CN113564387A - Method for extracting indium in chlorine-containing soot - Google Patents
Method for extracting indium in chlorine-containing soot Download PDFInfo
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- CN113564387A CN113564387A CN202110912274.8A CN202110912274A CN113564387A CN 113564387 A CN113564387 A CN 113564387A CN 202110912274 A CN202110912274 A CN 202110912274A CN 113564387 A CN113564387 A CN 113564387A
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- indium
- extracting
- leaching
- chlorine
- containing soot
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- 229910052738 indium Inorganic materials 0.000 title claims abstract description 107
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000004071 soot Substances 0.000 title claims abstract description 25
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000460 chlorine Substances 0.000 title claims abstract description 20
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 20
- 238000002386 leaching Methods 0.000 claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 26
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 10
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000005416 organic matter Substances 0.000 claims abstract description 4
- 239000002608 ionic liquid Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- XKBGEWXEAPTVCK-UHFFFAOYSA-M methyltrioctylammonium chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC XKBGEWXEAPTVCK-UHFFFAOYSA-M 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 18
- 239000000047 product Substances 0.000 description 11
- 239000011780 sodium chloride Substances 0.000 description 9
- 239000006227 byproduct Substances 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021617 Indium monochloride Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 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
- 238000004090 dissolution Methods 0.000 description 1
- -1 ethylene glycol indium chloride Chemical compound 0.000 description 1
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
Images
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
- C22B58/00—Obtaining gallium or indium
-
- 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
-
- 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
- C22B7/02—Working-up flue dust
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting indium from chlorine-containing soot, which comprises the following steps: (1) adding a leaching agent into an indium-containing soot material for leaching, wherein the leaching agent is an ionic liquid formed by ethylene glycol and lithium chloride, filtering after leaching is finished to obtain an indium-containing leachate, (2) adding an extracting agent into the leachate for indium extraction to obtain an indium-containing organic matter and a raffinate, and returning the raffinate to the step (1) for circular leaching, (3) washing the indium-containing organic matter with a washing impurity liquid to obtain an indium-containing washing impurity solution, and (4) performing back extraction on the indium-containing washing impurity solution with a back extraction agent to obtain an indium product. By adopting the method for extracting indium from chlorine-containing soot with the structure, the indium product with the purity of 98% can be obtained through simple processes of leaching, extracting, impurity washing and back extraction, the process flow is short, and the leaching agent and the extracting agent can be recycled, so that the method 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 indium from chlorine-containing soot.
Background
The indium is mainly an associated product in the smelting process of minerals such as copper, lead and zinc, and is mainly applied to high-tech industries such as liquid crystal display screens, light emitting diodes, photovoltaic cells and the like. All of these applications require very pure metallic indium, typically 99.9999% (6N) or higher in purity. The traditional indium refining process comprises more than 20 process steps, which relate to multiple precipitation and dissolution processes, and zinc, iron and tin are impurities which are difficult to remove in the indium refining process.
Disclosure of Invention
The invention aims to provide a method for extracting indium from chlorine-containing soot, which can obtain an indium product with the purity of up to 98 percent through simple processes of leaching, extracting, impurity washing and back extraction, 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 purpose, the invention provides a method for extracting indium from chlorine-containing soot, which comprises the following steps:
(1) adding a leaching agent into the indium-containing soot material for leaching, wherein the leaching agent is an ionic liquid formed by ethylene glycol and lithium chloride, and filtering to obtain an indium-containing leaching solution after leaching is finished;
(2) adding an extracting agent into the leachate for indium extraction to obtain indium-containing organic matters and raffinate, and returning the raffinate to the step (1) for circular leaching;
(3) washing impurities of the indium-containing organic matter by using impurity washing liquid to obtain indium-containing impurity washing liquid;
(4) carrying out back extraction on the indium-containing impurity-washed liquid by using a back extractant to obtain an indium product;
(5) and further purifying the indium product by using an alkaline solvent to remove impurities such as zinc and the like which are not cleaned in the product.
Preferably, the liquid-solid ratio of the indium-containing soot 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 lithium chloride in the leaching agent in the step (1) is 0-3.5 mol/L.
Preferably, the equipment used for the filtration in the step (1) is one or more of a centrifuge, a thickener and the like.
Preferably, in the leaching process in the step (1), the indium leaching rate is as high as 90%.
Preferably, the extractant in the step (2) is one of a phosphorus extractant and an amine extractant.
Preferably, the extractant is one or more of Cyphos101, Aliquat336 and A327.
