CN114480887B - Method for selectively extracting scandium from lateritic nickel ore by sulfuric acid roasting-water leaching method - Google Patents
Method for selectively extracting scandium from lateritic nickel ore by sulfuric acid roasting-water leaching method Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052706 scandium Inorganic materials 0.000 title claims abstract description 83
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002386 leaching Methods 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 56
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 51
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 49
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000012074 organic phase Substances 0.000 claims abstract description 23
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- OMMFSGNJZPSNEH-UHFFFAOYSA-H oxalate;scandium(3+) Chemical compound [Sc+3].[Sc+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O OMMFSGNJZPSNEH-UHFFFAOYSA-H 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 229910001710 laterite Inorganic materials 0.000 claims abstract description 8
- 239000011504 laterite Substances 0.000 claims abstract description 8
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002893 slag Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000003350 kerosene Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 19
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- 230000001180 sulfating effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 2
- KOQOJLXRPCIFKW-UHFFFAOYSA-N oxalic acid scandium Chemical compound [Sc].C(C(=O)O)(=O)O.[Sc] KOQOJLXRPCIFKW-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 32
- 239000000047 product Substances 0.000 description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910000542 Sc alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- LUKDNTKUBVKBMZ-UHFFFAOYSA-N aluminum scandium Chemical compound [Al].[Sc] LUKDNTKUBVKBMZ-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- 239000003864 humus Substances 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- -1 preferably Chemical compound 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/06—Sulfating roasting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for selectively extracting scandium from lateritic nickel ores by adopting a sulfuric acid roasting-water leaching method, which comprises the following steps of: (1) Crushing and finely grinding laterite nickel ore, and then mixing and roasting with concentrated sulfuric acid; (2) Leaching the roasting product obtained in the step (1) by water to obtain leaching liquid and leaching slag; (3) Extracting the leaching solution to obtain scandium-containing organic phase and raffinate; (4) Back-extracting the scandium-containing organic phase to obtain scandium-rich solution and organic phase; (5) And adding a oxalic acid solution into the scandium-rich solution to precipitate to obtain scandium oxalate. According to the invention, the laterite nickel ore is treated by a sulfating roasting-water leaching method, scandium can be selectively leached, the problem of difficulty in subsequent iron removal is effectively avoided, and Cyanex572 is selected as an extractant, so that the extractant has a good scandium selective extraction effect and a good extraction enrichment effect, the impurity content in the obtained scandium-rich solution is extremely low, and the scandium oxide product obtained by subsequent oxalic acid scandium precipitation and calcination has higher quality.
Description
Technical Field
The invention belongs to the field of metallurgical engineering, and particularly relates to a method for selectively extracting scandium from lateritic nickel ores by adopting a sulfuric acid roasting-water leaching method.
Background
Scandium is a rare and expensive strategic metal, has the characteristics of high activity, high melting point, light weight, softness and the like, and is widely applied to the high-tech fields of national defense, war industry and the like, and the demand is continuously increased. It is a typical rare, dispersed, parent stone element, whose individual minerals are very rare in nature, but widely distributed among other minerals. Scandium content in lateritic nickel ore is between 50g/t and 600g/t, and is considered as the most promising scandium resource in the future. Laterite nickel ores can be simply classified into a humus type and a limonite type, the former can be effectively treated by a pyrometallurgical process, but high-value scandium cannot be recovered. And brown iron type laterite nickel ore is usually treated by High Pressure Acid Leaching (HPAL), scandium is recycled as a byproduct in the nickel cobalt extraction process. The method completely ignores the economic value and application prospect of scandium metal, has a full-process recovery rate of about 45%, does not realize efficient extraction and high-value preparation of scandium in lateritic nickel, and adopts high-pressure acid leaching (HPAL) treatment to use a high-pressure titanium autoclave, so that the investment is high.
