CN117385207A - Method for recycling scandium in ultra-lean vanadium titano-magnetite iron tailings - Google Patents
Method for recycling scandium in ultra-lean vanadium titano-magnetite iron tailings Download PDFInfo
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- CN117385207A CN117385207A CN202311685886.3A CN202311685886A CN117385207A CN 117385207 A CN117385207 A CN 117385207A CN 202311685886 A CN202311685886 A CN 202311685886A CN 117385207 A CN117385207 A CN 117385207A
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- 229910052706 scandium Inorganic materials 0.000 title claims abstract description 64
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 22
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 19
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004064 recycling Methods 0.000 title claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 14
- 229910052742 iron Inorganic materials 0.000 title abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 69
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 239000012074 organic phase Substances 0.000 claims abstract description 31
- 238000002386 leaching Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 48
- 238000005406 washing Methods 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 239000012535 impurity Substances 0.000 claims description 17
- 235000006408 oxalic acid Nutrition 0.000 claims description 16
- LQPWUWOODZHKKW-UHFFFAOYSA-K scandium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Sc+3] LQPWUWOODZHKKW-UHFFFAOYSA-K 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 12
- 239000003350 kerosene Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 4
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000009854 hydrometallurgy Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 49
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 239000013049 sediment Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 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 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229910000542 Sc alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- MOCSSSMOHPPNTG-UHFFFAOYSA-N [Sc].[Y] Chemical compound [Sc].[Y] MOCSSSMOHPPNTG-UHFFFAOYSA-N 0.000 description 1
- LUKDNTKUBVKBMZ-UHFFFAOYSA-N aluminum scandium Chemical compound [Al].[Sc] LUKDNTKUBVKBMZ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021652 non-ferrous alloy Inorganic materials 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- -1 scandium sodium halogen Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for recycling scandium in ultra-lean vanadium titano-magnetite tailings, and relates to the technical field of hydrometallurgy. Comprising the following steps: grinding the ultra-lean vanadium titano-magnetite tailings to obtain a sample with the particle size smaller than 0.074 mm; mixing a sample with sodium hydroxide and roasting to obtain a roasted material; mixing the roasting material with sulfuric acid solution, and leaching under stirring to obtain leaching solution; mixing the leaching solution with an extractant, extracting to obtain scandium-loaded organic phase and the like. The method provided by the invention realizes the recovery of scandium in the ultra-lean vanadium titano-magnetite iron tailings in the Maillard region and the Liaoxi region, and the recovery rate of scandium reaches 88%.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for recycling scandium in ultra-lean vanadium titano-magnetite tailings.
Background
Scandium is a transition metal element, the element symbol Sc, is a soft, silvery metal, often mixed with rare earth ores, such as black-thin gold ores. Scandium is also contained in some tin and tungsten ores, and the scandium yttrium is contained in a higher content. Scandium has been used for preparing products such as aluminum scandium alloy, fuel cell, scandium sodium halogen lamp, tracer, laser crystal, etc. due to its own special physical and chemical properties, and has wide application prospect in fields such as special steel, nonferrous alloy, high-performance ceramic, catalyst, etc. At present, a certain amount of scandium contained in the ultra-lean vanadium titano-magnetite iron tailings in the Dewar region and the Liaoxi region cannot be effectively recovered, so that the resource waste is caused.
Disclosure of Invention
In order to solve the problems, the invention provides a method for recycling scandium in the ultra-lean vanadium titano-magnetite tailings, and the method provided by the invention realizes recycling scandium in the ultra-lean vanadium titano-magnetite tailings in the Maillard region and the Liaoxi region.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for recycling scandium in ultra-lean vanadium titano-magnetite tailings, which comprises the following steps:
1) Grinding the ultra-lean vanadium titano-magnetite tailings to obtain a sample with the particle size smaller than 0.074 mm;
2) Mixing the sample obtained in the step 1) with sodium hydroxide, and roasting to obtain a roasting material;
3) Mixing the roasting material obtained in the step 2) with sulfuric acid solution, and leaching under stirring to obtain leaching solution;
the concentration of the sulfuric acid solution is 6mol/L;
4) Mixing the leaching solution obtained in the step 3) with an extracting agent, and extracting to obtain scandium-loaded organic phase;
the extractant comprises P204 and kerosene;
5) Washing the scandium-loaded organic phase obtained in the step 4) by using a washing water solution to obtain a scandium-loaded organic phase after impurity removal;
the washing water solution comprises sulfuric acid and hydrogen peroxide;
6) Mixing the organic phase loaded with scandium after impurity removal obtained in the step 5) with sodium hydroxide solution, performing back extraction to obtain a back extract, and filtering the back extract to obtain crude scandium hydroxide precipitate;
the concentration of the sodium hydroxide solution is 2.5mol/L;
7) Dissolving the crude scandium hydroxide precipitate obtained in the step 6) by using a hydrochloric acid solution, adjusting the pH value to be 1.2-1.5, and mixing with oxalic acid to obtain a precipitate;
8) And 7) sequentially drying and burning the precipitate obtained in the step 7) to obtain scandium oxide.
