity in precipitation thus, the purity of scandium can be improved thus further.According to a particular embodiment of the invention, the degree of above-mentioned calcining can be regulated by the temperature and calcination time controlling calcining, according to concrete example of the present invention, according to the physicochemical property of scandium element, specifically can adopt by containing scandium be deposited in 700 ~ 900 degrees Celsius under carry out calcination processing 1 ~ 6 hour.Other impurity in precipitation can be removed thus to greatest extent, to improve the purity of Scium trioxide further.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiments are only descriptive, and do not limit the present invention in any way.
Embodiment 1
Certain red soil nickel ore constituent content is as table 1, and wherein, the content of scandium is 0.0033%.
Concentration in table 1 red soil nickel ore constituent content and high pressure pickling liquor thereof
| Element | Content (%) in red soil nickel ore | Concentration (g/L) in pickling liquor |
| Ni | 1.07 | 3.85 |
| Co | 0.1 | 0.32 |
| Cu | <0.02 | 0.01 |
| Fe | 41.9 | 1.32 |
| Mn | 0.653 | 2.05 |
| Zn | 〈0.05 | 0.11 |
| Pb | 〈0.02 | <0.001 |
| Si | 7.15 | 0.094 |
| Al | 1.83 | 1.69 |
| Ca | 0.157 | 0.14 |
| Mg | 1.98 | 3.59 |
| Cr | 0.5 | 0.022 |
| Sc | 0.0033 | 0.0117 |
By above-mentioned red soil nickel ore temperature be 255 degrees Celsius, pressure uses sulfuric acid leaching under being 5Mpa high pressure in autoclave.Valuable metal scandium (0.0117g/L), nickel (3.85g/L), cobalt (0.32g/L) major part enter in high pressure pickling liquor; The iron contamination of major part (~ 97%) then enters leached tailings with stable rhombohedral iron ore form, and make most of iron be separated removing as impurity, in high pressure pickling liquor, Fe concentration is 0.93g/L.
Add NaOH and regulate above-mentioned pickling liquor pH to 4.0, temperature 70 degrees Celsius, generate iron aluminium slag precipitation, filtered, make most of iron aluminium impurity be separated removing.Continue to add in NaOH to filtrate and regulate its pH to 7.5, generation precipitation, filtration obtain scandium hydroxide nickel cobalt precipitation.In scandium hydroxide nickel cobalt precipitation, scandium content is 0.075%, is 22.7 times of scandium content in red soil nickel ore, is able to enrichment.
Principal element content in table 2 nickel hydroxide cobalt precipitation
Get above-mentioned scandium hydroxide nickel cobalt precipitation, according to solid-to-liquid ratio S:L=1:10, add 20%(mass percent) sulphuric acid soln, stirring reaction leaches, and filters, and collects filtrate and cooks leach liquor, and filtrate is mainly containing Ni, Co, Mn, Ca, Mg, Sc, Fe, Al.
Get above-mentioned scandium hydroxide nickel cobalt sulphuric leachate, adjust ph is 0.2, according to aqueous phase: organic phase=10:1, the sulfonated kerosene solution added containing 10%Cyanex72 carries out extractive reaction.The percent extraction of Sc is 99.9%, Ni, Co, Fe, Al percentage extraction is respectively 0.05%, 0.1%, 0.3% and 0.Impurity extraction rate is low and be separated with scandium.By load organic phases, according to aqueous phase: organic phase=2:1, wash 2 grades with 10% sulphuric acid soln, a small amount of Fe, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in containing scandium organic phase.By after above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:5, add 0.5M HCl solution and carry out 5 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration.Calcine precipitation 2 hours, obtain the Scium trioxide that purity is 99.9% for 800 degrees Celsius.
Raffinate after above-mentioned extracting scandium, is sublimed nickel and cobalt solution after removing Sc, obtains nickel cobalt metal by the method for refining such as solvent extraction and separation, electrolysis.
Embodiment 2
Constituent content in certain nickel hydroxide cobalt precipitation is in table 2.Get above-mentioned scandium hydroxide nickel cobalt precipitation, according to solid-to-liquid ratio S:L=1:5, add 20%(mass percent) sulphuric acid soln, stirring reaction leaches, and filters, and collects filtrate.Filtrate is mainly containing Ni, Co, Mn, Sc, Fe, Al, Ca.
