CN118109692A - Method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag - Google Patents
Method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag Download PDFInfo
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- CN118109692A CN118109692A CN202410230242.3A CN202410230242A CN118109692A CN 118109692 A CN118109692 A CN 118109692A CN 202410230242 A CN202410230242 A CN 202410230242A CN 118109692 A CN118109692 A CN 118109692A
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- scandium
- back extraction
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052706 scandium Inorganic materials 0.000 title claims abstract description 71
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 64
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000002893 slag Substances 0.000 title claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000003723 Smelting Methods 0.000 title claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000005065 mining Methods 0.000 title claims abstract description 18
- 238000004064 recycling Methods 0.000 title claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 84
- 239000012074 organic phase Substances 0.000 claims abstract description 60
- 238000002386 leaching Methods 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 239000002253 acid Substances 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 11
- 239000010941 cobalt Substances 0.000 claims abstract description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003599 detergent Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 4
- 125000005587 carbonate group Chemical group 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims 1
- 238000005191 phase separation Methods 0.000 abstract description 13
- 239000012071 phase Substances 0.000 abstract description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052748 manganese Inorganic materials 0.000 abstract description 5
- 239000011572 manganese Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 5
- 239000001099 ammonium carbonate Substances 0.000 description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910017709 Ni Co Inorganic materials 0.000 description 3
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- XTOOSYPCCZOKMC-UHFFFAOYSA-L [OH-].[OH-].[Co].[Ni++] Chemical compound [OH-].[OH-].[Co].[Ni++] XTOOSYPCCZOKMC-UHFFFAOYSA-L 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000010409 ironing Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 nickel cobalt manganese iron aluminum Chemical compound 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007790 solid phase 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0221—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
- C22B60/0226—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag, which comprises the following steps: carrying out acid leaching treatment on laterite-nickel ore smelting iron-making aluminum slag to obtain leaching liquid and leaching slag; extracting the leaching solution by using DY366 extractant to obtain raffinate and a loaded organic phase I; washing the loaded organic phase I by using a detergent to obtain a nickel-containing washing liquid and a loaded organic phase II; carrying out back extraction on the loaded organic phase II by using a first back extraction agent to obtain uranium-containing back extraction liquid and a loaded organic phase III; and carrying out back extraction on the loaded organic phase III by using a second back extraction agent to obtain scandium-containing back extraction liquid and a blank organic phase. According to the invention, through acid leaching, extraction and two-step back extraction, no solid slag phase is generated in the back extraction process, the back extraction time is short, the phase separation is fast, and the efficient separation of scandium, uranium, cobalt, nickel and manganese in the iron-aluminum slag leaching solution is realized.
Description
Technical Field
The invention belongs to the technical field of metal recovery, and particularly relates to a method for recovering scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag.
Background
The laterite-nickel ore contains a large amount of nickel cobalt manganese iron aluminum and a small amount of scandium and uranium elements, and scandium and uranium are difficult to directly recycle because of various impurities and high content, and are usually sent to iron-aluminum slag and MHP products. Scandium and uranium in MHP are sent to an extractant of an iron-aluminum slag and P204 impurity removal extraction line in the wet cobalt-nickel-manganese recovery process, scandium and uranium in the extractant are difficult to strip off on the extraction line, and the impurity removal effect and the phase separation speed of the extraction line are seriously affected after scandium concentration in P204 is enriched.
At present, organic phosphoric acid extractant such as P204, P507, TBP and the like is basically adopted for scandium recovery, and then alkaline stripping agent is used for precipitating scandium in the form of hydroxide. In the method, scandium extraction rate can be over 95%, but a large amount of solids are generated in the back extraction process, the phase separation of oil, water and solid phases in the system is extremely slow, the reaction temperature is over 70 ℃, the reaction time is over 30min, the scandium back extraction rate and the phase separation speed can be higher, and the extractant can be recycled after acid regeneration after back extraction. The process flow is long, the reaction temperature is high, the back extraction and phase separation time is long, the alkali consumption is high, and the cost is high. For recycling uranium in laterite-nickel ores, no suitable process is found.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a method for recycling scandium and uranium from laterite-nickel mining and smelting iron-aluminum slag, which aims to solve the problems of high scandium recycling reaction temperature, long back extraction and phase separation time and incapability of synchronously recycling uranium at present.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
The invention provides a method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag, which comprises the following steps:
(1) Carrying out acid leaching treatment on laterite-nickel ore smelting iron-making aluminum slag to obtain leaching liquid and leaching slag;
(2) Extracting the leaching solution by using DY366 extractant to obtain raffinate and a loaded organic phase I;
(3) Washing the loaded organic phase I by using a detergent to obtain a nickel-containing washing liquid and a loaded organic phase II;
(4) Carrying out back extraction on the loaded organic phase II by using a first back extraction agent to obtain uranium-containing back extraction liquid and a loaded organic phase III;
(5) And carrying out back extraction on the loaded organic phase III by using a second back extraction agent to obtain scandium-containing back extraction liquid and a blank organic phase.