Preferably, the impurity washing liquid in the step (3) is an indium chloride glycol solution, wherein the indium concentration is 0.1-1 g/L.
Preferably, the indium product in the step (4) is in (OH)3、InCl3One or more mixtures of (a).
Preferably, the stripping agent in step (5) is one of alkaline, acidic or neutral stripping agent.
Preferably, the stripping agent is NaOH, Ca (OH)2、KOH、HCl、HNO3One or more mixtures of stripping agents such as ammonia water and pure water.
The invention has the beneficial effects that: the leaching agent used in the invention has the advantages of low inflammability, high thermal stability, negligible vapor pressure and the like, is a green non-aqueous solution leaching agent, can realize a continuous and sustainable indium leaching and extraction process, has closed and circulated solution in the whole process flow, is simple to operate and environment-friendly, and can achieve the aim of efficiently and environmentally extracting indium.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a process flow diagram of a method for extracting indium from chlorine-containing soot according to the present invention;
FIG. 2 is a structural diagram of ethylene glycol indium chloride in the leaching solution of the method for extracting indium from chlorine-containing soot according to the invention.
Detailed Description
The technical scheme of the invention is further illustrated by the attached drawings and examples, and various chemicals and reagents used in the examples are all purchased from the market without specific description.
Example 1
Configuring LiCl3And (2) leaching the indium-containing ash by using an ethylene glycol leaching agent with the concentration of 3mol/L for 2 hours at the temperature of 30 ℃ and the indium-containing ash liquid-solid ratio of 20:1, and filtering to obtain an indium-containing leachate, wherein the indium-containing leachate is prepared by using an extractant Aliquate336 according to the following ratio of 1: 1, extracting to obtain indium-containing organic matters and raffinate after extraction is finished. The indium-containing organic solvent is 0.5g/L impurity washing liquid InCl3(EG)2Carrying out 2-stage countercurrent washing to obtain indium impurity-washed liquid, and carrying out back extraction on the indium impurity-washed liquid by using a sodium hydroxide solution to obtain in (OH)3And NaCl solution in which in (OH)3The yield of (a) was 90.1%. The filtered indium product can be purified by adjusting the pH value with sodium hydroxide, and the NaCl solution can be used for preparing a NaCl byproduct.
Example 2
Configuring LiCl3And (2) leaching the indium-containing ash by using an ethylene glycol leaching agent with the concentration of 3mol/L for 2 hours at the temperature of 50 ℃ and the indium-containing ash liquid-solid ratio of 20:1, and filtering to obtain an indium-containing leachate, wherein the indium-containing leachate is prepared by using an extractant Aliquate336 according to the following ratio of 1: 1, extracting to obtain indium-containing organic matters and raffinate after extraction is finished. The indium-containing organic solvent is 0.5g/L impurity washing liquid InCl3(EG)2Carrying out 2-stage countercurrent washing to obtain indium impurity-washed liquid, and carrying out back extraction on the indium impurity-washed liquid by using a sodium hydroxide solution to obtain in (OH)3And NaCl solution in which in (OH)3The yield of (a) was 92.4%. The filtered indium product can be purified by adjusting the pH value with sodium hydroxide, and the NaCl solution can be used for preparing a NaCl byproduct.
Example 3
Configuring LiCl3And (2) leaching the indium-containing ash by using an ethylene glycol leaching agent with the concentration of 3mol/L for 2 hours at the temperature of 20 ℃ and the solid-to-liquid ratio of the indium-containing ash of 20:1, filtering to obtain an indium-containing leachate, and extracting the indium-containing leachate by using an extractant Aliquate336 according to the proportion of 1: 1, extracting to obtain indium-containing organic matters and raffinate after extraction is finished. Comprises0.1g/L impurity washing liquid InCl is used for indium organization3(EG)2Carrying out 4-stage countercurrent washing to obtain indium impurity-washed liquid, and carrying out back extraction on the indium impurity-washed liquid by using a sodium hydroxide solution to obtain in (OH)3And NaCl solution in which in (OH)3The yield of (3) was 93.6%. The filtered indium product can be purified by adjusting the pH value with sodium hydroxide, and the NaCl solution can be used for preparing a NaCl byproduct.