Get above-mentioned scandium hydroxide nickel cobalt sulphuric leachate, adjust ph is 0.5, according to aqueous phase: organic phase=5:1, and the kerosin added containing 10%N235+5%N503 carries out extractive reaction.The percent extraction of Sc is 99.8%, Ni, Co, Fe, Al percentage extraction is respectively 0.1%, 0.2%, 1.0% and 0.2%.Impurity extraction rate is low and be separated with scandium.By load organic phases, according to aqueous phase: organic phase=2:1, wash 4 grades with 5% sulphuric acid soln, a small amount of Fe, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in containing scandium organic phase.By after above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:1, add 0.2M HCl solution and carry out 2 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration.Calcine precipitations 1 hour at 850 degrees Celsius, obtain the Scium trioxide that purity is 99.9%.
Raffinate after above-mentioned extracting scandium, is sublimed nickel and cobalt solution after removing Sc, obtains nickel cobalt metal by the method for refining such as solvent extraction and separation, electrolysis.
Embodiment 3
Constituent content in certain laterite nickel ore by sulfuric acid leaching liquid is in table 1.By lye pH adjustment to 3.8, make the iron aluminium in leach liquor form iron aluminium slag, scandium is separated with iron, aluminium impurity.And then by lye pH adjustment to 8.0, nickel cobalt is precipitated, obtain nickel hydroxide cobalt precipitation.Scandium obtains enrichment with nickel hydroxide cobalt Precipitation, and content is 0.139%, and constituent content is in table 3.
Principal element content in table 3 nickel hydroxide cobalt precipitation
Get above-mentioned scandium hydroxide nickel cobalt precipitation, according to solid-to-liquid ratio S:L=1:5, add 20%(mass percent) sulphuric acid soln, stirring reaction leaches, and filters, and collects filtrate and cooks leach liquor, and filtrate is mainly containing Ni, Co, Mn, Ca, Mg, Sc, Fe, Al.
Get above-mentioned scandium hydroxide nickel cobalt sulphuric leachate, adjust ph is 0.5, according to aqueous phase: organic phase=5:1, and the kerosin added containing 15%P204+5%TBP carries out extractive reaction.The percent extraction of Sc is 99.8%, Ni, Co, Fe, Al percentage extraction is respectively 0.1%, 0.2%, 0.1% and 0.Impurity extraction rate is low and be separated with scandium.By load organic phases, according to aqueous phase: organic phase=2:1, wash 4 grades with 5% sulphuric acid soln, a small amount of Fe, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in containing scandium organic phase.By after above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:10, add 2MHCl solution and carry out 10 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration.Calcine precipitations 1 hour at 850 degrees Celsius, obtain the Scium trioxide that purity is 99.9%.
Embodiment 4
The principal element content of laterite nickel ore by sulfuric acid leaching liquid is as table 1, and adjust the pH to 4.5 of laterite nickel ore by sulfuric acid leaching liquid with saturated Ca (OH) 2 solution, temperature 70 degrees Celsius, makes the iron aluminium element in leach liquor form the first iron aluminium slag.Scandium is with iron, aluminium element co-precipitation, and in above-mentioned iron aluminium slag precipitation, scandium content is 0.032%, and compared with red soil nickel ore, scandium obtains about 10 times of enrichments, is separated with nickel cobalt etc. simultaneously.
Raffinate after above-mentioned extracting scandium, is sublimed nickel and cobalt solution after removing Sc, obtains nickel cobalt metal by the method for refining such as solvent extraction and separation, electrolysis.
The principal element content of table 4 first iron aluminium slag
The principal element content of the first iron aluminium slag is as table 4.Wherein, by above-mentioned first iron aluminium slag precipitation, according to solid-to-liquid ratio S:L=1:10, add the sulphuric acid soln that concentration is 2mol/L, mix and blend, filter, to carry out the second leaching process, obtain the first iron aluminium slag leach liquor, it is mainly containing Fe, Al and a small amount of Sc, Ni, Ca, Mn.First iron aluminium slag infusion solution analytical data is as following table 5:
Concentration of element in table 5 first iron aluminium slag leach liquor
Do organic phase with 5%Cyanex272+1%TBP, compare A:O=10:1 with organic phase, pH extracts above-mentioned solution in 0.2 situation, and the percentage extraction of scandium reaches 96.53%.From the first iron aluminium slag sulphuric leachate, the percent extraction of extracting scandium is as table 6:
The percent extraction of extracting scandium in table 6 first iron aluminium slag sulphuric leachate
Visible, impurity extraction rate is low and scandium percentage extraction is high, thus is separated with scandium.By load organic phases, according to aqueous phase: organic phase=2:1, wash 4 grades with 5% sulphuric acid soln, a small amount of Fe, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in containing scandium organic phase.