Preferably, the acid leaching treatment in the step (1) has a liquid-solid ratio of 1-3:1, a pH of 1.0-3.5, a temperature of 50-70 ℃ and a time of 0.5-2 h; scandium concentration in the leaching solution is more than or equal to 0.6g/L.
Preferably, the concentration of the extractant in the step (2) is 10-40%, and the ratio of the extractant to the leaching solution is (0.5-4): 1, the extraction reaction temperature is 10-50 ℃, and the extraction stage number is 1-10.
Preferably, the detergent in the step (3) is hydrochloric acid and/or sulfuric acid solution, and the concentration of the detergent is 0.5-2N.
Preferably, the washing conditions in step (3) are: the ratio of the loaded organic phase to the detergent is (1-20): 1, the temperature is 10-50 ℃, and the washing stage number is 1-10.
Preferably, in the step (4), the first stripping agent is carbonate and/or bicarbonate solution, and the concentration of the first stripping agent is 1-2 mol/L.
Preferably, in the step (4), the loaded organic phase II is (1-10) compared with the first stripping agent: 1, the back extraction reaction temperature is 10-50 ℃, and the back extraction stage number is 1-10.
Preferably, in the step (5), the second stripping agent is 2-10N acid solution, and the acid solution is one or two of sulfuric acid and hydrochloric acid.
Preferably, the third loaded organic phase is (1-10) compared with the second stripping agent: 1, the back extraction reaction temperature is 10-50 ℃, and the back extraction stage number is 1-10.
Preferably, the step further comprises the step of mixing the leaching residue obtained in the step (1) with the raffinate obtained in the step (2) to recover nickel and cobalt.
The beneficial effects of the invention are as follows:
(1) According to the invention, scandium and uranium in laterite-nickel ore smelting iron-making aluminum slag and MHP refining iron-removing slag are circularly leached and enriched, and then scandium and uranium are extracted and recovered, so that the treatment capacity of an extraction procedure is greatly reduced, and the leached slag can be leached and recovered for the second time to recover cobalt-nickel-manganese solution without scandium and uranium, thereby eliminating the adverse effect of scandium and uranium on the recovery of cobalt-nickel-manganese by back-end extraction.
(2) According to the invention, scandium and uranium can be selectively recovered from the leaching solution after scandium and uranium enrichment through one-step extraction, the scandium extraction rate is over 96%, the uranium extraction rate is over 80%, metals such as cobalt, nickel and manganese are remained in the raffinate, the cobalt, nickel and manganese loss is lower than 5%, the efficient separation of scandium, uranium and cobalt, nickel and manganese in the iron-aluminum slag leaching solution is realized, and the comprehensive recovery and utilization of metal elements are performed.
(3) The back extraction process of the extractant used in the invention can be carried out at normal temperature without heating, no third phase is generated in the back extraction process, and the phase separation is rapid and efficient.
(4) The invention utilizes different stripping agents to strip scandium and uranium in the loaded organic phase step by step to respectively obtain uranium-containing stripping solution and scandium-containing stripping solution, wherein the scandium concentration in the uranium-containing stripping solution is below 5mg/L, and the uranium concentration in the scandium-containing stripping solution is below 1 mg/L.
Drawings
In order to more clearly illustrate the technical solution of the embodiments of the present invention, the following description will briefly explain the drawings of the embodiments.
FIG. 1 is a flow chart of a method for recovering scandium and uranium from lateritic nickel mining iron-making aluminum slag.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Referring to fig. 1, the method for recovering scandium and uranium from lateritic nickel mining and smelting iron-aluminum slag provided by the invention comprises the following steps:
(1) Carrying out acid leaching treatment on laterite-nickel ore smelting iron-making aluminum slag by utilizing sulfuric acid, wherein the liquid-solid ratio of the acid leaching treatment is 1-3:1, the pH value is 1.0-3.5, the temperature is 50-70 ℃ and the time is 0.5-2 h, so as to obtain leaching liquid and leaching slag; the acid leaching process can be repeatedly circulated for many times until the scandium concentration in the leaching solution is more than or equal to 0.6g/L.
