CN109797295B - Method for extracting cobalt from cobalt-containing iron concentrate - Google Patents
Method for extracting cobalt from cobalt-containing iron concentrate Download PDFInfo
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- CN109797295B CN109797295B CN201910116904.3A CN201910116904A CN109797295B CN 109797295 B CN109797295 B CN 109797295B CN 201910116904 A CN201910116904 A CN 201910116904A CN 109797295 B CN109797295 B CN 109797295B
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- 239000010941 cobalt Substances 0.000 title claims abstract description 155
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 155
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 133
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000012141 concentrate Substances 0.000 title claims abstract description 68
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002386 leaching Methods 0.000 claims abstract description 80
- 238000000605 extraction Methods 0.000 claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 239000012074 organic phase Substances 0.000 claims description 17
- 229910052720 vanadium Inorganic materials 0.000 claims description 15
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000012716 precipitator Substances 0.000 claims description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 8
- FQMNUIZEFUVPNU-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co] FQMNUIZEFUVPNU-UHFFFAOYSA-N 0.000 claims description 7
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 3
- 229940039790 sodium oxalate Drugs 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 5
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 32
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 239000003350 kerosene Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 229910001784 vanadium mineral Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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
Abstract
The invention relates to a method for extracting cobalt from cobalt-containing iron ore concentrate, belonging to the technical field of cobalt extraction chemical industry. The invention solves the technical problem that the cobalt content in the iron ore concentrate is rare and the cobalt in the iron ore concentrate can not be effectively extracted. The invention discloses a method for extracting cobalt from cobalt-containing iron ore concentrate, which comprises the steps of mixing a part of cobalt-containing iron ore concentrate with water, adding an auxiliary leaching agent for leaching to obtain a cobalt-containing solution, taking the cobalt-containing solution as a leaching agent for leaching the rest of cobalt-containing iron ore concentrate in batches, using a leaching solution obtained after each leaching for leaching the next batch of iron ore concentrate to obtain a high-cobalt solution, and then extracting, back-extracting and precipitating cobalt to obtain cobalt precipitate. The invention realizes the high-efficiency extraction of cobalt from the cobalt-containing iron concentrate, has high leaching rate and back extraction rate of cobalt, simple and easy process, wide application range and low cost, and has very high social benefit and economic benefit.
Description
Technical Field
The invention belongs to the technical field of cobalt extraction chemical industry, and particularly relates to a method for extracting cobalt from cobalt-containing iron ore concentrate.
Background
Cobalt has excellent physical and chemical properties and is an important raw material for high-temperature alloys, magnetic materials, chemical industry, electronic industry and the like. There are hundreds of kinds of cobalt minerals found in nature, and industrial cobalt-containing ores are divided into two main categories, namely sulfide ores and oxide ores, wherein the sulfide ores are generally smelted by a pyrogenic process to produce various cobalt products, and the oxide ores are generally treated by a reduction acid leaching process except for smelting cobalt alloys by a pyrogenic process because cobalt is a high-priced cobalt oxide, such as cobalt earth ores and cobalt hydroores. In addition to the recovery of cobalt from cobalt ore by smelting, cobalt is often associated with other metal ores, such as nickel ore, zinc ore, pyrite, and the recovery of cobalt from associated ores has become an important source of cobalt production, and in the smelting of associated ores, cobalt is mostly produced as a by-product of cobalt slag, such as cobalt slag, from which cobalt is then extracted by means of reduction leaching.
The reserves of vanadium in China are in the fourth place of the world, more than 10 provinces and cities (regions) in China all have vanadium mineral resources, but the reserves of vanadium are mainly concentrated in Panzhihua areas in Sichuan and Chengdu areas in Hebei, particularly the reserves of vanadium in Panzhihua areas are quite rich, the reserve of proven vanadium-titanium magnetite is nearly 100 hundred million tons, the reserve of vanadium pentoxide is 1578 million tons, and the cobalt content is more than 200 million tons.
