CN114717415A - Method for separating multi-metal mixed solution - Google Patents
Method for separating multi-metal mixed solution Download PDFInfo
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- CN114717415A CN114717415A CN202210321811.6A CN202210321811A CN114717415A CN 114717415 A CN114717415 A CN 114717415A CN 202210321811 A CN202210321811 A CN 202210321811A CN 114717415 A CN114717415 A CN 114717415A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 59
- 239000011259 mixed solution Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000002184 metal Substances 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 204
- 239000012074 organic phase Substances 0.000 claims abstract description 147
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 113
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 107
- 229910052738 indium Inorganic materials 0.000 claims abstract description 63
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052742 iron Inorganic materials 0.000 claims abstract description 47
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 33
- CEKJAYFBQARQNG-UHFFFAOYSA-N cadmium zinc Chemical compound [Zn].[Cd] CEKJAYFBQARQNG-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 30
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 30
- 239000011701 zinc Substances 0.000 claims abstract description 30
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 29
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 238000007127 saponification reaction Methods 0.000 claims description 8
- 239000003350 kerosene Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 abstract description 27
- 238000000926 separation method Methods 0.000 abstract description 12
- 239000003960 organic solvent Substances 0.000 abstract description 10
- 238000000746 purification Methods 0.000 abstract description 7
- 238000005272 metallurgy Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 description 9
- 238000003723 Smelting Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000009854 hydrometallurgy Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- NJWNEWQMQCGRDO-UHFFFAOYSA-N indium zinc Chemical compound [Zn].[In] NJWNEWQMQCGRDO-UHFFFAOYSA-N 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000010310 metallurgical process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 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
- 239000012535 impurity Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B15/00—Other processes for the manufacture of iron from iron compounds
-
- 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
- C22B17/00—Obtaining cadmium
- C22B17/04—Obtaining cadmium by wet 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
-
- 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
- C22B58/00—Obtaining gallium or indium
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for separating a multi-metal mixed solution, and belongs to the technical field of wet metallurgy. The method comprises the following steps: extracting the multi-metal ion mixed solution by using an organic phase solution so as to transfer metal elements to be extracted in the multi-metal ion mixed solution to the organic phase solution; and then, extracting the organic phase solution by using a zinc-cadmium stripping agent, an indium stripping agent and an iron stripping agent in sequence, so that zinc elements, cadmium elements, indium elements and iron elements in the organic phase solution are transferred to the corresponding stripping agents. According to the method provided by the invention, the metal elements in the mixed solution are extracted into the organic solvent containing the extracting agent at one time, and then different stripping agents are adopted for carrying out back extraction step by step, so that different metal elements are respectively transferred into the corresponding stripping agents from the organic solvent, and the separation and purification of the multi-metal mixed solution are realized. In addition, the method provided by the invention is simple, efficient, easy to implement, high in equipment utilization rate and easy to realize industrial application.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for separating a multi-metal mixed solution.
Background
The wet metallurgy has the characteristics of investment saving, quick response, short flow, environmental friendliness and the like, obtains good economic benefits, social benefits and environmental benefits in industrial application, and is more and more widely applied in the field of metallurgy. However, a large amount of metal elements remain in by-products generated in the metallurgical process, how to separate, extract and purify the metal elements becomes a key constraint factor for the development of hydrometallurgy, and the feasibility of a hydrometallurgy scheme is directly determined. Therefore, the metal element separation technology is the main driving force for the forward development of the hydrometallurgy technology.
In the waste materials or by-products generated in the hydrometallurgical process, various metal mixtures exist, and due to the complex and various types of the metal mixtures, the targeted separation and purification technology needs to be adopted for different metallurgical processes and different reaction products. The waste leachate generated by the zinc-indium smelting process contains a large amount of metal elements such as indium, cadmium, zinc and iron, and because the composition of the mixed solution is complex, a separation and purification method aiming at the solution is not available in the prior art.
Therefore, in the technical field of hydrometallurgy, it is necessary to develop a method for separating a multi-metal mixed solution, so as to solve the problem of how to separate and purify metal elements such as indium, cadmium, zinc and iron in a waste leachate generated in a zinc-indium smelting process.
Disclosure of Invention
The invention mainly aims to provide a method for separating a multi-metal mixed solution, which aims to solve the problem of how to separate and purify metal elements such as indium, cadmium, zinc and iron in a waste leaching solution generated in a zinc-indium smelting process.