Example 4
Configuring LiCl3And (2) leaching the indium-containing ash for 1h by using an ethylene glycol leaching agent with the concentration of 3mol/L at the temperature of 20 ℃ and the solid-to-liquid ratio of the indium-containing ash of 20:1, filtering to obtain an indium-containing leachate, wherein the indium-containing leachate is prepared by using an extracting agent Cyphos101 according to the ratio of 1: 1, extracting to obtain indium-containing organic matters and raffinate after extraction is finished. The indium-containing organic solvent is 0.1g/L impurity washing liquid InCl3(EG)2Carrying out 4-stage countercurrent washing to obtain indium impurity-washing liquid, and carrying out back extraction on the indium impurity-washing liquid by using calcium hydroxide solution to obtain in (OH)3And CaCl2Solution of in (OH)3The yield of (a) was 92.8%. The filtered indium product can be purified by adjusting pH with calcium hydroxide, CaCl2The solution can be used for preparing CaCl2By-products.
Example 5
Configuring LiCl3And (2) leaching the indium-containing ash for 1h by using an ethylene glycol leaching agent with the concentration of 3mol/L at the temperature of 20 ℃ and the solid-to-liquid ratio of the indium-containing ash of 20:1, filtering to obtain an indium-containing leachate, wherein the indium-containing leachate is prepared by using an extracting agent Cyphos101 according to the ratio of 1: 1, extracting to obtain indium-containing organic matters and raffinate after extraction is finished. The indium-containing organic solvent is 0.1g/L impurity washing liquid InCl3(EG)2Carrying out 4-stage countercurrent washing to obtain indium impurity-washed liquid, and carrying out back extraction on the indium impurity-washed liquid by using an ammonia solution to obtain in (OH)3And NH4Cl solution of in (OH)3The yield of (a) was 91.1%. The filtered indium product can be purified by adjusting the pH value with ammonia water, and NH4Cl solution can be used for preparing NH4Cl by-product.
Therefore, according to the embodiments 1 to 5, the method for extracting indium from chlorine-containing soot provided by the invention can achieve the purpose of efficiently extracting indium in a green manner.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting 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 (10)
1. A method for extracting indium from chlorine-containing soot is characterized by comprising the following steps: the method comprises the following steps:
(1) adding a leaching agent into the indium-containing soot material for leaching, wherein the leaching agent is an ionic liquid formed by ethylene glycol and lithium chloride, and filtering to obtain an indium-containing leaching solution after leaching is finished;
(2) adding an extracting agent into the leachate for indium extraction to obtain indium-containing organic matters and raffinate, and returning the raffinate to the step (1) for circular leaching;
(3) washing impurities of the indium-containing organic matter by using impurity washing liquid to obtain indium-containing impurity washing liquid;
(4) carrying out back extraction on the indium-containing impurity-washed liquid by using a back extractant to obtain an indium product;
(5) and further purifying the indium product by using an alkaline solvent to remove impurities such as zinc and the like which are not cleaned in the product.
2. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the liquid-solid ratio of the indium-containing soot 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.
3. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the concentration of lithium chloride in the leaching agent in the step (1) is 0-3.5 mol/L.
4. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the equipment used for filtering in the step (1) is one or a combination of more than one of a centrifuge, a thickener and the like.
5. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the extractant in the step (2) is one of a phosphorus extractant or an amine extractant.
6. The method for extracting indium in chlorine-containing soot as claimed in claim 5, wherein: the extractant is one or more of Cyphos101, Aliquat336 and A327.
7. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the impurity washing liquid in the step (3) is an indium chloride glycol solution, wherein the indium concentration is 0.1-1 g/L.
8. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the indium product in the step (4) is in (OH)3、InCl3One or more mixtures of (a).
9. The method for extracting indium from chlorine-containing soot as claimed in claim 1, wherein: the stripping agent in the step (5) is one of alkaline, acidic or neutral stripping agents.
10. The method for extracting indium from chlorine-containing soot as claimed in claim 9, wherein: the back extractant is NaOH, Ca (OH)2、KOH、HCl、HNO3One or more mixtures of stripping agents such as ammonia water and pure water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202110912274.8A CN113564387A (en) | 2021-08-10 | 2021-08-10 | Method for extracting indium in chlorine-containing soot |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110912274.8A CN113564387A (en) | 2021-08-10 | 2021-08-10 | Method for extracting indium in chlorine-containing soot |
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| CN113564387A true CN113564387A (en) | 2021-10-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115321585A (en) * | 2022-08-09 | 2022-11-11 | 先导薄膜材料有限公司 | Washing process of indium hydroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115321585A (en) * | 2022-08-09 | 2022-11-11 | 先导薄膜材料有限公司 | Washing process of indium hydroxide |
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