CN114836632B - Method for extracting cadmium by using ionic liquid - Google Patents
Method for extracting cadmium by using ionic liquid Download PDFInfo
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- CN114836632B CN114836632B CN202210670284.XA CN202210670284A CN114836632B CN 114836632 B CN114836632 B CN 114836632B CN 202210670284 A CN202210670284 A CN 202210670284A CN 114836632 B CN114836632 B CN 114836632B
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- cadmium
- leaching
- ionic liquid
- solution
- extracting
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- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 78
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002386 leaching Methods 0.000 claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000012074 organic phase Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000004070 electrodeposition Methods 0.000 claims abstract description 7
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- -1 1-hexyl-3-methylimidazole hexafluorophosphate Chemical compound 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 18
- 239000005416 organic matter Substances 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 description 6
- 229910000331 cadmium sulfate Inorganic materials 0.000 description 6
- 238000000151 deposition Methods 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910021646 siderite Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance 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
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/387—Cyclic or polycyclic compounds
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting cadmium by using ionic liquid, which comprises the following steps: (1) Adding a leaching agent into the cadmium-containing material for leaching, and filtering after leaching to obtain a cadmium-containing leaching solution; (2) Adding an extractant into the cadmium-containing leaching solution to carry out cadmium extraction to obtain a cadmium-containing organic phase and raffinate, and returning the raffinate to the step (1) for cyclic leaching; (3) Washing impurities of the cadmium-containing organic phase by using impurity washing liquid to obtain a cadmium-containing organic phase after impurity washing; (4) Carrying out back extraction on the organic phase after washing impurities containing cadmium by using a back extractant to obtain a cadmium-containing rich solution; and (5) obtaining cadmium metal by using an electrodeposition process for the cadmium-containing pregnant solution. The method for extracting cadmium by using the ionic liquid has the advantages that the cadmium product with the purity of 99.99% can be obtained through simple processes of leaching, extracting, impurity washing, back extraction and electrodeposition, the process flow is short, and the leaching agent and the extracting agent can be recycled, so that the method is a novel environment-friendly process.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for extracting cadmium by using ionic liquid.
Background
Cadmium is mainly an associated product in the smelting process of zinc-containing plumbite such as siderite, sulfur lead ore and the like, and is mainly applied to manufacturing cadmium-nickel alloy, pigment, plastic stabilizer, fluorescent powder, insecticide, bactericide, paint, electrical switch, automobile relay, battery and the like, and particularly has outstanding effects in the aspects of aviation industry, atomic reactor, electroplating corrosion prevention and the like. All these applications require very pure cadmium metal, typically 99.99% or more pure. The traditional cadmium refining process has complicated steps, involves multiple filtering, dissolving and replacing processes, and zinc, lead and copper are impurities which are difficult to remove in the cadmium refining process.
Disclosure of Invention
The invention aims to provide a method for extracting cadmium by using ionic liquid, which can obtain a cadmium product with purity up to 99.99% through simple processes of leaching, extracting, impurity washing, back extraction and electrodeposition.
In order to achieve the above object, the present invention provides a method for extracting cadmium by using an ionic liquid, comprising the following steps:
(1) Adding a leaching agent into the cadmium-containing material for leaching, and filtering after leaching to obtain a cadmium-containing leaching solution;
(2) Adding an extractant into the cadmium-containing leaching solution to carry out cadmium extraction to obtain a cadmium-containing organic phase and raffinate, and returning the raffinate to the step (1) for cyclic leaching; the extractant is ionic liquid;
(3) Washing impurities of the cadmium-containing organic phase by using impurity washing liquid to obtain a cadmium-containing organic phase after impurity washing;
(4) Carrying out back extraction on the organic phase after washing impurities containing cadmium by using a back extractant to obtain a cadmium-containing rich solution; the back extraction agent is one of alkaline, acidic or neutral back extraction agents;
(5) And (3) the cadmium-containing pregnant solution is subjected to an electrodeposition process to obtain cadmium metal, and the solution after the electrodeposition is returned to the step (4) for cyclic back extraction.
Preferably, the liquid-solid ratio of the cadmium-containing material to the leaching agent in the step (1) is 5-50, the leaching temperature is 20-100 ℃, and the reaction time is 0.5-4 h.