The invention is realized by the following technical scheme:
the first aspect of the embodiment of the invention discloses a method for separating a multi-metal mixed solution, which comprises the following steps:
step 1, extracting a multi-metal ion mixed solution by using an organic phase solution so as to transfer metal elements to be extracted in the multi-metal ion mixed solution to an organic phase solution to obtain a first loaded organic phase solution; the metal elements to be extracted comprise iron elements, zinc elements, cadmium elements and indium elements;
and 4, extracting the third loaded organic phase solution by using an iron stripping agent so as to transfer the iron element in the third loaded organic phase solution to the iron stripping agent, thereby obtaining a fourth loaded organic phase solution and an iron stripping agent solution for extracting the iron element.
Further, the pH value of the mixed solution of the multiple metal ions is within the range of 1.5-2.
Further, the organic phase solution comprises 30 volume percent of P204 extractant and 70 volume percent of sulfonated kerosene.
Further, step 1 comprises:
and mixing the multi-metal ion mixed solution with the organic phase solution according to the volume ratio of 10:2, oscillating for a first target duration, standing for layering, and then separating to obtain the first loaded organic phase solution.
Further, the zinc-cadmium back-extraction agent is a sulfuric acid solution of 150g/L, the indium back-extraction agent is a hydrochloric acid solution of 3mol/L, and the iron back-extraction agent is a hydrochloric acid solution of 6 mol/L.
Further, step 2 comprises:
mixing the zinc-cadmium stripping agent with the first loaded organic phase solution according to the volume ratio of 2:10, oscillating for a second target duration, standing for layering, and separating to obtain a second loaded organic phase solution and a zinc-cadmium stripping solution extracted with zinc elements and cadmium elements.
Further, step 3 comprises:
and mixing the indium stripping agent and the second loaded organic phase solution according to the volume ratio of 2:10, oscillating for a third target duration, standing for layering, and then separating to obtain a third loaded organic phase solution and an indium stripping agent solution for extracting indium element.
Further, step 4 comprises:
mixing the iron stripping agent with the third loaded organic phase solution according to the volume ratio of 2:10, oscillating for a fourth target time, standing for layering, and separating to obtain a fourth loaded organic phase solution and an iron stripping agent solution for extracting iron elements.
Further, the method further comprises:
adding a sodium hydroxide solution into the fourth loaded organic phase solution for saponification, mixing for a fifth target time length, standing for layering, and then separating to obtain a regenerated organic phase solution;
wherein, the regenerated organic phase solution is used as the organic phase solution for extracting the mixed solution of the multiple metal ions in the step 1.
Further, the saponification rate of the fourth organic phase-loaded solution was 70%.
The invention provides a method for separating a multi-metal mixed solution, which comprises the following steps of firstly, extracting the multi-metal ion mixed solution by using an organic phase solution so as to transfer metal elements to be extracted in the multi-metal ion mixed solution into the organic phase solution; and then, extracting the organic phase solution by using a zinc-cadmium stripping agent, an indium stripping agent and an iron stripping agent in sequence, so that the zinc element, the cadmium element, the indium element and the iron element in the organic phase solution are transferred to the corresponding stripping agents. According to the method provided by the invention, the metal elements in the mixed solution are extracted into the organic solvent containing the extracting agent at one time, and then different stripping agents are adopted for carrying out back extraction step by step, so that different metal elements are respectively transferred into the corresponding stripping agents from the organic solvent, and the separation and purification of the multi-metal mixed solution are realized. In addition, the method provided by the invention is simple, efficient, easy to implement, high in equipment utilization rate and easy to realize industrial application.
Compared with the prior art, the invention has the following specific beneficial effects:
1) realizing the separation of different metal elements. The invention adopts a solvent extraction technology, utilizes different binding capacities of an extracting agent to different metal ions so as to require different characteristics to an extraction environment system, extracts valuable metal ions into an organic solvent containing the extracting agent at one time, and then adopts different stripping agents to perform back extraction step by step, so that different metal ions are respectively transferred into corresponding stripping agents from the organic solvent, thereby realizing the separation and purification of multiple metal elements.