The cobalt content of vanadium titano-magnetite is very rare in relation to the total amount of vanadium titano-magnetite and it is therefore very uneconomical if cobalt is extracted directly from vanadium titano-magnetite. A more feasible method is to further extract cobalt from the iron ore concentrate after vanadium extraction. However, in practice, such low levels of minerals are rarely extracted.
Disclosure of Invention
The invention solves the technical problem that the cobalt content in the iron ore concentrate is rare and the cobalt in the iron ore concentrate can not be effectively extracted.
The technical scheme for solving the problems is to provide a method for extracting cobalt from cobalt-containing iron ore concentrate, which comprises the following steps:
a. crushing the cobalt-iron containing concentrate to remove coarser particles;
b. mixing a part of crushed cobalt-containing iron ore concentrate with water, adding an auxiliary leaching agent for leaching, and performing liquid-solid separation to obtain a cobalt-containing solution, wherein the auxiliary leaching agent is at least one of ferrous sulfate, sodium thiosulfate and sodium sulfite;
c. b, taking the cobalt-containing solution obtained in the step b as a leaching agent, leaching the residual cobalt-containing iron ore concentrate in batches, wherein a leaching solution obtained after each leaching is used for leaching the next batch of iron ore concentrate, so that a high-cobalt leaching solution is obtained by performing cyclic leaching for 10-20 times, and adding an extracting agent into the high-cobalt solution to obtain a high-cobalt organic phase;
d. and (3) carrying out back extraction on the high-cobalt organic phase to obtain cobalt-rich liquid, adding a precipitator, and carrying out solid-liquid separation to obtain cobalt precipitate.
Wherein the cobalt-containing iron ore concentrate is obtained by performing high-temperature roasting on the iron ore concentrate subjected to sodium modification vanadium extraction, and the high-temperature roasting condition is 1200 ℃ for 2 hours.
Wherein, the average particle size of the iron ore concentrate after vanadium extraction is less than 0.125mm after crushing; the cobalt content in the cobalt-containing iron ore concentrate is more than 0.01 percent.
Wherein the pH value is controlled to be 0.2-0.8 in the leaching process in the step b and the step c; the leaching temperature in the step b and the step c is 20-80 ℃.
Wherein the liquid-solid ratio of the water to the iron ore concentrate in the step b is 1: 1-4: 1; and (c) in the step (b), the molar ratio of the leaching aid to the cobalt content in the cobalt-containing iron ore concentrate is 2.0-10.0.
Wherein the stirring speed in the leaching in the step b and the step c is 100-500 r/min; the leaching time in the step b and the step c is 30-180 min.
Wherein, the extractant in the step c is P204, namely di (2-ethylhexyl) phosphate; the extraction time is 10-120 min.
Wherein, the stripping agent in the step d is sulfuric acid, and the concentration is 10-20%.
Wherein, the precipitator in the step d is at least one of ammonium oxalate, sodium oxalate and potassium oxalate.
Wherein the molar ratio of the precipitator to the cobalt in the cobalt-rich liquid in the step d is 1.5-3.
The invention has the beneficial effects that:
the invention adopts the adaptive leaching aid to leach, matches with the mode of circularly leaching and enriching cobalt, and finally adopts certain extraction and back extraction processes, particularly aims at the iron concentrate after vanadium extraction, realizes the high-efficiency extraction of cobalt from the cobalt-containing iron concentrate, and has high leaching rate and back extraction rate of cobalt; the invention has the advantages of simple and easy process, wide application range, low cost and high social and economic benefits.