Preferably, the mass ratio of the sample in the step 2) to the sodium hydroxide is 1:2-3;
the roasting conditions include: the temperature was 550℃and the time was 4 hours.
Preferably, the volume ratio of the mass of the roasting material in the step 3) to the sulfuric acid solution is 1g to 3ml;
the stirring adopts magnetic stirring, and the rotating speed of the magnetic stirring is 800-1000 rpm.
Preferably, the leaching conditions in the step 3) include: the temperature is 60-80 ℃ and the time is 12-14 h.
Preferably, the volume ratio of the P204 to the kerosene in the step 4) is 1:4;
the volume ratio of the leaching liquid to the extractant is 1:4-8;
the conditions of the extraction include: shaking for 15min, and standing for 30min.
Preferably, the concentration of sulfuric acid in the washing water solution in the step 5) is 4.5mol/L, and the concentration of hydrogen peroxide is 1mol/L.
Preferably, the volume ratio of the scandium-loaded organic phase to the washing water solution in the step 5) is 5:1;
the number of washes was 4.
Preferably, the volume ratio of scandium-loaded organic phase to sodium hydroxide solution after the impurity removal in the step 6) is 4:1;
the conditions of the stripping include: the temperature is 70 ℃, shake is carried out for 20min, and the mixture is kept stand for 30min.
Preferably, the mass ratio of the crude scandium hydroxide precipitate to oxalic acid in the step 7) is 1:4;
the mixing conditions include: oxalic acid was added while stirring at 90 ℃.
Preferably, the drying temperature in the step 8) is 100-105 ℃;
the firing conditions include: the temperature was 850℃and the time was 2 hours.
Advantageous effects
The method provided by the invention realizes the recovery of scandium in the ultra-lean vanadium titano-magnetite iron tailings in the Maillard region and the Liaoxi region, and the recovery rate of scandium reaches 88%.
Detailed Description
The invention provides a method for recycling scandium in ultra-lean vanadium titano-magnetite tailings, which comprises the following steps:
1) Grinding the ultra-lean vanadium titano-magnetite tailings to obtain a sample with the particle size smaller than 0.074 mm;
2) Mixing the sample obtained in the step 1) with sodium hydroxide, and roasting to obtain a roasting material;
3) Mixing the roasting material obtained in the step 2) with sulfuric acid solution, and leaching under stirring to obtain leaching solution;
the concentration of the sulfuric acid solution is 6mol/L;
4) Mixing the leaching solution obtained in the step 3) with an extracting agent, and extracting to obtain scandium-loaded organic phase;
the extractant comprises P204 and kerosene;
5) Washing the scandium-loaded organic phase obtained in the step 4) by using a washing water solution to obtain a scandium-loaded organic phase after impurity removal;
the washing water solution comprises sulfuric acid and hydrogen peroxide;
6) Mixing the organic phase loaded with scandium after impurity removal obtained in the step 5) with sodium hydroxide solution, performing back extraction to obtain a back extract, and filtering the back extract to obtain crude scandium hydroxide precipitate;
the concentration of the sodium hydroxide solution is 2.5mol/L;
7) Dissolving the crude scandium hydroxide precipitate obtained in the step 6) by using a hydrochloric acid solution, adjusting the pH value to be 1.2-1.5, and mixing with oxalic acid to obtain a precipitate;
8) And 7) sequentially drying and burning the precipitate obtained in the step 7) to obtain scandium oxide.
According to the invention, the ultra-lean vanadium titano-magnetite tailings are ground, so that a sample with the particle size smaller than 0.074mm is obtained. The conditions for the grinding are not particularly limited, and conventional methods may be employed. In the invention, the steps of filtering and drying are further carried out after grinding, so that a sample is obtained, and the temperature of drying is 80-100 ℃.
The obtained sample is mixed with sodium hydroxide and roasted to obtain a roasted material. In the invention, the mass ratio of the sample to the sodium hydroxide is preferably 1:2-3. In the present invention, the conditions of the firing preferably include: the temperature was 550℃and the time was 4 hours.