As a traditional smelting process, a sulfating roasting-water leaching method has been proved by researchers to selectively extract nickel and cobalt from laterite-nickel ores, but no report has been made on the use of the process for extracting scandium from laterite-nickel ores. Both Chinese patent 201310660501.8 and 201811260391.5 disclose a method for recovering scandium from red mud by a sulfating roasting-water leaching method, but the property difference between the red mud and lateritic nickel ore is large, the red mud is wet slag generated in the Bayer process production process, and the treatment difficulty of the red mud is lower than that of original mineral resources. Scandium is usually present in the red mud in a surface adsorption form and is very easy to extract, while scandium in the lateritic nickel is usually present in refractory minerals such as goethite and silicate in a similar form. With the increasing demand of aluminum scandium alloys and solid fuel cells year by year, a scandium supply chain with sufficient resources, stable process and reasonable price is needed. Therefore, development of a method for cleanly and efficiently recycling scandium from lateritic nickel ore, which is simple in process and low in production cost, is imperative.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a method for selectively extracting scandium from lateritic nickel ores by adopting a sulfuric acid roasting-water leaching method.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for selectively extracting scandium from lateritic nickel ore by adopting a sulfuric acid roasting-water leaching method comprises the following steps:
(1) Crushing and finely grinding laterite nickel ore, and then mixing and roasting with concentrated sulfuric acid;
(2) Leaching the roasting product obtained in the step (1) by water to obtain leaching liquid and leaching slag;
(3) Extracting the leaching solution to obtain scandium-containing organic phase and raffinate;
(4) Back-extracting the scandium-containing organic phase to obtain scandium-rich solution and organic phase;
(5) And adding a oxalic acid solution into the scandium-rich solution to precipitate to obtain scandium oxalate.
In the step (1), the main chemical reactions involved in the sulfatizing roasting process of laterite-nickel ore are as follows:
Sc 2 O 3 +3H 2 SO 4 ＝Sc 2 (SO 4 ) 3 +3H 2 O(g)；
Fe 2 O 3 +3H 2 SO 4 ＝Fe 2 (SO 4 ) 3 +3H 2 O(g)；
Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g)。
in the above method for selectively extracting scandium, preferably, in the step (3), the volume ratio of the extracting agent is 1-10: 1 to 10 of Cyanex572 and sulfonated kerosene, and the ratio of the Cyanex572 to the sulfonated kerosene in the extraction process is 1 to 10:10, the extraction time is 10-30 min, and the extraction stage number is 3-5. The Cyanex572 extractant is applied to separation and extraction of heavy rare earth elements for a long time, but is never applied to the field of scandium extraction in laterite-nickel ore high-pressure leaching solution.
In the above method for selectively extracting scandium, the concentrated sulfuric acid is preferably a sulfuric acid solution having a concentration of 70% or more.
In the above method for selectively extracting scandium, preferably, in the step (4), the stripping agent is hydrochloric acid solution with a concentration of 2-5 mol/L, and the ratio of the stripping agent in the stripping process is 1-5: 1, the back extraction time is 10-30 min, and the back extraction stage number is 1-5.
In the above method for selectively extracting scandium, preferably, in the step (5), the oxalic acid solution is 10-30wt% oxalic acid solution; the pH of the solution during precipitation is 1.5-2.0.
In the method for selectively extracting scandium, preferably, in the step (2), the liquid-solid ratio of the water leaching process is 2-10, the ratio unit is mL/g, the water leaching time is 0.5-3.0 h, and the water leaching temperature is 30-80 ℃.
In the above method for selectively extracting scandium, preferably, in the step (1), the ratio of the concentrated sulfuric acid to the lateritic nickel ore is 0.1-1.0, and the ratio is in mL/g.
In the above method for selectively extracting scandium, preferably, in the step (1), the roasting temperature is 500 to 800 ℃, and the roasting time is 1.0 to 5.0 hours.
In the above method for selectively extracting scandium, preferably, scandium oxalate obtained in the step (5) is calcined to obtain a scandium oxide product.
In the above method for selectively extracting scandium, the calcination temperature is preferably 500 to 600 ℃ and the calcination time is preferably 2 to 4 hours.
In the above method for selectively extracting scandium, preferably, in the step (1), the particle size of the finely ground lateritic nickel ore is-0.074 mm.
Compared with the prior art, the invention has the advantages that:
(1) According to the invention, the laterite nickel ore is treated by a sulfating roasting-water leaching method, scandium can be selectively leached, the problem of difficulty in subsequent iron removal is effectively avoided, and Cyanex572 is selected as an extractant, so that the extractant has a good scandium selective extraction effect and a good extraction enrichment effect, the impurity content in the obtained scandium-rich solution is extremely low, and the scandium oxide product obtained by subsequent oxalic acid scandium precipitation and calcination has higher quality.
(2) The method has the advantages of simple and convenient operation condition, easy control, simple and easily obtained production equipment, low investment cost and production cost, high scandium recovery rate and product quality, realization of clean and efficient extraction and high-valued preparation of trace scandium with high added value in low-grade lateritic nickel ore, and suitability for large-scale popularization and application.