(2) Extracting the leaching solution by using DY366 extractant, wherein the concentration of the extractant is 10-40%, and the ratio of the extractant to the leaching solution is (0.5-4): 1, extracting reaction temperature is 10-50 ℃, extraction stage number is 1-10, and raffinate and loaded organic phase I are obtained; wherein the raffinate contains cobalt, nickel and manganese, and the loaded organic phase I contains scandium and uranium.
(3) Washing the first loaded organic phase by using hydrochloric acid and/or sulfuric acid solution with the concentration of 0.5-2N as a detergent, wherein the ratio of the first loaded organic phase to the detergent is (1-20): 1, the temperature is 10-50 ℃, the washing stage number is 1-10, and a nickel-containing washing liquid and a loaded organic phase II are obtained; the nickel-containing washing liquid is incorporated into the leaching liquid and extracted.
(4) Carrying out back extraction on a second loaded organic phase by using carbonate and/or bicarbonate solution with the concentration of 1-2 mol/L as a first back extraction agent, wherein the second loaded organic phase is (1-10) compared with the first back extraction agent: 1, the back extraction reaction temperature is 10-50 ℃, the back extraction stage number is 1-10, and uranium-containing back extraction liquid and a loaded organic phase III are obtained; carbonates include, but are not limited to, sodium carbonate, ammonium carbonate, bicarbonates include, but are not limited to, one or more of sodium bicarbonate, ammonium bicarbonate.
(5) Carrying out back extraction on a third loaded organic phase by using an acid solution with the concentration of 2-10N as a second back extraction agent, wherein the acid solution is one or two of sulfuric acid and hydrochloric acid, and the third loaded organic phase is (1-10) compared with the second back extraction agent: 1, the back extraction reaction temperature is 10-50 ℃, the back extraction stage number is 1-10, and scandium-containing back extraction liquid and a blank organic phase are obtained.
In some preferred embodiments, step (1) further comprises acid leaching the cobalt nickel hydroxide refined de-ironing slag to effect simultaneous recovery of scandium and uranium in the cobalt nickel hydroxide refined de-ironing slag.
In some preferred embodiments, the above step further comprises mixing the leaching residue obtained in step (1) with the raffinate obtained in step (2) to recover nickel cobalt, and the recovery method of nickel and cobalt is conventional in the art.
According to the invention, different scandium and uranium leaching and enriching processes and different kinds of extractants are adopted, scandium and uranium in the leaching solution can be enriched, the volume of a solution for extracting scandium and uranium after enrichment is greatly reduced, scandium and uranium are extracted, scandium and uranium are subjected to step-wise normal-temperature stripping, no solid slag phase is generated in the stripping process, the stripping time is short, the phase separation is fast, scandium and uranium elements in a system are efficiently recovered at low cost, and adverse effects of scandium and uranium enrichment on the recovery of cobalt, nickel and manganese at the rear end are avoided.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
Example 1
(1) Mixing laterite-nickel ore smelting iron-making aluminum slag and MHP refining iron-removing slag thereof with water and sulfuric acid for acid leaching treatment, wherein the solid ratio of the acid leaching solution is 2:1, the pH value is 3.0, the temperature is 65 ℃, leaching is carried out for 1h, filtering, mixing filtrate with the iron-aluminum slag and adding sulfuric acid, continuing acid leaching treatment according to the conditions, and filtering to obtain leaching solution and leaching slag;
(2) Countercurrent extraction of the leachate with DY366 at a concentration of 30% at 25℃to a 1.2:1 ratio of stage 4 to obtain a raffinate and a loaded organic phase I;
(3) Countercurrent washing the loaded organic phase with 1N sulfuric acid at 25 ℃ according to the ratio of 5:1 for 4 stages, separating phases to obtain a nickel-containing washing liquid and a loaded organic phase II, and mixing the nickel-containing washing liquid into a leaching liquid for extraction;
(4) Countercurrent and back-extracting the loaded organic phase II with 1mol/L ammonium bicarbonate solution at 25 ℃ according to the ratio of 4:1 for 3 stages, and obtaining uranium-containing back-extracting solution and loaded organic phase III after phase separation;
(5) And carrying out countercurrent back extraction on the loaded organic phase by using a three-purpose 4N sulfuric acid solution at 25 ℃ according to the ratio of 10:1 for 3 stages, and obtaining scandium-containing back extraction liquid and a blank organic phase after phase separation.
