CN114836632A - Method for extracting cadmium by using ionic liquid - Google Patents
Method for extracting cadmium by using ionic liquid Download PDFInfo
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- CN114836632A CN114836632A CN202210670284.XA CN202210670284A CN114836632A CN 114836632 A CN114836632 A CN 114836632A CN 202210670284 A CN202210670284 A CN 202210670284A CN 114836632 A CN114836632 A CN 114836632A
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- 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
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- 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
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- 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
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- 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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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 to obtain cadmium-containing leachate after leaching is finished; (2) adding an extracting agent into the cadmium-containing leaching solution for cadmium extraction to obtain a cadmium-containing organic phase and raffinate, and returning the raffinate to the step (1) for circulating leaching; (3) washing impurities of the cadmium-containing organic phase by using impurity washing liquid to obtain a cadmium-containing impurity-washed organic phase; (4) carrying out back extraction on the cadmium-containing impurity-washed organic phase by using a back extractant to obtain a cadmium-containing rich solution; (5) the cadmium-containing pregnant solution is used for obtaining cadmium metal by an electrodeposition process. The method for extracting cadmium by using the ionic liquid with the structure can obtain the cadmium product with the purity of 99.99 percent by simple processes of leaching, extracting, impurity washing, back extraction and electrodeposition, has short process flow, can recycle the leaching agent and the extracting agent, and is a new green and 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-lead-copper-containing minerals such as calamine, sulfur-lead ore and the like, and is mainly applied to manufacturing cadmium-nickel alloy, pigment, plastic stabilizer, fluorescent powder, insecticide, bactericide, paint, electrical switches, automobile relays, batteries and the like, and particularly has outstanding effects in the aspects of aviation industry, atomic reactors, electroplating corrosion prevention and the like. All of these applications require very pure cadmium metal, typically 99.99% or more pure. The traditional cadmium refining process has complicated steps, relates to multiple filtering, dissolving and replacing processes, and is characterized in that 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 the purity of 99.99 percent by simple processes of leaching, extraction, impurity washing, back extraction and electrodeposition, has short process flow, can recycle a leaching agent and an extracting agent, and is a novel green and environment-friendly process.
In order to achieve the aim, the invention provides a method for extracting cadmium by using an ionic liquid, which comprises the following steps:
(1) adding a leaching agent into the cadmium-containing material for leaching, and filtering to obtain cadmium-containing leachate after leaching is finished;
(2) adding an extracting agent into the cadmium-containing leaching solution for cadmium extraction to obtain a cadmium-containing organic phase and raffinate, and returning the raffinate to the step (1) for circulating 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 impurity-washed organic phase;
(4) carrying out back extraction on the cadmium-containing impurity-washed organic phase by using a back extractant to obtain a cadmium-containing rich solution; the stripping agent is one of alkaline, acidic or neutral stripping agents;
(5) and (4) obtaining cadmium metal from the cadmium-containing rich solution by using an electrodeposition process, and returning the electrodeposited solution to the step (4) for circular 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, leaching is carried outThe agent is HCl and H 2 SO 4 、HNO 3 And one or more of HBr and 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 One or more mixtures of (a).
Preferably, the stripping agent is NaOH, 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 with the structure has the advantages of high ionic conductivity, nonflammability, nonvolatility, high thermal stability, high solvent property, wide liquid phase temperature range and the like, is a green non-aqueous solution extracting agent, can realize a continuous and sustainable cadmium leaching and extracting process, is simple to operate and environment-friendly, and can achieve the aim of efficiently and environmentally extracting cadmium.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a schematic process flow diagram of a method for extracting cadmium by using 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 containing H 2 SO 4 An acidic leaching agent, leaching for 2h at 30 deg.C with a liquid-solid ratio of 20:1, filtering to obtain cadmium-containing leachate, and extracting with extractant [ HMPSM ]][PF6]The ionic liquid is prepared by the following steps: 1, extracting for 50min with cadmium extraction rate of 90%, and obtaining the product after extractionTo cadmium containing organic and raffinate. And (3) washing the cadmium-containing organic matter with a washing solution to obtain the cadmium-containing washed organic matter, performing back extraction on the cadmium-containing washed organic matter with a sulfuric acid solution to obtain a cadmium sulfate rich solution, performing electrodeposition on the cadmium sulfate rich solution to obtain cadmium metal and a post-electrodeposition solution, and performing circular back extraction on the post-electrodeposition solution.
Example 2
Configuration containing H 2 SO 4 An acidic leaching agent, leaching for 2h at 30 ℃ at a liquid-solid ratio of 20:1 of the cadmium-containing material, filtering to obtain a cadmium-containing leaching solution, and extracting with an extractant [ BMPSM ] to obtain the cadmium-containing leaching solution][PF6]The ionic liquid is prepared by the following steps: 1, extracting for 30min, wherein the cadmium extraction rate is 90%, and obtaining cadmium-containing organic matters and raffinate after extraction is finished. And (3) washing the cadmium-containing organic matter with a washing solution to obtain the cadmium-containing washed organic matter, performing back extraction on the cadmium-containing washed organic matter with a sulfuric acid solution to obtain a cadmium sulfate rich solution, performing electrodeposition on the cadmium sulfate rich solution to obtain cadmium metal and a post-electrodeposition solution, and performing circular back extraction on the post-electrodeposition solution.