Mixing the obtained roasting material with sulfuric acid solution, and leaching under stirring to obtain leaching liquid; the concentration of the sulfuric acid solution is 6mol/L. In the invention, the ratio of the mass of the roasting material to the volume of the sulfuric acid solution is preferably 1 g/3 ml. In the invention, magnetic stirring is preferably adopted, and the rotating speed of the magnetic stirring is preferably 800-1000 rpm. In the present invention, the leaching conditions preferably include: the temperature is 60-80 ℃ and the time is 12-14 h. Realizes the leaching rate of scandium above 90 percent.
The obtained leaching solution is mixed with an extractant and extracted to obtain scandium-loaded organic phase; the extractant includes P204 and kerosene. In the invention, the volume ratio of the P204 to the kerosene is preferably 1:4, the invention has no special limitation on the evolution of the P204 and the kerosene, and the invention can be realized by adopting a conventional commercial product. In the invention, the volume ratio of the leaching solution to the extractant is preferably 1:4-8. In the present invention, the conditions of the extraction preferably include: shaking for 15min, and standing for 30min. Finally, the extraction rate of scandium can reach more than 99.4 percent.
The obtained scandium-loaded organic phase is washed by a washing water solution to obtain a scandium-loaded organic phase after impurity removal; the washing water solution comprises sulfuric acid and hydrogen peroxide. In the invention, the concentration of sulfuric acid in the aqueous solution is preferably 4.5mol/L, and the concentration of hydrogen peroxide is preferably 1mol/L. In the invention, the volume ratio of the scandium-loaded organic phase to the washing water solution is preferably 5:1; the number of times of washing is preferably 4.
Mixing the obtained organic phase loaded with scandium after impurity removal with sodium hydroxide solution, carrying out back extraction to obtain a back extract, and filtering the back extract to obtain crude scandium hydroxide precipitate; the concentration of the sodium hydroxide solution is 2.5mol/L. In the invention, the volume ratio of scandium-loaded organic phase to sodium hydroxide solution after impurity removal is preferably 4:1. In the present invention, the conditions of the stripping preferably include: the temperature is 70 ℃, shake is carried out for 20min, and the mixture is kept stand for 30min.
According to the method, the obtained crude scandium hydroxide precipitate is dissolved by hydrochloric acid solution, the pH value is adjusted to be 1.2-1.5, and then the obtained crude scandium hydroxide precipitate is mixed with oxalic acid to obtain the precipitate. In the present invention, the mass ratio of the crude scandium hydroxide precipitate to oxalic acid is preferably 1:4. In the present invention, the mixing conditions preferably include: oxalic acid was added while stirring at 90 ℃.
The obtained precipitate is dried and burned in sequence to obtain scandium oxide. In the invention, the drying temperature is 100-105 ℃. In the present invention, the firing conditions preferably include: the temperature was 850℃and the time was 2 hours.
The present invention will be described in detail with reference to examples for further illustration of the invention, but they should not be construed as limiting the scope of the invention.
Example 1
a, grinding the scandium grade of 0.0197 percent (mass percent) in the iron tailings of certain beard ultra-lean vanadium titano-magnetite to be less than 0.074mm and accounting for more than 90 percent, filtering, drying at 90 ℃, uniformly mixing according to the mass ratio of the tailings to the sodium hydroxide of 1:2, and roasting in a muffle furnace at 550 ℃ for 4 hours;
b, naturally cooling the roasted sample to room temperature, adding 6mol/L sulfuric acid solution according to the sample mass and sulfuric acid volume ratio of 1g to 3ml, leaching at 65 ℃ for 12 hours, leaching under magnetic stirring at 800rpm, and finally obtaining scandium leaching rate of 90.85%;
c, uniformly mixing and oscillating the leaching solution and an extractant (P204: kerosene with a volume ratio of 1:4) for 15min according to a volume ratio of 4:1, standing and layering for 30min to obtain an organic phase loaded with scandium, wherein the scandium extraction rate is 99.43%;
d, uniformly mixing the scandium-loaded organic phase obtained by extraction with a washing water solution (4.5 mol/L sulfuric acid and 1mol/L hydrogen peroxide) according to a volume ratio of 5:1, oscillating for 10min, standing and layering for 20min, discharging raffinate, and repeatedly washing for 4 times to finally obtain a scandium-loaded organic phase after impurity removal, wherein the scandium loss rate in the impurity removal process is 1.27%;
e, adding a 2.5mol/L sodium hydroxide solution with the temperature of 70 ℃ and the organic phase loaded with scandium after impurity removal according to the volume ratio of 1:4, uniformly mixing, oscillating for 20min, standing and layering for 30min, generating 3 items of oil, water and sediment, filtering to obtain crude scandium hydroxide sediment, wherein the scandium loss rate in the process is 0.74%;
f, heating the coarse scandium hydroxide with excessive hydrochloric acid solution (the volume percentage content is 20 percent), adjusting the pH value of the solution to 1.4 by (1+1) ammonia water after the solid is completely dissolved, heating to 90 ℃, and mixing oxalic acid according to the mass ratio: adding solid oxalic acid into the solution while stirring to perform oxalic acid precipitation, clarification and suction filtration, drying scandium oxalate at 100 ℃, heating to 850 ℃ and burning for 2 hours to obtain Sc with purity not less than 99% 2 O 3 The scandium loss rate of the product in the process is 0.58%;
g, preparing Sc with purity more than or equal to 99% 2 O 3 The product realizes a scandium recovery of 88.01%.