2) The method provided by the invention is simple and efficient. The method can extract various metal elements by simple extraction operation, has simple and easy extraction operation, simple reaction conditions, short consumed time, easy acquisition of required instruments and low cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments of the present invention will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without inventive labor.
FIG. 1 is a flow chart of the steps for separating a mixed multi-metal solution according to an embodiment of the present invention;
fig. 2 is a flow chart of the extraction of a multi-metal mixed solution according to an embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings in which embodiments of the invention are shown. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Detailed description of the preferred embodiment
An embodiment of the present invention provides a method for separating a mixed solution of multiple metals, where fig. 1 is a flow chart of steps of the method, and as shown in fig. 1, the method includes:
step 1, extracting a multi-metal ion mixed solution by using an organic phase solution so as to transfer metal elements to be extracted in the multi-metal ion mixed solution to an organic phase solution to obtain a first loaded organic phase solution; the metal elements to be extracted comprise iron elements, zinc elements, cadmium elements and indium elements;
extraction refers to a separation method in which a substance is extracted from one solvent into another solvent by utilizing the difference in solubility between the substance and the two mutually incompatible solvents, thereby separating the solute from the solvent. The multi-metal ion mixed liquid contains a plurality of metal elements including iron, zinc, cadmium and indium. Illustratively, the multi-metal ion mixed liquid can contain 1-4g/L of iron element, 1-10mg/L of indium element, 1-5mg/L of cadmium element and 1-10g/L of zinc element.
And adding the organic phase solution into the multi-metal ion mixed solution by utilizing the characteristic that the solubility of the organic phase solution to the metal elements is greater than that of the mixed solution so as to transfer the multiple metal elements into the organic phase solution. Then, the organic phase solution and the mixed solution are separated by standing and layering by utilizing the characteristic that the organic phase solution is incompatible with the mixed solution. At this time, the plural metal elements originally in the mixed solution are transferred to the organic phase solution, and the first loaded organic phase solution is obtained.
Optionally, the PH of the mixed solution of the multiple metal ions is in the range of 1.5-2.
The PH value affects the solubility of the solute, so the PH value of the solution needs to be adjusted to a proper range, specifically, 1.5-2 before the extraction of the multi-metal ion mixed solution. If the pH of the mixed liquor is too high, the metal elements can form precipitates which are filtered out along with other impurities, and the subsequent extraction operation is not facilitated.
Optionally, the organic phase solution is 30% by volume of the P204 extractant and 70% by volume of sulfonated kerosene.
The P204 extractant is fully called di (2-ethylhexyl) phosphate and belongs to an acidic extractant. Sulfonated kerosene is also named as No. 260 solvent oil and is formed by sulfonating kerosene. The two extracting agents form an organic phase solution according to a certain proportion, so that iron elements, zinc elements, cadmium elements and indium elements are extracted from the mixed solution. It should be noted that the composition and the proportion of the organic phase solution need to be considered not only to extract the four metal elements, but also to achieve the technical effect of the subsequent fractional extraction. In addition, the P204 extracting agent and the sulfonated kerosene belong to common extracting agents, and the raw materials are easy to obtain and have lower cost.
Optionally, step 1 includes:
and mixing the multi-metal ion mixed solution with the organic phase solution according to the volume ratio of 10:2, oscillating for a first target time, standing for layering, and separating to obtain the first loaded organic phase solution.
The amount of the adopted organic phase solution needs to reach a certain proportion, so that all free metal elements in the multi-metal ion mixed solution can be extracted, and the waste caused by remaining in the mixed solution is avoided. And mixing the multi-metal ion mixed solution and the organic phase solution, and oscillating, so that the two solutions are fully and uniformly mixed, specifically, the oscillation time can reach the first target time to ensure full reaction. For example, the first target duration may be 5 min.
the first loaded organic phase solution comprises iron element, zinc element, cadmium element and indium element. By adding the zinc-cadmium stripping agent into the solution, the zinc element and the cadmium element are transferred into the zinc-cadmium stripping agent by utilizing the characteristic that the solubility of the zinc element and the cadmium element in the zinc-cadmium stripping agent is higher than that of the organic phase solution, so that the extraction of the zinc element and the cadmium element is realized, and the zinc-cadmium stripping solution containing the zinc element and the cadmium element and the second loaded organic phase solution containing the iron element and the indium element are obtained.