By after above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:3, add 2M HCl solution and carry out 3 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration.Calcine precipitations 1 hour at 850 degrees Celsius, obtain the Scium trioxide that purity is 99.9%.
Embodiment 5
By the first iron aluminium slag sulphuric leachate shown in table 1, adjust ph is 3.0, according to aqueous phase: organic phase fluid ratio=5:1, add containing 15%(v/v) kerosin of carboxylic acid extraction agent CA12 carries out 10 grades of extractive reactions, the percentage extraction of Sc is 95.5%, the percentage extraction of Fe is 37.5%, the percentage extraction of Ni and Co close to 0, the percentage extraction of Mn is 0.2%, the percentage extraction of Mg is 0.5%.By load organic phases according to aqueous phase: organic phase fluid ratio=1:1, wash 20 grades with 0.02mol/L sulphuric acid soln, a small amount of Fe, Ni, Co, Mn, Mg impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in organic phase.By above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase fluid ratio=1:5, add 0.2M HCl solution and carry out 10 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2.5mol/L oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration, calcine precipitations 4 hours at 750 degrees Celsius, obtain the Scium trioxide that purity is 99.8%.
Embodiment 6
Constituent content in certain nickel hydroxide cobalt precipitation is in table 2.Get above-mentioned scandium hydroxide nickel cobalt precipitation, according to solid-to-liquid ratio S:L=1:10, add 10%(mass percent) sulphuric acid soln, stirring reaction 3 hours, filters, and collects filtrate.Filtrate is mainly containing Ni, Co, Mn, Sc, Fe, Al, Ca.Be pH4.8 by NaOH acid adjustment basicity, temperature 70 degrees Celsius, generates the second iron aluminium slag precipitation, filters.The second iron aluminium slag principal element content that analysis obtains is as following table 7:
Table 7 second iron aluminium slag principal element content
In second iron aluminium slag, the content of scandium is 1.14%, is enriched about 15 times compared with in nickel hydroxide cobalt, with red soil nickel ore in compared be enriched about 345 times.By above-mentioned secondary iron aluminium slag according to solid-to-liquid ratio S:L=1:10, add 10%(mass percent) sulphuric acid soln Leaching of Scandium, stirring reaction 2 hours, filters, and collects filtrate.
Get above-mentioned second iron aluminium slag sulphuric leachate, adjust ph is 0.5, according to aqueous phase: organic phase=5:1, and the kerosin added containing 10%N235+5%N503 carries out extractive reaction.The percent extraction of Sc is 99.8%, Ni, Co, Fe, Al percentage extraction is respectively 0.15%, 0.2%, 5.0% and 0.2%.By load organic phases, according to aqueous phase: organic phase=2:1, wash 5 grades with 5% sulphuric acid soln, a small amount of Fe, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in containing scandium organic phase.By after above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:1, add 0.2M HCl solution and carry out 2 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration.Calcine precipitations 1 hour at 850 degrees Celsius, obtain the Scium trioxide that purity is 99.9%.
By the second iron aluminium slag precipitation, the filtrate of filtering rear gained, for removing the nickel and cobalt solution after the impurity purifying such as Fe, Si, obtain nickel cobalt metal by the method for refining such as solvent extraction and separation, electrolysis.
Embodiment 7
Constituent content in certain second iron aluminium slag precipitation is in table 7.Get above-mentioned scandium hydroxide nickel cobalt precipitation, according to solid-to-liquid ratio S:L=1:10, add 10%(mass percent) sulphuric acid soln, stirring reaction 3 hours, filters, and collects filtrate.Filtrate is mainly containing Ni, Co, Mn, Sc, Fe, Al, Ca.Be pH5.5 by NaOH acid adjustment basicity, temperature 70 degrees Celsius, generates the second iron aluminium slag precipitation, filters.
By above-mentioned secondary iron aluminium slag according to solid-to-liquid ratio S:L=1:10, add 10%(mass percent) sulphuric acid soln Leaching of Scandium, stirring reaction 2 hours, filters, and collects filtrate.
Get above-mentioned second iron aluminium slag sulphuric leachate, adjust ph is 0.5, according to aqueous phase: organic phase=5:1, and the kerosin added containing 10%P204 carries out extractive reaction.The percent extraction of Sc is 99.8%, Ni, Co, Fe, Al percentage extraction is respectively 0.1%, 0.15%, 0.8% and 0.By load organic phases, according to aqueous phase: organic phase=5:1, wash 5 grades with 5% sulphuric acid soln, a small amount of Fe, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in containing scandium organic phase.By after above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:5, add 1M HCl solution and carry out 10 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 2M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration.Calcine precipitations 1 hour at 850 degrees Celsius, obtain the Scium trioxide that purity is 99.9%.