Example 3
Preparing an HCl-containing acidic leaching agent, leaching for 2 hours at the liquid-solid ratio of a cadmium-containing material of 20:1 and 30 ℃, filtering to obtain a cadmium-containing leachate after leaching is finished, and extracting the cadmium-containing leachate with an extractant [ BMPSM ] [ PF6] ionic liquid according to the proportion of 1: 1, extracting for 30min, wherein the cadmium extraction rate is 80 percent, and obtaining cadmium-containing organic and raffinate after extraction is finished. And (3) washing the cadmium-containing organic matter with a washing solution to obtain the cadmium-containing washed organic matter, performing back extraction on the cadmium-containing washed organic matter with a sulfuric acid solution to obtain a cadmium sulfate rich solution, performing electrodeposition on the cadmium sulfate rich solution to obtain cadmium metal and a post-electrodeposition solution, and performing circular back extraction on the post-electrodeposition solution.
Finally, it should be noted that: the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (7)
1. A method for extracting cadmium by using ionic liquid is characterized by comprising the following steps:
(1) adding a leaching agent into the cadmium-containing material for leaching, and filtering to obtain cadmium-containing leachate after leaching is finished;
(2) adding an extracting agent into the cadmium-containing leaching solution for cadmium extraction to obtain a cadmium-containing organic phase and raffinate, and returning the raffinate to the step (1) for circulating 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 impurity-washed organic phase;
(4) carrying out back extraction on the cadmium-containing impurity-washed organic phase by using a back extraction agent to obtain a cadmium-containing rich solution; the stripping agent is one of alkaline, acidic or neutral stripping agents;
(5) and (4) obtaining cadmium metal from the cadmium-containing rich solution by using an electrodeposition process, and returning the electrodeposited solution to the step (4) for circular back extraction.
2. The method of claim 1, wherein the ionic liquid is selected from the group consisting of: 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 of claim 1, wherein the ionic liquid is selected from the group consisting of: the concentration of the leaching agent is 0-3 mol/L.
4. The method of claim 1, wherein the ionic liquid is selected from the group consisting of: the leaching agent is HCl and H 2 SO 4 、HNO 3 And one or more of HBr and NaCl aqueous solution.
5. The method of claim 1, wherein the ionic liquid is selected from the group consisting of: 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 ].
6. According to the rightThe method for extracting cadmium by using the ionic liquid, which is characterized by comprising the following steps: the cadmium-containing rich solution in the step (4) is Cd (NO) 3 ) 2 、CdCl 2 、CdSO 4 One or more mixtures of (a).
7. The method of claim 1, wherein the ionic liquid is selected from the group consisting of: 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.
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| CN202210670284.XA CN114836632B (en) | 2022-06-14 | 2022-06-14 | Method for extracting cadmium by using ionic liquid |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102513064A (en) * | 2011-12-23 | 2012-06-27 | 广东工业大学 | Preparation method and application of ionic liquid bonded silica adsorbent |
| CN104007099A (en) * | 2014-06-04 | 2014-08-27 | 傅科杰 | Testing method for cadmium in children clothing |
| CN107586959A (en) * | 2017-09-11 | 2018-01-16 | 陕西科技大学 | Utilize the method for heavy metal in intensified by ultrasonic wave functional ionic liquids extraction water |
| CN108977669A (en) * | 2018-09-13 | 2018-12-11 | 中南大学 | A method of cadmium in high-concentration sulfuric acid cobalt liquor is removed in depth and recycles cadmium |
| CN110745900A (en) * | 2019-11-04 | 2020-02-04 | 西安建筑科技大学 | Method for separating heavy metals chromium (VI) and cadmium (II) |
| CN111041221A (en) * | 2019-12-17 | 2020-04-21 | 中南大学 | Method for recovering cadmium from cadmium-containing high-arsenic soot |
| CN112981104A (en) * | 2021-02-05 | 2021-06-18 | 桐乡市思远环保科技有限公司 | Method for treating cadmium-containing waste residues and recovering metal cadmium |
| CN113260440A (en) * | 2018-12-11 | 2021-08-13 | 艾尼股份公司 | Process for the selective recovery of transition metals from organic residues |
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2022
- 2022-06-14 CN CN202210670284.XA patent/CN114836632B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102513064A (en) * | 2011-12-23 | 2012-06-27 | 广东工业大学 | Preparation method and application of ionic liquid bonded silica adsorbent |
| CN104007099A (en) * | 2014-06-04 | 2014-08-27 | 傅科杰 | Testing method for cadmium in children clothing |
| CN107586959A (en) * | 2017-09-11 | 2018-01-16 | 陕西科技大学 | Utilize the method for heavy metal in intensified by ultrasonic wave functional ionic liquids extraction water |
| CN108977669A (en) * | 2018-09-13 | 2018-12-11 | 中南大学 | A method of cadmium in high-concentration sulfuric acid cobalt liquor is removed in depth and recycles cadmium |
| CN113260440A (en) * | 2018-12-11 | 2021-08-13 | 艾尼股份公司 | Process for the selective recovery of transition metals from organic residues |
| CN110745900A (en) * | 2019-11-04 | 2020-02-04 | 西安建筑科技大学 | Method for separating heavy metals chromium (VI) and cadmium (II) |
| CN111041221A (en) * | 2019-12-17 | 2020-04-21 | 中南大学 | Method for recovering cadmium from cadmium-containing high-arsenic soot |
| CN112981104A (en) * | 2021-02-05 | 2021-06-18 | 桐乡市思远环保科技有限公司 | Method for treating cadmium-containing waste residues and recovering metal cadmium |
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