Optionally, step 2 includes:
and mixing the zinc-cadmium stripping agent with the first loaded organic phase solution according to the volume ratio of 2:10, oscillating for a second target time length, standing for layering and then separating to obtain a second loaded organic phase solution and a zinc-cadmium stripping solution for extracting zinc elements and cadmium elements.
The zinc-cadmium back-extraction agent and the organic phase solution can be mixed according to the volume ratio of 2:10, so that the using amount of the zinc-cadmium back-extraction agent is ensured, the zinc element and the cadmium element in the first loaded organic phase solution can be completely transferred into the zinc-cadmium back-extraction agent, and the situation that residual elements exist in the organic phase solution and can pollute iron elements and indium elements which are extracted subsequently is avoided. Similarly, after mixing, the second target duration is oscillated to ensure a sufficient reaction. For example, the second target time period may be 3 min. And finally, layering can occur after standing by utilizing the characteristic that the zinc-cadmium back extractant is not dissolved in the organic phase solution, so that the zinc-cadmium back extractant and the organic phase solution are separated.
the second loaded organic phase solution comprises iron element and indium element. By adding the indium stripping agent, the indium element is transferred into the indium stripping agent by utilizing the characteristic that the solubility of the indium element in the indium stripping agent is higher than that of the second loaded organic phase solution, so that the extraction of the indium element is realized, and the indium stripping agent solution containing the indium element and the third loaded organic phase solution containing the iron element are obtained.
Optionally, step 3 includes:
and mixing the indium stripping agent and the second loaded organic phase solution according to the volume ratio of 2:10, oscillating for a third target duration, standing for layering, and then separating to obtain a third loaded organic phase solution and an indium stripping agent solution for extracting indium element.
The indium back extractant and the second loaded organic phase solution can be mixed according to the volume ratio of 2:10, so that the using amount of the indium back extractant is ensured, the indium element in the second loaded organic phase solution can be completely transferred into the indium back extractant, and the situation that residual elements exist in the organic phase solution and can pollute the subsequent extracted iron element is avoided. Similarly, after mixing, the third target duration is oscillated to ensure a sufficient reaction. For example, the third target duration may be 3 min. And finally, layering can occur after standing by utilizing the characteristic that the indium stripping agent is immiscible with the second loaded organic phase solution, so that the indium stripping agent and the second loaded organic phase solution are separated.
And 4, extracting the third loaded organic phase solution by using an iron stripping agent so as to transfer the iron element in the third loaded organic phase solution to the iron stripping agent, thereby obtaining a fourth loaded organic phase solution and an iron stripping agent solution for extracting the iron element.
And (3) through the extraction operations of the steps 2 and 3, iron element is remained in the solution of the third loaded organic phase. By adding the iron stripping agent into the solution, the iron element is transferred into the iron stripping agent by utilizing the characteristic that the solubility of the iron element in the iron stripping agent is greater than that of the third loaded organic phase solution, so that the extraction of the iron element is realized, and the iron stripping agent solution containing the iron element and the fourth loaded organic phase solution are obtained.
Optionally, step 4 includes:
mixing the iron stripping agent with the third loaded organic phase solution according to the volume ratio of 2:10, oscillating for a fourth target duration, standing for layering, and then separating to obtain a fourth loaded organic phase solution and an iron stripping agent solution for extracting iron elements.
The proportion of the iron stripping agent to the third loaded organic phase solution can be mixed according to the volume ratio of 2:10, so that the using amount of the iron stripping agent is ensured, the iron element in the third loaded organic phase solution can be completely transferred to the iron stripping agent, and the waste caused by the residue in the organic phase solution is avoided. Similarly, after mixing, the fourth target duration is oscillated to ensure a sufficient reaction. For example, the fourth target duration may be 3 min. And finally, layering can occur after standing by utilizing the characteristic that the iron stripping agent is not dissolved in the third loaded organic phase solution, so that the iron stripping agent and the third loaded organic phase solution are separated.