Example 2
a, grinding the scandium grade of 0.0197 percent (mass percent) in the iron tailings of certain beard ultra-lean vanadium titano-magnetite to be less than 0.074mm and accounting for more than 90 percent, filtering, drying at 100 ℃, uniformly mixing according to the mass ratio of the tailings to the sodium hydroxide of 1:3, and roasting in a muffle furnace at 550 ℃ for 4 hours;
b, naturally cooling the roasted sample to room temperature, adding 6mol/L sulfuric acid solution according to the sample mass and sulfuric acid volume ratio of 1g to 3ml, leaching at 65 ℃ for 14 hours, leaching under magnetic stirring at 800rpm, and finally obtaining scandium leaching rate of 91.25%;
c, uniformly mixing and oscillating the leaching solution and an extractant (P204: kerosene with a volume ratio of 1:4) for 15min according to a volume ratio of 4:1, standing and layering for 30min to obtain an organic phase loaded with scandium, wherein the scandium extraction rate is 99.45%;
d, uniformly mixing the scandium-loaded organic phase obtained by extraction with a washing water solution (4.5 mol/L sulfuric acid and 1mol/L hydrogen peroxide) according to a volume ratio of 5:1, oscillating for 10min, standing and layering for 20min, discharging raffinate, and repeatedly washing for 4 times to finally obtain a scandium-loaded organic phase after impurity removal, wherein the scandium loss rate in the impurity removal process is 1.25%;
e, adding a 2.5mol/L sodium hydroxide solution with the temperature of 70 ℃ and the organic phase loaded with scandium after impurity removal according to the volume ratio of 1:4, uniformly mixing, oscillating for 20min, standing and layering for 30min, generating 3 items of oil, water and sediment, filtering to obtain crude scandium hydroxide sediment, wherein the scandium loss rate in the process is 0.73%;
f, heating the coarse scandium hydroxide with excessive hydrochloric acid solution (the volume percentage content is 20 percent), adjusting the pH value of the solution to 1.4 by (1+1) ammonia water after the solid is completely dissolved, heating to 90 ℃, and mixing oxalic acid according to the mass ratio: adding solid oxalic acid into the solution while stirring to perform oxalic acid precipitation, clarification and suction filtration, drying scandium oxalate at 105 ℃, heating to 850 ℃ and burning for 2 hours to obtain Sc with purity not less than 99% 2 O 3 The scandium loss rate of the product in the process is 0.54%;
g, preparing Sc with purity more than or equal to 99% 2 O 3 The recovery rate of scandium in the product is 88.12%.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.