Detailed Description
The invention provides a method for extracting cobalt from cobalt-containing iron ore concentrate, which comprises the following steps:
a. crushing the cobalt-iron containing concentrate to remove coarser particles;
b. mixing water with a part of crushed cobalt-containing iron ore concentrate, adding an auxiliary leaching agent for leaching, and performing liquid-solid separation to obtain a cobalt-containing solution, wherein the auxiliary leaching agent is at least one of ferrous sulfate, sodium thiosulfate and sodium sulfite;
c. b, taking the cobalt-containing solution obtained in the step b as a leaching agent, leaching the residual cobalt-containing iron ore concentrate in batches, wherein a leaching solution obtained after each leaching is used for leaching the cobalt-containing iron ore concentrate in the next batch, so that high-cobalt solution is obtained by performing cyclic leaching for 10-20 times, and adding an extracting agent into the high-cobalt solution to obtain a high-cobalt organic phase;
d. and (3) carrying out back extraction on the high-cobalt organic phase to obtain cobalt-rich liquid, adding a precipitator, and carrying out solid-liquid separation to obtain cobalt precipitate.
Wherein the cobalt-containing iron ore concentrate is obtained by performing high-temperature roasting on the iron ore concentrate subjected to sodium modification vanadium extraction, and the high-temperature roasting condition is 1200 ℃ for 2 hours.
Wherein, the average particle size of the cobalt-iron containing concentrate after crushing is less than 0.125 mm; the cobalt content in the cobalt-containing iron ore concentrate is more than 0.01 percent.
Wherein the pH value is controlled to be 0.2-0.8 in the leaching process in the step b and the step c; the leaching temperature in the step b and the step c is 20-80 ℃.
Wherein the liquid-solid ratio of the water to the iron ore concentrate in the step b is 1: 1-4: 1; and (c) in the step (b), the molar ratio of the leaching aid to the cobalt content of the cobalt-iron ore concentrate is 2.0-10.0.
Wherein the stirring speed in the leaching in the step b and the step c is 100-500 r/min; the leaching time in the step b and the step c is 30-180 min.
Wherein the extractant in the step c is P204, and specifically, the P204 is dissolved in the kerosene, and the mass fraction is controlled to be 10-20%; the extraction time is 10-120 min, preferably 10-60 min.
Wherein the volume ratio of the organic phase to the aqueous phase extracted in the step c is 10-50.
Wherein, the stripping agent in the step d is sulfuric acid, and the concentration is 10-20%.
Wherein the ratio of the organic phase to the sulfuric acid in the back extraction in the step d is 0.5-1.
Wherein the back extraction time in the step d is 20-120 min.
Wherein, the precipitator in the step d is at least one of ammonium oxalate, sodium oxalate and potassium oxalate.
Wherein the molar ratio of the precipitator to the cobalt in the cobalt-rich liquid in the step d is 1.5-3.
Wherein the precipitation time in the step d is 40-180 min.
The invention is further illustrated by the following examples.
The chemical compositions and contents of the vanadium-extracted cobalt-containing iron concentrate used in the examples are shown in table 1.
TABLE 1
Example 1
a. Crushing the cobalt-containing iron ore concentrate after vanadium extraction to be less than 0.125mm, wherein the quantity reaches 20000 g;
b. mixing 1000g of the mixed solution with 1000ml of water, adding sulfuric acid to adjust the pH value to 0.5, adding 0.02mol of ferrous sulfate, keeping the temperature at 40 ℃, reacting for 60min, and filtering and separating to obtain a low-cobalt solution;
c. b, taking the low-cobalt solution in the step b as a leaching agent, leaching the rest cobalt-containing iron ore concentrate in batches, wherein each batch is leached with 1000g under the same leaching condition as the step b, and the leachate obtained after each leaching is used for leaching the next batch of iron ore concentrate and is cyclically leached for 20 times to obtain a high-cobalt solution, wherein the cobalt content reaches 5.1g/L, the volume is 1000ml, and the leaching rate is 85%;
d. extracting the high cobalt solution, wherein an organic phase is 25% of P204+ 75% of sulfonated kerosene which is saponified in advance, and performing 8-grade countercurrent extraction, wherein the extraction flow ratio (qo/qa) is 1/5; the loaded organic phase was washed with 3 stages of countercurrent with 1.0mol/L sulfuric acid solution at a wash flow ratio (qo/qa) of 1/8. The cobalt-containing organic phase is subjected to 3-stage back extraction by using a sulfuric acid solution with the mass fraction of 10%, the back extraction flow ratio (qo/qa) is 45/10, and the cobalt back extraction rate is more than 99.8%. After the cobalt back-extraction liquid is acidified by oxalic acid, 0.13mol of ammonium oxalate is added, and the solution is precipitated for 40min to obtain 12.46g of cobalt oxalate.