In the separation method provided by this embodiment, first, an organic phase solution is used to extract a multi-metal ion mixed solution, so that a metal element to be extracted in the multi-metal ion mixed solution is transferred to the organic phase solution; and then, extracting the organic phase solution by using a zinc-cadmium stripping agent, an indium stripping agent and an iron stripping agent in sequence, so that zinc elements, cadmium elements, indium elements and iron elements in the organic phase solution are transferred to the corresponding stripping agents. According to the method provided by the invention, the metal elements in the mixed solution are extracted into the organic solvent containing the extracting agent at one time, and then different stripping agents are adopted for carrying out back extraction step by step, so that different metal elements are respectively transferred into the corresponding stripping agents from the organic solvent, and the separation and purification of the multi-metal mixed solution are realized. In addition, the method provided by the invention is simple, efficient, easy to implement, high in equipment utilization rate and easy to realize industrial application.
In one embodiment, the zinc-cadmium stripping agent is a sulfuric acid solution of 150g/L, the indium stripping agent is a hydrochloric acid solution of 3mol/L, and the iron stripping agent is a hydrochloric acid solution of 6 mol/L.
In this example, the choice of stripping agent for each step is important. The three back extractants not only can extract the target metal element from the organic phase solution, but also can meet the requirement that the subsequent operation of extracting other metal elements is not influenced. In addition, the effect of the pH of the stripping agent on the organic phase solution can be taken into account.
In one embodiment, the method further comprises:
adding a sodium hydroxide solution into the fourth loaded organic phase solution for saponification, mixing for a fifth target time length, standing for layering, and then separating to obtain a regenerated organic phase solution;
wherein, the regenerated organic phase solution is used as the organic phase solution for extracting the mixed solution of the multiple metal ions in the step 1. Wherein the fourth loaded organic phase solution has a saponification rate of 70%.
For acidic extractants, saponification is required and the resulting acid is neutralized with an alkaline substance, thereby increasing the amount of extraction. After multiple back extraction operations, the pH value of the obtained fourth loaded organic phase solution is acidic, so that a sodium hydroxide solution needs to be added for neutralization. Specifically, the two solutions are fully mixed for a fifth target time, standing is carried out after full reaction, and separation is carried out after the solutions are layered to obtain a regenerated organic phase solution. For example, the fifth target duration may be 3 min. The regenerated organic phase solution can be used for extracting metal elements again, and specifically, the regenerated organic phase solution can be used for extracting the metal elements in the multi-metal ion mixed solution in the step 1. By the method, the organic phase solution can be recovered and reused, and the implementation cost of the method is further reduced.
Referring to fig. 2, which schematically illustrates an extraction process, a method for separating a mixed multi-metal solution according to the present application is schematically illustrated by a specific experimental example:
step 1, obtaining a smelting waste leachate A, wherein the leachate A contains 1.5g/L of iron element, 8mg/L of indium element, 4mg/L of cadmium element and 5g/L of zinc element, and the PH value is 2.5.
And 3, mixing the stripping solution 1 and the loaded organic phase solution F according to the volume ratio of 2:10, oscillating for 3min, standing for layering, and separating to obtain the loaded organic phase solution G and the Zn and Cd stripping solution. The stripping solution 1 is a sulfuric acid solution of 150 g/L.
And 4, mixing the stripping solution 2 with the loaded organic phase solution G according to the volume ratio of 2:10, oscillating for 3min, standing for layering, and separating to obtain a loaded organic phase solution H and an In stripping solution. The stripping solution 2 is 3mol/L hydrochloric acid solution.
And 5, mixing the stripping solution 3 with the loaded organic phase solution H according to the volume ratio of 2:10, oscillating for 3min, standing for layering, and separating to obtain a regenerated organic phase I and Fe stripping solution. The back extraction solution 3 is 6mol/L hydrochloric acid solution.
And 6, adding sodium hydroxide into the regenerated organic phase I for saponification, mixing for 3min, standing for layering, separating, and reusing the obtained organic phase solution in the step 2 to extract the smelting waste leachate A.
The invention provides a method for separating a multi-metal mixed solution, which comprises the following steps of firstly, extracting the multi-metal ion mixed solution by using an organic phase solution so as to transfer metal elements to be extracted in the multi-metal ion mixed solution into the organic phase solution; and then, extracting the organic phase solution by using a zinc-cadmium stripping agent, an indium stripping agent and an iron stripping agent in sequence, so that zinc elements, cadmium elements, indium elements and iron elements in the organic phase solution are transferred to the corresponding stripping agents. According to the method provided by the invention, the metal elements in the mixed solution are extracted into the organic solvent containing the extracting agent at one time, and then different stripping agents are adopted for carrying out back extraction step by step, so that different metal elements are respectively transferred into the corresponding stripping agents from the organic solvent, and the separation and purification of the multi-metal mixed solution are realized. In addition, the method provided by the invention is simple, efficient, easy to implement, high in equipment utilization rate and easy to realize industrial application.