The main metal concentrations in the leachate, raffinate, uranium-containing strip liquor and scandium-containing strip liquor are shown in table 1 below under the above conditions:
TABLE 1 Main Metal concentration of each solution (Unit: g/L)
| Main element | Ni | Co | Mn | Sc | U | Fe |
| Leachate solution | 33.1 | 2.53 | 2.59 | 0.6 | 0.29 | 0.038 |
| Raffinate from a process for the preparation of a liquid extract | 31 | 2.12 | 2.47 | 0.014 | 0.026 | 0.002 |
| Uranium-containing back extraction liquid | 0.065 | 0.003 | 0.002 | 0.004 | 0.75 | 0.001 |
| Scandium-containing back extraction liquid | 0.25 | 0.001 | 0.001 | 5.56 | 0.001 | 0.21 |
Example 2
(1) Mixing laterite-nickel ore smelting iron-aluminum slag and MHP refining iron-removing slag thereof with water and sulfuric acid for acid leaching treatment, wherein the solid ratio of the acid leaching solution is 3:1, the pH value is 2.0, the temperature is 60 ℃, leaching is carried out for 1.5 hours, filtering liquid is mixed with the iron-aluminum slag and added with sulfuric acid, cyclic acid leaching treatment is carried out according to the conditions, and leaching liquid and leaching slag are obtained after filtering;
(2) Countercurrent extraction of the leachate with DY366 at a concentration of 20% at 35 ℃ for 6 stages in a ratio of 1.4:1 to obtain a raffinate and a loaded organic phase I;
(3) Countercurrent washing the loaded organic phase with 0.5N hydrochloric acid at 35 ℃ according to the ratio of 4:1 for 5 grades, separating phases to obtain a nickel-containing washing liquid and a loaded organic phase II, and mixing the nickel-containing washing liquid into the leaching liquid for extraction;
(4) Countercurrent back-extracting the loaded organic phase with 1.5mol/L ammonium bicarbonate solution at 45 ℃ according to the ratio of 3:1 for 3-level, and separating phases to obtain uranium-containing back-extracting solution and loaded organic phase III;
(5) And carrying out countercurrent back extraction on the three-purpose 2N sulfuric acid solution loaded with the organic phase at 35 ℃ according to the ratio of 5:1 for 3 stages, and obtaining scandium-containing back extraction liquid and a blank organic phase after phase separation.
The main metal concentrations in the leachate, raffinate, uranium-containing strip liquor and scandium-containing strip liquor under the above conditions are shown in table 2 below:
TABLE 2 Main Metal concentrations (units: g/L) for each solution
| Main element | Ni | Co | Mn | Sc | U | Fe |
| Leachate solution | 54.8 | 2.14 | 2.13 | 1.02 | 0.42 | 0.11 |
| Raffinate from a process for the preparation of a liquid extract | 49.7 | 1.82 | 1.77 | 0.014 | 0.036 | 0.001 |
| Uranium-containing back extraction liquid | 0.23 | 0.005 | 0.002 | 0.004 | 0.91 | 0.001 |
| Scandium-containing back extraction liquid | 0.056 | 0.002 | 0.002 | 2.88 | 0.001 | 0.45 |
Example 3
(1) Mixing laterite-nickel ore smelting iron-making aluminum slag and MHP refining iron-removing slag thereof with water and sulfuric acid for acid leaching treatment, wherein the solid ratio of the acid leaching solution is 1.5:1, the pH value is 4.0, the temperature is 70 ℃, leaching is carried out for 2 hours, filtering, mixing filtrate with the iron-aluminum slag and adding sulfuric acid, carrying out cyclic acid leaching treatment according to the conditions, and filtering to obtain acid leaching solution and leached slag;
(2) Countercurrent extraction of the wash liquor with 15% DY366 at 50℃for 4 stages in a 2:1 ratio to give a raffinate and a loaded organic phase I;
(3) Countercurrent washing the loaded organic phase with 1.5N sulfuric acid at 50 ℃ according to the ratio of 7:1 for 4 stages, separating phases to obtain a nickel-containing washing liquid and a loaded organic phase II, and mixing the nickel-containing washing liquid into the leaching liquid for extraction;
(4) Countercurrent and back-extracting the loaded organic phase with 2mol/L ammonium bicarbonate solution at 45 ℃ according to the ratio of 6:1 for 4 stages, and obtaining uranium-containing back-extracting solution and loaded organic phase III after phase separation;
(5) And carrying out countercurrent back extraction on the loaded organic phase by using a 3N sulfuric acid solution at 45 ℃ according to a ratio of 6:1 for 4 levels, and obtaining scandium-containing back extraction liquid and a blank organic phase after phase separation.