Example 2
a. Crushing the cobalt-containing iron ore concentrate after vanadium extraction to be less than 0.125mm, wherein the quantity reaches 20000 g;
b. mixing 1000g of the mixed solution with 1000ml of water, adding sulfuric acid to adjust the pH value to 0.4, adding 0.015mol of sodium thiosulfate, keeping the temperature at 50 ℃, reacting for 100min, and filtering and separating to obtain a low-cobalt solution;
c. b, taking the low-cobalt solution in the step b as a leaching agent, leaching the rest cobalt-containing iron ore concentrate in batches, wherein each batch is leached with 1000g under the same leaching condition as the step b, and the leachate obtained after each leaching is used for leaching the next batch of iron ore concentrate and is cyclically leached for 20 times to obtain a high-cobalt solution, wherein the cobalt content reaches 5.4g/L, the volume is 1000ml, and the leaching rate is 90%;
d. extracting the high cobalt solution, wherein an organic phase is 25% of P204+ 75% of sulfonated kerosene which is saponified in advance, and performing 8-grade countercurrent extraction, wherein the extraction flow ratio (qo/qa) is 1/4; the loaded organic phase was washed with 3 stages of countercurrent with 1.5mol/L sulfuric acid solution at a wash flow ratio (qo/qa) of 1/6. The cobalt-containing organic phase is subjected to 3-stage back extraction by using a sulfuric acid solution with the mass fraction of 10%, the back extraction flow ratio (qo/qa) is 35/10, and the cobalt back extraction rate is more than 99.8%. After the cobalt back-extraction liquid is acidified by oxalic acid, 0.2mol of ammonium oxalate is added, and the solution is precipitated for 40min to obtain 13.2g of cobalt oxalate.
Example 3
a. Crushing the cobalt-containing iron ore concentrate after vanadium extraction to be less than 0.125mm, wherein the quantity reaches 15000 g;
b. mixing 1000g of the mixed solution with 1000ml of water, adding sulfuric acid to adjust the pH value to 0.5, adding 0.03mol of sodium sulfite, keeping the temperature at 40 ℃, reacting for 60min, and filtering and separating to obtain a low-cobalt solution;
c. b, taking the low-cobalt solution in the step b as a leaching agent, leaching the rest cobalt-containing iron ore concentrate in batches, wherein each batch is leached with 1000g, the leaching conditions are the same as those in the step b, the leachate obtained after each leaching is used for leaching the next batch of iron ore concentrate, and the leaching is circulated for 15 times to obtain a high-cobalt solution, wherein the cobalt content reaches 4.27g/L, the volume is 1000ml, and the leaching rate is 95%;
d. extracting the high cobalt solution, wherein an organic phase is 25% of P204+ 75% of sulfonated kerosene which is saponified in advance, and performing 8-grade countercurrent extraction, wherein the extraction flow ratio (qo/qa) is 1/6; the loaded organic phase was washed with 2.0mol/L sulfuric acid solution in 3 stages in countercurrent, the washing flow ratio (qo/qa) being 1/6. The cobalt-containing organic phase is subjected to 3-stage back extraction by using a sulfuric acid solution with the mass fraction of 15%, the back extraction flow ratio (qo/qa) is 25/6, and the cobalt back extraction rate is more than 99.8%. After the cobalt back-extraction liquid is acidified by oxalic acid, 0.14mol of ammonium oxalate is added, and the solution is precipitated for 40min to obtain 10.3g of cobalt oxalate.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications, equivalent variations and modifications made to the above embodiment according to the technical spirit of the present invention still fall within the scope of the technical solution of the present invention.