Drawings
FIG. 1 is a schematic diagram of a method for selectively extracting scandium from lateritic nickel ore according to the present invention.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
The various reagents and materials used in the present invention are commercially available or may be prepared by known methods unless otherwise specified.
Example 1:
the laterite-nickel ore treated in this example consisted of: 0.75wt.% of Ni, 0.061wt.% of Co, 0.57wt.% of Mn, 0.0055wt.% of sc, 47.8wt.% of Fe, 0.43wt.% of Mg, 3.98wt.% of Al, and 1wt.% of Cr.
The method for selectively extracting scandium from lateritic nickel ore by adopting a sulfuric acid roasting-water leaching method in the embodiment is shown in a figure 1, and comprises the following steps:
(1) Grinding: crushing and grinding laterite-nickel ore to obtain laterite-nickel ore with granularity of-0.074 mm;
(2) Sulfating roasting: fully and uniformly mixing the laterite-nickel ore obtained in the step (1) with concentrated sulfuric acid, wherein the dosage ratio of the concentrated sulfuric acid to the laterite-nickel ore is 0.5mL/g, and then placing the mixture in a tubular atmosphere furnace for roasting at 600 ℃ for 2.0h to obtain a roasting product;
(3) Soaking in water: leaching the roasting product obtained in the step (2) in water, wherein the solid ratio of the leaching solution is 5mL/g, the leaching time is 2.0h, the leaching temperature is 80 ℃, filtering is carried out after the leaching is finished, and leaching solution and leaching slag are obtained, and the leaching rates of Ni, co, sc and Fe are 71.89%, 81.98%, 81.79% and 5.14% respectively;
(4) Extraction: extracting the leaching solution obtained in the step (3), wherein an extraction system comprises the following components in a volume ratio of 2:8 and sulfonated kerosene, the ratio (O/A) of which is 1:5, extracting for 10min, wherein the extraction stage number is 2, oscillating, standing, and separating to obtain scandium-containing organic phase and raffinate, wherein in the process, the extraction rates of Sc and Fe are 93.67% and 1.05% respectively;
(5) Back extraction: carrying out back extraction on the scandium-containing organic phase obtained in the step (4), wherein the back extraction agent is hydrochloric acid solution with the concentration of 3mol/L, and the ratio (O/A) is 1:1, the back extraction time is 10min, the back extraction stage number is 3, vibration and standing are carried out, scandium-rich solution and organic phase are obtained by separation, the organic phase is recycled in the step (4), and the back extraction rate of Sc is 90.91%;
(6) Scandium precipitation by oxalic acid: scandium precipitation is carried out on the scandium-rich solution obtained in the step (5), the scandium precipitation pH is 2.0, and the mass fraction of the oxalic acid solution is 20wt%, so that scandium oxalate is obtained;
(7) Calcining: calcining scandium oxalate obtained in the step (6) at 600 ℃ for 2 hours to obtain a scandium oxide product with the yield of 90.52% and the purity of 96.75%.
Example 2:
the laterite-nickel ore treated in this example consisted of: 0.75wt.% of Ni, 0.061wt.% of Co, 0.57wt.% of Mn, 0.0055wt.% of sc, 47.8wt.% of Fe, 0.43wt.% of Mg, 3.98wt.% of Al, and 1wt.% of Cr.