Embodiment 8
Certain red soil nickel ore constituent content is as table 1, and wherein, the content of iron, aluminium, magnesium, nickel, manganese, calcium, scandium is respectively 41.9%, 1.83%, 1.98%, 1.07%, 0.65%, 0.18%, 0.0033%.The acidleach of sulfuric acid high pressure is carried out to above-mentioned red soil nickel ore and leaches process, obtain sulphuric leachate composition as table 1.
Get above-mentioned laterite nickel ore by sulfuric acid leaching liquid, adjust ph is 3.5, according to aqueous phase: organic phase fluid ratio=5:1, add containing 5%(v/v) kerosin of carboxylic acid extraction agent CA12 carries out 5 grades of extractive reactions, the percentage extraction of Sc is 98.5%, the percentage extraction of Fe is 25%, the percentage extraction of Ni and Co close to 0, the percentage extraction of Mn is 0.15%, the percentage extraction of Mg is 0.46%.By load organic phases according to aqueous phase: organic phase fluid ratio=1:2, wash 15 grades with 0.01M sulphuric acid soln, a small amount of Fe, Ni, Co, Mn, Mg impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in organic phase.By above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase fluid ratio=1:10, add 0.5M HCl solution and carry out 5 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 1M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration, calcine precipitations 4 hours at 750 degrees Celsius, obtain the Scium trioxide that purity is 99.8%.
Raffinate after above-mentioned extracting scandium, is sublimed nickel and cobalt solution after removing Sc, obtains nickel cobalt metal by the method for refining such as solvent extraction and separation, electrolysis.
Embodiment 9
Getting pH is that the above-mentioned laterite sulphuric leachate 2.0L(of 0.2 is as table 1), mix with 200mL3%P204-1%TBP-sulfonated kerosene organic solution, stir to carry out extractive reaction, the reaction times is 10 minutes.The percentage of extracting scandium is 99.5%, and the percentage extraction of impurity Ca, Mg, Mn, Ni, Fe, Al is all lower than 10%.The elements by extraction percentage directly extracted from laterite leach liquor is as table 8:
The elements by extraction percentage that table 8 laterite leach liquor directly extracts
By load organic phases according to aqueous phase: organic phase fluid ratio=1:1, wash 2 grades with 0.1M sulphuric acid soln, a small amount of Fe, Al, Ni, Ca, Mg, Mn impurity extracted is washed off, and Sc remains in organic phase.Therefore, scandium and magazins' layout, and be enriched in organic phase.By above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase fluid ratio=1:10, add 1MHCl solution and carry out 10 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 3M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration, calcine precipitations 1 hour at 800 degrees Celsius, obtain the Scium trioxide that purity is 99.8%.
Embodiment 10
Get containing 3.3mg/L Sc, 0.26g/L Fe, 0.15g/L Ca, 1.45g/L Mg, 0.81g/L Mn, 1.24g/L Ni, 0.12g/L Co, the laterite sulphuric leachate 2.0L of pH0.2, mix with 100mL5%N235-1%N503-sulfonated kerosene organic solution, stir to carry out extractive reaction, the reaction times is 2 minutes.The percentage of extracting scandium is 98.0%, and the percentage extraction of impurity F e, Al, Ca, Mg, Mn, Ni, Co is respectively 8.5%, 3.2%, 1.2%, 1.0%, 0.2%, 0.1%, 0.15%.By load organic phases according to aqueous phase: organic phase fluid ratio=1:1, wash 5 grades with 0.2M sulphuric acid soln, Fe, Al, Ca, Mg, Mn, Ni, Co impurity extracted is washed off, and Sc remains in organic phase.
By above-mentioned purifying containing scandium organic phase, according to aqueous phase: organic phase=1:2, add 0.5M HCl solution and carry out 2 grades of reextraction, obtain containing scandium strip liquor.
In strip liquor, add 3M oxalic acid solution, oxalic scandium precipitates.By sedimentation and filtration, calcine precipitations 1 hour at 800 degrees Celsius, obtain the Scium trioxide that purity is 99.9%.