Claims (8)
1. The method for extracting cobalt from the cobalt-containing iron concentrate is characterized by comprising the following steps of:
a. crushing the cobalt-iron containing concentrate to remove coarser particles; the average particle size of the cobalt-iron-containing concentrate after crushing is less than 0.125 mm; the mass percentage of cobalt in the cobalt-iron-containing concentrate is 0.01-0.03%;
b. mixing a part of crushed cobalt-containing iron ore concentrate with water, adding an auxiliary leaching agent for leaching, and performing liquid-solid separation to obtain a cobalt-containing solution, wherein the auxiliary leaching agent is at least one of ferrous sulfate, sodium thiosulfate and sodium sulfite; controlling the pH value to be 0.2-0.8 in the leaching process; the leaching temperature is 20-80 ℃; the liquid-solid ratio of the water to the iron ore concentrate is 1: 1-4: 1, and the molar ratio of the leaching aid to the cobalt content in the cobalt-containing iron ore concentrate is 2.0-10.0; leaching for 30-180 min;
c. b, taking the cobalt-containing solution obtained in the step b as a leaching agent, leaching the residual cobalt-containing iron ore concentrate in batches, wherein a leaching solution obtained after each leaching is used for leaching the next batch of cobalt-containing iron ore concentrate, so that a high-cobalt leaching solution is obtained by performing cyclic leaching for 10-20 times, and adding an extracting agent into the high-cobalt solution to obtain a high-cobalt organic phase; controlling the pH value to be 0.2-0.8 in the leaching process; the leaching temperature is 20-80 ℃; leaching for 30-180 min;
d. and (3) carrying out back extraction on the high-cobalt organic phase to obtain a cobalt-rich solution, adding a precipitator to precipitate cobalt, and carrying out solid-liquid separation to obtain a cobalt precipitate.
2. The method of claim 1, wherein the cobalt is extracted from the cobalt-containing iron concentrate, and the method comprises the following steps: the cobalt-containing iron ore concentrate in the step a is iron ore concentrate obtained after high-temperature roasting and sodium modification vanadium extraction; the high-temperature roasting condition is that roasting is carried out for 2 hours at 1200 ℃.
3. A method for extracting cobalt from a cobalt-containing iron concentrate according to claim 1 or 2, characterized in that: and c, using the same amount of the cobalt-containing iron concentrate for leaching in each batch in the step c, and using the same amount of the cobalt-containing iron concentrate in the step b.
4. The method of claim 1, wherein the cobalt is extracted from the cobalt-containing iron concentrate, and the method comprises the following steps: and c, stirring speed is 100-500 r/min during leaching in the step b and the step c.
5. The method of claim 1, wherein the cobalt is extracted from the cobalt-containing iron concentrate, and the method comprises the following steps: in the step c, the extractant is P204; the extraction time is 10-120 min.
6. The method of claim 1, wherein the cobalt is extracted from the cobalt-containing iron concentrate, and the method comprises the following steps: in the step d, the stripping agent is sulfuric acid, and the concentration is 10-20%.
7. The method of claim 1, wherein the cobalt is extracted from the cobalt-containing iron concentrate, and the method comprises the following steps: in the step d, the precipitator is at least one of ammonium oxalate, sodium oxalate and potassium oxalate.
8. The method of claim 1, wherein the cobalt is extracted from the cobalt-containing iron concentrate, and the method comprises the following steps: and d, the molar ratio of the precipitator to the cobalt in the cobalt-rich liquid in the step d is 1.5-3.
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| CN112250120B (en) * | 2020-12-21 | 2021-04-02 | 矿冶科技集团有限公司 | Method for preparing ternary precursor and lithium carbonate by using waste lithium ion battery black powder and nickel cobalt sulfide ore in synergy mode and application |
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