The method for selectively extracting scandium from lateritic nickel ore by adopting a sulfuric acid roasting-water leaching method in the embodiment is shown in a figure 1, and comprises the following steps:
(1) Grinding: crushing and grinding laterite-nickel ore to obtain laterite-nickel ore with granularity of-0.074 mm;
(2) Sulfating roasting: fully and uniformly mixing the laterite-nickel ore obtained in the step (1) with concentrated sulfuric acid, wherein the dosage ratio of the concentrated sulfuric acid to the laterite-nickel ore is 0.3mL/g, and then placing the mixture into a tubular atmosphere furnace for roasting at 800 ℃ for 2.0h to obtain a roasting product;
(3) Soaking in water: leaching the roasting product obtained in the step (2) in an aqueous solution, wherein the solid ratio of the leaching solution is 10mL/g, the leaching time is 2.0h, the leaching temperature is 60 ℃, filtering is carried out after the leaching is finished, and leaching solution and leaching residues are obtained, wherein the leaching rates of Ni, co, sc and Fe are 63.84%, 70.48%, 73.04% and 3.61% respectively;
(4) Extraction: extracting the leaching solution obtained in the step (3), wherein an extraction system comprises Cyanex572 and sulfonated kerosene according to a volume ratio of 1:9, and the ratio (O/A) is 1:1, extracting for 10min, wherein the extraction stage number is 3, oscillating, standing, and separating to obtain scandium-containing organic phase and raffinate, wherein the extraction rates of Sc and Fe are 89.94% and 1.88% respectively;
(5) Back extraction: carrying out back extraction on the scandium-containing organic phase obtained in the step (4), wherein the back extraction agent is hydrochloric acid solution with the concentration of 5mol/L, and the ratio (O/A) is 1:1, the back extraction time is 20min, the back extraction stage number is 1, vibration and standing are carried out, scandium-rich solution and organic phase are obtained by separation, the organic phase is recycled in the step S4, and the back extraction rate of Sc is 83.66%;
(6) Scandium precipitation by oxalic acid: scandium precipitation is carried out on the scandium-rich solution obtained in the step (5), the scandium precipitation pH is 1.8, and the mass fraction of the oxalic acid solution is 15wt%, so that scandium oxalate is obtained;
(7) Calcining: calcining scandium oxalate obtained in the step (6) at 550 ℃ for 3 hours to obtain a scandium oxide product with the yield of 88.91% and the purity of 92.16%.
Example 3:
the laterite-nickel ore treated in this example consisted of: 0.75wt.% of Ni, 0.061wt.% of Co, 0.57wt.% of Mn, 0.0055wt.% of sc, 47.8wt.% of Fe, 0.43wt.% of Mg, 3.98wt.% of Al, and 1wt.% of Cr.
The method for selectively extracting scandium from lateritic nickel ore by adopting a sulfuric acid roasting-water leaching method in the embodiment is shown in a figure 1, and comprises the following steps:
(1) Grinding: crushing and grinding laterite-nickel ore to obtain laterite-nickel ore with granularity of-0.074 mm;
(2) Sulfating roasting: fully and uniformly mixing the laterite-nickel ore obtained in the step (1) with concentrated sulfuric acid, wherein the dosage ratio of the concentrated sulfuric acid to the laterite-nickel ore is 1.0mL/g, and then placing the mixture into a tubular atmosphere furnace for roasting at the temperature of 500 ℃ for 3.0h to obtain a roasting product;
(3) Soaking in water: leaching the roasting product obtained in the step (2) in an aqueous solution, wherein the solid ratio of the leaching solution is 3mL/g, the leaching time is 2.0h, the leaching temperature is 80 ℃, filtering is carried out after the leaching is completed, and leaching solution and leaching slag are obtained, and the leaching rates of Ni, co, sc and Fe are 72.49%, 75.46%, 78.68% and 9.28%, respectively;
(4) Extraction: extracting the leaching solution obtained in the step (3), wherein an extraction system comprises Cyanex572 and sulfonated kerosene according to a volume ratio of 3:7, and the ratio (O/A) is 1:1, extracting for 20min, wherein the extraction stage number is 3, oscillating, standing, and separating to obtain scandium-containing organic phase and raffinate, wherein the extraction rates of Sc and Fe are respectively 95.08% and 2.35%;
(5) Back extraction: carrying out back extraction on the scandium-containing organic phase obtained in the step (4), wherein a back extraction agent is hydrochloric acid solution with the concentration of 5mol/L, and the ratio of O/A is 1:1, the back extraction time is 20min, the back extraction stage number is 3, vibration and standing are carried out, scandium-rich solution and organic phase are obtained by separation, the organic phase is recycled in the step (4), and the back extraction rate of Sc is 92.73%;
(6) Scandium precipitation by oxalic acid: scandium precipitation is carried out on the scandium-rich solution obtained in the step (5), the scandium precipitation pH is 2.0, and the mass fraction of the oxalic acid solution is 20wt%, so that scandium oxalate is obtained;
(7) Calcining: calcining scandium oxalate obtained in the step (6) at 600 ℃ for 3 hours to obtain a scandium oxide product with the yield of 91.74% and the purity of 95.60%.