The main metal concentrations in the leachate, raffinate, uranium-containing strip liquor and scandium-containing strip liquor under the above conditions are shown in table 3 below:
TABLE 3 Main Metal concentrations (units: g/L) for each solution
| Main element | Ni | Co | Mn | Sc | U | Fe |
| Leachate solution | 32.7 | 2.65 | 2.64 | 1.15 | 0.35 | 0.001 |
| Raffinate from a process for the preparation of a liquid extract | 28.5 | 2.43 | 2.51 | 0.0008 | 0.013 | 0.001 |
| Uranium-containing back extraction liquid | 0.18 | 0.005 | 0.003 | 0.003 | 1.02 | 0.001 |
| Scandium-containing back extraction liquid | 0.044 | 0.001 | 0.002 | 3.54 | 0.001 | 0.017 |
In summary, scandium and uranium in the iron-aluminum slag are leached firstly, nickel and cobalt can be recycled from leaching slag after enrichment, scandium and uranium in the leaching liquid are selectively extracted by using a novel extractant, cobalt and nickel are still remained in the raffinate and can be recycled, and then the separation of scandium and uranium is realized by a two-stage back extraction process, so that a uranium-containing back extraction liquid with low scandium and a scandium back extraction liquid without basically uranium are respectively obtained, and the comprehensive utilization of metal elements in the lateritic nickel ore is realized.
It should be noted that, the foregoing embodiments all belong to the same inventive concept, and the descriptions of the embodiments have emphasis, and where the descriptions of the individual embodiments are not exhaustive, reference may be made to the descriptions of the other embodiments.
The foregoing examples merely illustrate embodiments of the invention and are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag, which is characterized by comprising the following steps:
(1) Carrying out acid leaching treatment on laterite-nickel ore smelting iron-making aluminum slag to obtain leaching liquid and leaching slag;
(2) Extracting the leaching solution by using DY366 extractant to obtain raffinate and a loaded organic phase I;
(3) Washing the loaded organic phase I by using a detergent to obtain a nickel-containing washing liquid and a loaded organic phase II;
(4) Carrying out back extraction on the loaded organic phase II by using a first back extraction agent to obtain uranium-containing back extraction liquid and a loaded organic phase III;
(5) And carrying out back extraction on the loaded organic phase III by using a second back extraction agent to obtain scandium-containing back extraction liquid and a blank organic phase.
2. The method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag according to claim 1, wherein in the step (1), the acid leaching treatment has a liquid-solid ratio of 1-3:1, a pH of 1.0-3.5, a temperature of 50-70 ℃ and a time of 0.5-2 h; scandium concentration in the leaching solution is more than or equal to 0.6g/L.
3. The method for recovering scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag according to claim 1, wherein the concentration of the extractant in the step (2) is 10 to 40%, and the ratio of the extractant to the leaching solution is (0.5 to 4): 1, the extraction temperature is 10-50 ℃, and the extraction stage number is 1-10.
4. The method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag according to claim 1, wherein the detergent in the step (3) is hydrochloric acid and/or sulfuric acid solution, and the concentration of the detergent is 0.5-2N.
5. The method for recovering scandium and uranium from lateritic nickel mining iron-making aluminum slag according to claim 1, wherein the washing conditions in step (3) are: the ratio of the loaded organic phase to the detergent is (1-20): 1, the temperature is 10-50 ℃, and the washing stage number is 1-10.
6. The method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag according to claim 1, wherein in the step (4), the first stripping agent is carbonate and/or bicarbonate solution, and the concentration of the first stripping agent is 1-2 mol/L.
7. The method for recovering scandium and uranium from lateritic nickel mining and smelting iron and aluminum slag according to claim 1, wherein in the step (4), the ratio of the loaded organic phase two to the first stripping agent is (1 to 10): 1, the back extraction temperature is 10-50 ℃, and the back extraction stage number is 1-10.
8. The method for recycling scandium and uranium from lateritic nickel mining and smelting iron-making aluminum slag according to claim 1, wherein in the step (5), the second stripping agent is an acid solution of 2-10N, and the acid solution is one or both of sulfuric acid and hydrochloric acid.
9. The method for recovering scandium and uranium from lateritic nickel mining and smelting aluminum slag according to claim 1, wherein in step (5), the ratio of the loaded organic phase three to the second stripping agent is (1 to 10): 1, the back extraction temperature is 10-50 ℃, and the back extraction stage number is 1-10.
10. The method for recycling scandium and uranium from lateritic nickel mining and smelting iron-aluminum slag according to claim 1, further comprising recycling nickel and cobalt after mixing leaching slag obtained in the step (1) with raffinate obtained in the step (2).
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