Preferably, the concentration of the leaching agent is 0-3 mol/L.
Preferably, the leaching agent is HCl, H 2 SO 4 、HNO 3 One or more of HBr, naCl aqueous solution.
Preferably, the ionic liquid is one or more of 1-hexyl-3-methylimidazolium hexafluorophosphate ionic liquid [ HMPSM ] [ PF6] and 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid [ BMPSM ] [ PF6 ].
Preferably, the cadmium-containing rich solution in the step (4) is Cd (NO) 3 ) 2 、CdCl 2 、CdSO 4 Is a mixture of one or more of the following.
Preferably, the stripping agent is NaOH or Ca (OH) 2 、KOH、HCl、HNO 3 、H 2 SO 4 One or more of ammonia water and pure water.
Therefore, the method for extracting cadmium by using the ionic liquid has the advantages of high ionic conductivity, nonflammability, non-volatility, high thermal stability, high solvent property, wide liquid phase temperature range and the like, is a green nonaqueous solution extractant, can realize a continuous and sustainable cadmium leaching extraction process, has the advantages of closed solution circulation in the whole process flow, simple operation and environment friendliness, and can achieve the aim of efficiently extracting cadmium in a green way.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic process flow diagram of a method for extracting cadmium with an ionic liquid according to the present invention.
Detailed Description
The present invention will be further described with reference to examples in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
Configuration contains H 2 SO 4 The acid leaching agent is leached for 2 hours under the conditions that the liquid-solid ratio of the cadmium-containing material is 20:1 and the temperature is 30 ℃, and the leaching agent is filtered after the leaching is finished to obtain a cadmium-containing leaching solution, wherein the cadmium-containing leaching solution uses an extractant [ HMPSM ]][PF6]The ionic liquid is characterized in that the ratio of the ionic liquid to the ionic liquid is 1:1 for 50min, the extraction rate of cadmium is 90%, and the organic matter containing cadmium and raffinate are obtained after the extraction is completed. Washing the cadmium-containing organic matter with impurity washing liquid to obtain cadmium-containing washed organic matter, back extracting the cadmium-containing washed organic matter with sulfuric acid solution to obtain cadmium sulfate rich liquid, and electro-depositing the cadmium sulfate rich liquid to obtain cadmium metal and electro-deposited liquid, and back extracting the electro-deposited liquid circularly.
Example 2
Configuration contains H 2 SO 4 The acid leaching agent is leached for 2 hours under the conditions that the liquid-solid ratio of the cadmium-containing material is 20:1 and the temperature is 30 ℃, and the leaching agent is filtered after the leaching is finished to obtain a cadmium-containing leaching solution, wherein the cadmium-containing leaching solution adopts an extractant [ BMPSM ]][PF6]The ionic liquid is characterized in that the ratio of the ionic liquid to the ionic liquid is 1:1 for 30min, the extraction rate of cadmium is 90%, and the organic matter containing cadmium and raffinate are obtained after the extraction is completed. Washing the cadmium-containing organic matter with impurity washing liquid to obtain cadmium-containing washed organic matter, back extracting the cadmium-containing washed organic matter with sulfuric acid solution to obtain cadmium sulfate rich liquid, and electro-depositing the cadmium sulfate rich liquid to obtain cadmium metal and electro-deposited liquid, and back extracting the electro-deposited liquid circularly.