Claims (5)
1. The method for recycling scandium in the ultra-lean vanadium titano-magnetite tailings is characterized by comprising the following steps:
1) Grinding the ultra-lean vanadium titano-magnetite tailings to obtain a sample with the particle size smaller than 0.074 mm;
2) Mixing the sample obtained in the step 1) with sodium hydroxide, and roasting to obtain a roasting material;
3) Mixing the roasting material obtained in the step 2) with sulfuric acid solution, and leaching under stirring to obtain leaching solution;
the concentration of the sulfuric acid solution is 6mol/L;
4) Mixing the leaching solution obtained in the step 3) with an extracting agent, and extracting to obtain scandium-loaded organic phase;
the extractant is P204 and kerosene;
5) Washing the scandium-loaded organic phase obtained in the step 4) by using a washing water solution to obtain a scandium-loaded organic phase after impurity removal;
the washing water solution comprises sulfuric acid and hydrogen peroxide;
6) Mixing the organic phase loaded with scandium after impurity removal obtained in the step 5) with sodium hydroxide solution, performing back extraction to obtain a back extract, and filtering the back extract to obtain crude scandium hydroxide precipitate;
the concentration of the sodium hydroxide solution is 2.5mol/L;
7) Dissolving the crude scandium hydroxide precipitate obtained in the step 6) by using a hydrochloric acid solution, adjusting the pH value to be 1.2-1.5, and mixing with oxalic acid to obtain a precipitate;
8) Sequentially drying and burning the precipitate obtained in the step 7) to obtain scandium oxide;
the mass ratio of the sample in the step 2) to the sodium hydroxide is 1:2-3;
the roasting conditions include: the temperature is 550 ℃ and the time is 4 hours;
the volume ratio of the P204 to the kerosene in the step 4) is 1:4;
the volume ratio of the leaching liquid to the extractant is 1:4-8;
the conditions of the extraction include: shaking for 15min, and standing for 30min;
the concentration of sulfuric acid in the washing water solution in the step 5) is 4.5mol/L, and the concentration of hydrogen peroxide is 1mol/L;
the volume ratio of scandium-loaded organic phase to sodium hydroxide solution after impurity removal in the step 6) is 4:1;
the conditions of the stripping include: oscillating for 20min at 70 ℃, and standing for 30min;
the mass ratio of the coarse scandium hydroxide precipitate to oxalic acid in the step 7) is 1:4;
the mixing conditions include: oxalic acid was added while stirring at 90 ℃.
2. The method according to claim 1, wherein the volume ratio of the mass of the calcined material to the sulfuric acid solution in step 3) is 1 g/3 ml;
the stirring adopts magnetic stirring, and the rotating speed of the magnetic stirring is 800-1000 rpm.
3. The method according to claim 1, wherein the leaching conditions of step 3) include: the temperature is 60-80 ℃ and the time is 12-14 h.
4. The method according to claim 1, characterized in that the volume ratio of the scandium loaded organic phase to the aqueous washing solution of step 5) is 5:1;
the number of washes was 4.
5. The method according to claim 1, wherein the drying temperature in step 8) is 100-105 ℃;
the firing conditions include: the temperature was 850℃and the time was 2 hours.
Priority Applications (1)
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| FI884137A0 (en) * | 1987-09-11 | 1988-09-08 | Gte Laboratories Inc | JONBYTARMETOD FOER UTVINNING AV SKANDIUM. |
| CN106636686A (en) * | 2016-11-17 | 2017-05-10 | 攀枝花学院 | Method for extracting scandium from artificial rutile leaching mother liquor produced by hydrochloric acid method |
| US20170233849A1 (en) * | 2016-02-11 | 2017-08-17 | Bloom Energy Corporation | Method of refining of scandium oxide from concentrates using solvent extraction |
| CN112978805A (en) * | 2021-01-26 | 2021-06-18 | 北京科技大学 | Comprehensive recovery method of titanium, iron and sulfate radicals in titanium white waste acid |
| CN115852177A (en) * | 2022-12-29 | 2023-03-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling scandium from fused salt chlorination dust collection slag |
| CN117165792A (en) * | 2023-09-11 | 2023-12-05 | 承德宝通矿业有限公司 | Technological process for recycling scandium from vanadium titano-magnetite tailings |
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| FI884137A0 (en) * | 1987-09-11 | 1988-09-08 | Gte Laboratories Inc | JONBYTARMETOD FOER UTVINNING AV SKANDIUM. |
| US20170233849A1 (en) * | 2016-02-11 | 2017-08-17 | Bloom Energy Corporation | Method of refining of scandium oxide from concentrates using solvent extraction |
| CN106636686A (en) * | 2016-11-17 | 2017-05-10 | 攀枝花学院 | Method for extracting scandium from artificial rutile leaching mother liquor produced by hydrochloric acid method |
| CN112978805A (en) * | 2021-01-26 | 2021-06-18 | 北京科技大学 | Comprehensive recovery method of titanium, iron and sulfate radicals in titanium white waste acid |
| CN115852177A (en) * | 2022-12-29 | 2023-03-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling scandium from fused salt chlorination dust collection slag |
| CN117165792A (en) * | 2023-09-11 | 2023-12-05 | 承德宝通矿业有限公司 | Technological process for recycling scandium from vanadium titano-magnetite tailings |
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