In the description of this specification sheets, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (9)
1., containing a treatment process for scandium nickel hydroxide cobalt, it is characterized in that, comprising:
Sulfuric acid is utilized to carry out the first leaching process, to obtain nickel cobalt leach liquor to containing scandium nickel hydroxide cobalt precipitation;
Organic extractant is utilized to carry out scandium extraction treatment to described nickel cobalt leach liquor, to obtain nickel and cobalt containing solution and the organic phase containing scandium;
Nickel cobalt is reclaimed from described nickel and cobalt containing solution; And
Scandium is reclaimed from the described organic phase containing scandium,
Wherein, described organic extractant is be selected from least one in organo phosphoric extractant, neutral phosphorus-dased extractant, organic carboxyl acid extraction agent, organic amine extraction agent and organic chelated extraction agent,
Described organo phosphoric extractant is at least one of P204 and CYANEX272, described neutral phosphorus-dased extractant is TBP, described organic carboxyl acid extraction agent is at least one of naphthenic acid and CA12, and described organic amine extraction agent is N235, and described organic chelated extraction agent is N503.
2. method according to claim 1, is characterized in that, reclaims scandium comprise further from the described organic phase containing scandium:
Sulphuric acid soln is utilized to wash the described organic phase containing scandium, so that the organic phase containing scandium described in purifying;
Hydrochloric acid soln is utilized to strip, to obtain strip liquor to the organic phase containing scandium described in after purifying;
By described strip liquor and precipitant mix, to obtain the precipitation containing scandium;
The described precipitation containing scandium is calcined, to obtain Scium trioxide.
3. method according to claim 1, is characterized in that, reclaims nickel cobalt comprise further from described nickel and cobalt containing solution:
Described nickel and cobalt containing solution is carried out the process of heavy iron aluminium, to obtain iron aluminium slag and the nickel and cobalt containing solution through purification;
Nickel and cobalt containing solution through purification is carried out wet-process refining, to reclaim nickel cobalt.
4. method according to claim 3, is characterized in that, comprises further and reclaims scandium from described iron aluminium slag through the following steps:
Utilize sulfuric acid to carry out the second leaching process to described iron aluminium slag, to obtain the second leach liquor, wherein, described second leach liquor contains iron, aluminium and scandium,
Organic extractant is utilized to carry out scandium extraction treatment to described second leach liquor, to obtain the organic phase containing scandium;
Hydrochloric acid soln is utilized to strip, to obtain strip liquor to the described organic phase containing scandium;
By described strip liquor and precipitant mix, to obtain the precipitation containing scandium;
The described precipitation containing scandium is calcined, to obtain Scium trioxide.
5. the method according to claim 2 or 4, is characterized in that, the concentration of described hydrochloric acid soln is 0.01mol/L ~ 5mol/L.
6. the method according to claim 2 or 4, is characterized in that, described precipitation agent is at least one being selected from NaOH, ammoniacal liquor, sodium carbonate, sodium bicarbonate, oxalic acid, and the concentration of described precipitant solution is 0.1mol/L ~ 5mol/L.
7. the method according to claim 2 or 4, is characterized in that, the described precipitation containing scandium is carried out calcining being temperature lower calcination 1 ~ 6 hour at 700 ~ 900 degrees Celsius and completing.
8. method according to claim 1, it is characterized in that, utilizing before sulfuric acid carries out the first leaching process to described nickel hydroxide cobalt precipitation, slurrying process is carried out to described nickel hydroxide cobalt precipitation, to obtain nickel hydroxide cobalt slurries, and described first leaching process is carried out to described nickel hydroxide cobalt slurries.
9. method according to claim 8, is characterized in that, the solid-to-liquid ratio of described nickel hydroxide cobalt slurries is (1:20) ~ (1:1).
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| JP5854065B2 (en) * | 2014-02-19 | 2016-02-09 | 住友金属鉱山株式会社 | Scandium recovery method |
| CN104862503B (en) * | 2015-04-20 | 2017-07-04 | 中国恩菲工程技术有限公司 | The method that scandium is extracted from lateritic nickel ore |
| CN107739829A (en) * | 2017-09-29 | 2018-02-27 | 中国恩菲工程技术有限公司 | The recovery method of nickel element, cobalt element, copper and Zn-ef ficiency in smelting laterite-nickel ores and in slag |
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| CN113120941A (en) * | 2019-12-31 | 2021-07-16 | 中冶瑞木新能源科技有限公司 | Method for extracting high-purity scandium oxide from scandium-containing nickel cobalt hydroxide in short process |
| RU2729282C1 (en) * | 2020-03-10 | 2020-08-05 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method of extracting scandium from scandium-containing materials |
| CN115896465A (en) * | 2022-12-29 | 2023-04-04 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting scandium from by-product of molten salt chlorination comprehensive utilization |
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