Claims (5)
1. The method for selectively extracting scandium from lateritic nickel ore by adopting a sulfuric acid roasting-water leaching method is characterized by comprising the following steps of:
(1) Crushing and finely grinding laterite nickel ore, and then mixing and roasting with concentrated sulfuric acid; the ratio of the concentrated sulfuric acid to the laterite nickel ore is 0.1-1.0, the ratio is in mL/g, the roasting temperature is 500-800 ℃, and the roasting time is 1.0-5.0 h;
(2) Leaching the roasting product obtained in the step (1) by water to obtain leaching liquid and leaching slag; wherein the liquid-solid ratio in the water leaching process is 2-10, the ratio unit is mL/g, the water leaching time is 0.5-3.0 h, and the water leaching temperature is 30-80 ℃;
(3) Extracting the leaching solution to obtain scandium-containing organic phase and raffinate; the volume ratio of the adopted extractant is 1-10: 1-10 of Cyanex572 and sulfonated kerosene, wherein the volume ratio of an organic phase to a water phase in the extraction process is 1-10: 10, the extraction time is 10-30 min, and the extraction stage number is 3-5;
(4) Back-extracting the scandium-containing organic phase to obtain scandium-rich solution and organic phase; the stripping agent is hydrochloric acid solution with the concentration of 2-5 mol/L, and the volume ratio of the organic phase to the water phase in the stripping process is 1-5: 1, the back extraction time is 10-30 min, and the back extraction stage number is 1-5;
(5) And adding a oxalic acid solution into the scandium-rich solution to precipitate to obtain scandium oxalate.
2. The method for selectively extracting scandium according to claim 1, wherein in the step (5), the oxalic acid solution is 10-30wt% oxalic acid solution; the pH of the solution in the precipitation process is 1.5-2.0.
3. The method for selectively extracting scandium according to any one of claims 1-2, wherein scandium oxalate obtained in the step (5) is calcined to obtain a scandium oxide product.
4. The method for selectively extracting scandium according to claim 3, wherein the calcination temperature is 500-600 ℃ and the calcination time is 2-4 hours.
5. The method for selectively extracting scandium according to any one of claims 1 to 2, wherein in step (1), the particle size of the finely ground lateritic nickel ore is-0.074 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111544544.0A CN114480887B (en) | 2021-12-16 | 2021-12-16 | Method for selectively extracting scandium from lateritic nickel ore by sulfuric acid roasting-water leaching method |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102345019A (en) * | 2011-10-25 | 2012-02-08 | 北京矿冶研究总院 | Method for treating brown iron type laterite-nickel ore |
| CN103468978A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Method for extracting scandium from lateritic nickel ore sulfuric acid leaching solution |
| CN103468980A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Method for extracting scandium from lateritic nickel ore |
| WO2015021926A1 (en) * | 2013-08-15 | 2015-02-19 | 中国恩菲工程技术有限公司 | Method for processing laterite-nickel ore and method for recycling scandium |
| CN109777973A (en) * | 2019-03-20 | 2019-05-21 | 中国恩菲工程技术有限公司 | The method and device of Selectively leaching scandium from smelting laterite-nickel ores slag |
| CN109811122A (en) * | 2019-03-20 | 2019-05-28 | 中国恩菲工程技术有限公司 | The extracting method of rare earth oxide |
-
2021
- 2021-12-16 CN CN202111544544.0A patent/CN114480887B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102345019A (en) * | 2011-10-25 | 2012-02-08 | 北京矿冶研究总院 | Method for treating brown iron type laterite-nickel ore |
| CN103468978A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Method for extracting scandium from lateritic nickel ore sulfuric acid leaching solution |
| CN103468980A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Method for extracting scandium from lateritic nickel ore |
| WO2015021926A1 (en) * | 2013-08-15 | 2015-02-19 | 中国恩菲工程技术有限公司 | Method for processing laterite-nickel ore and method for recycling scandium |
| CN109777973A (en) * | 2019-03-20 | 2019-05-21 | 中国恩菲工程技术有限公司 | The method and device of Selectively leaching scandium from smelting laterite-nickel ores slag |
| CN109811122A (en) * | 2019-03-20 | 2019-05-28 | 中国恩菲工程技术有限公司 | The extracting method of rare earth oxide |
Non-Patent Citations (2)
| Title |
|---|
| Recovery of scandium from leaching solutions of tungsten residue using solvent extraction with Cyanex 572;Huaping Nie et al.;Hydrometallurgy;第175卷;117-123 * |
| 从钨渣中浸出氧化钪的试验研究;梁焕龙等;湿法冶金;第34卷(第02期);114-116 * |
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