For simplicity of description, the method embodiments are described as a series of operational combinations, but those skilled in the art will recognize that the invention is not limited by the order of operation, as some steps may occur in other orders or concurrently in accordance with the invention. Further, those skilled in the art will also appreciate that the embodiments described in the specification are presently preferred and that no requirement is necessarily placed on the invention for the exact operation and experimental conditions involved.
The method for separating a mixed solution of multiple metals provided by the present invention is described in detail above, and the principle and the embodiment of the present invention are explained in the present document by applying specific examples, and the description of the above examples is only used to help understanding the method of the present invention and the core idea thereof; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. A method of separating a mixed multi-metal solution, the method comprising:
step 1, extracting a multi-metal ion mixed solution by using an organic phase solution so as to transfer metal elements to be extracted in the multi-metal ion mixed solution to an organic phase solution to obtain a first loaded organic phase solution; the metal elements to be extracted comprise iron elements, zinc elements, cadmium elements and indium elements;
step 2, extracting the first loaded organic phase solution by using a zinc-cadmium stripping agent so as to transfer zinc elements and cadmium elements in the first loaded organic phase solution to the zinc-cadmium stripping agent to obtain a second loaded organic phase solution and a zinc-cadmium stripping solution for extracting the zinc elements and the cadmium elements;
step 3, extracting the second loaded organic phase solution by using an indium stripping agent so as to transfer indium element in the second loaded organic phase solution to the indium stripping agent, thereby obtaining a third loaded organic phase solution and an indium stripping agent solution for extracting indium element;
and 4, extracting the third loaded organic phase solution by using an iron stripping agent so as to transfer the iron element in the third loaded organic phase solution to the iron stripping agent, thereby obtaining a fourth loaded organic phase solution and an iron stripping agent solution for extracting the iron element.
2. The method of claim 1, wherein the pH of the multi-metal ion mixture is in the range of 1.5-2.
3. The method of claim 1, wherein the organic phase solution is 30% by volume of the P204 extractant and 70% by volume of sulfonated kerosene.
4. The method of claim 1, wherein step 1 comprises:
and mixing the multi-metal ion mixed solution with the organic phase solution according to the volume ratio of 10:2, oscillating for a first target time, standing for layering, and separating to obtain the first loaded organic phase solution.
5. The method of claim 1, wherein the zinc-cadmium stripping agent is a 150g/L sulfuric acid solution, the indium stripping agent is a 3mol/L hydrochloric acid solution, and the iron stripping agent is a 6mol/L hydrochloric acid solution.
6. The method of claim 1, wherein step 2 comprises:
and mixing the zinc-cadmium stripping agent with the first loaded organic phase solution according to the volume ratio of 2:10, oscillating for a second target time length, standing for layering and then separating to obtain a second loaded organic phase solution and a zinc-cadmium stripping solution for extracting zinc elements and cadmium elements.
7. The method of claim 1, wherein step 3 comprises:
and mixing the indium stripping agent and the second loaded organic phase solution according to the volume ratio of 2:10, oscillating for a third target duration, standing for layering, and then separating to obtain a third loaded organic phase solution and an indium stripping agent solution for extracting indium element.
8. The method of claim 1, wherein the step 4 comprises:
mixing the iron stripping agent with the third loaded organic phase solution according to the volume ratio of 2:10, oscillating for a fourth target duration, standing for layering, and then separating to obtain a fourth loaded organic phase solution and an iron stripping agent solution for extracting iron elements.
9. The method of claim 1, further comprising:
adding a sodium hydroxide solution into the fourth loaded organic phase solution for saponification, mixing for a fifth target time, standing for layering, and separating to obtain a regenerated organic phase solution;
wherein, the regenerated organic phase solution is used as the organic phase solution for extracting the mixed solution of the multiple metal ions in the step 1.
10. The method of claim 9, wherein the fourth loaded organic phase solution has a saponification rate of 70%.
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