Example 3
Preparing an HCl-containing acidic leaching agent, leaching for 2 hours under the conditions that the liquid-solid ratio of a cadmium-containing material is 20:1 and the temperature is 30 ℃, filtering after leaching to obtain a cadmium-containing leaching solution, and comparing the cadmium-containing leaching solution with an extracting agent [ BMPSM ] [ PF6] ionic liquid according to the ratio of 1:1 for 30min, the extraction rate of cadmium is 80%, and the organic matter containing cadmium and raffinate are obtained after the extraction is completed. Washing the cadmium-containing organic matter with impurity washing liquid to obtain cadmium-containing washed organic matter, back extracting the cadmium-containing washed organic matter with sulfuric acid solution to obtain cadmium sulfate rich liquid, and electro-depositing the cadmium sulfate rich liquid to obtain cadmium metal and electro-deposited liquid, and back extracting the electro-deposited liquid circularly.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (4)
1. A method for extracting cadmium by using ionic liquid, which is characterized by comprising the following steps:
(1) Adding a leaching agent into the cadmium-containing material for leaching, and filtering after leaching to obtain a cadmium-containing leaching solution;
the leaching agent is HCl, H 2 SO 4 、HNO 3 One or more of HBr, aqueous NaCl solution;
(2) Adding an extractant into the cadmium-containing leaching solution to carry out cadmium extraction to obtain a cadmium-containing organic phase and raffinate, and returning the raffinate to the step (1) for cyclic leaching; the extractant is ionic liquid;
the ionic liquid is one or more of 1-hexyl-3-methylimidazole hexafluorophosphate ionic liquid [ HMPSM ] [ PF6] and 1-butyl-3-methylimidazole hexafluorophosphate ionic liquid [ BMPSM ] [ PF6 ];
(3) Washing impurities of the cadmium-containing organic phase by using impurity washing liquid to obtain a cadmium-containing organic phase after impurity washing;
(4) Carrying out back extraction on the organic phase after washing impurities containing cadmium by using a back extractant to obtain a cadmium-containing rich solution; the back extractant is alkaliOne of a sex, acidic or neutral stripping agent; the back extractant is NaOH, ca (OH) 2 、KOH、HCl、HNO 3 、H 2 SO 4 One or more of ammonia water and pure water;
(5) And (3) the cadmium-containing pregnant solution is subjected to an electrodeposition process to obtain cadmium metal, and the solution after the electrodeposition is returned to the step (4) for cyclic back extraction.
2. The method for extracting cadmium by using ionic liquid according to claim 1, wherein: in the step (1), the liquid-solid ratio of the cadmium-containing material to the leaching agent is 5-50, the leaching temperature is 20-100 ℃, and the reaction time is 0.5-4 h.
3. The method for extracting cadmium by using ionic liquid according to claim 1, wherein: the concentration of the leaching agent is 0-3 mol/L.
4. The method for extracting cadmium by using ionic liquid according to claim 1, wherein: the cadmium-containing rich solution in the step (4) is Cd (NO) 3 ) 2 、CdCl 2 、CdSO 4 Is a mixture of one or more of the following.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210670284.XA CN114836632B (en) | 2022-06-14 | 2022-06-14 | Method for extracting cadmium by using ionic liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210670284.XA CN114836632B (en) | 2022-06-14 | 2022-06-14 | Method for extracting cadmium by using ionic liquid |
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| Publication Number | Publication Date |
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| CN114836632A CN114836632A (en) | 2022-08-02 |
| CN114836632B true CN114836632B (en) | 2023-07-21 |
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| CN116655472B (en) * | 2023-04-17 | 2025-01-07 | 天津大学 | Thioether-containing diammonium cationic liquid, preparation method and application thereof in Cd in aqueous solution2+And Pb2+Is separated by a separation method of (2) |
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| CN102513064A (en) * | 2011-12-23 | 2012-06-27 | 广东工业大学 | Preparation method and application of ionic liquid bonded silica adsorbent |
| CN104007099B (en) * | 2014-06-04 | 2017-01-04 | 傅科杰 | The detection method of cadmium in a kind of garment for children |
| CN107586959B (en) * | 2017-09-11 | 2018-11-30 | 陕西科技大学 | Utilize the method for heavy metal in intensified by ultrasonic wave functional ionic liquids extraction water |
| CN108977669B (en) * | 2018-09-13 | 2020-07-17 | 中南大学 | A method for deep removal of cadmium in high-concentration cobalt sulfate solution and recovery of cadmium |
| CN113260440B (en) * | 2018-12-11 | 2023-07-14 | 艾尼股份公司 | Method for selective recovery of transition metals from organic residues |
| CN110745900B (en) * | 2019-11-04 | 2022-05-10 | 西安建筑科技大学 | A kind of separation method of heavy metal hexavalent chromium and divalent cadmium |
| CN111041221B (en) * | 2019-12-17 | 2022-07-12 | 中南大学 | A method for recovering cadmium from cadmium-containing high-arsenic soot |
| CN112981104B (en) * | 2021-02-05 | 2023-04-25 | 桐乡市思远环保科技有限公司 | Method for treating cadmium-containing waste residues and recycling metal cadmium |
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