CN117385177A - Method for separating In, cd and Ag In target - Google Patents
Method for separating In, cd and Ag In target Download PDFInfo
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- CN117385177A CN117385177A CN202311349745.4A CN202311349745A CN117385177A CN 117385177 A CN117385177 A CN 117385177A CN 202311349745 A CN202311349745 A CN 202311349745A CN 117385177 A CN117385177 A CN 117385177A
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- acid leaching
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- 229910052738 indium Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 37
- 238000002386 leaching Methods 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 235000021110 pickles Nutrition 0.000 claims abstract description 4
- -1 alkali metal halogen salt Chemical class 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 5
- 229910052736 halogen Inorganic materials 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001508 alkali metal halide Inorganic materials 0.000 claims description 3
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000013522 chelant Substances 0.000 claims 1
- 229910052793 cadmium Inorganic materials 0.000 abstract description 12
- 239000002244 precipitate Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- 238000005292 vacuum distillation Methods 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229920001429 chelating resin Polymers 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005372 isotope separation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 230000005263 electron capture decay Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940121896 radiopharmaceutical Drugs 0.000 description 1
- 239000012217 radiopharmaceutical Substances 0.000 description 1
- 230000002799 radiopharmaceutical effect Effects 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
-
- 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
- C22B17/02—Obtaining cadmium by dry 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
- C22B17/00—Obtaining cadmium
- C22B17/06—Refining
-
- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- 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
- C22B3/28—Amines
- C22B3/282—Aliphatic amines
-
- 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
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
-
- 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
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- 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
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
-
- 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
- C22B7/001—Dry 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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21G—CONVERSION OF CHEMICAL ELEMENTS; RADIOACTIVE SOURCES
- G21G1/00—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes
- G21G1/001—Recovery of specific isotopes from irradiated targets
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21G—CONVERSION OF CHEMICAL ELEMENTS; RADIOACTIVE SOURCES
- G21G1/00—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes
- G21G1/001—Recovery of specific isotopes from irradiated targets
- G21G2001/0057—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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Abstract
The invention discloses a method for separating In, cd and Ag In a target, and belongs to the technical field of isotope medicament preparation. The method comprises the steps of firstly heating a target In vacuum, and distilling to remove Cd to obtain a target substrate, wherein the target substrate contains In and Ag. And then, placing the target substrate into acid liquor for acid leaching to obtain acid leaching liquor, wherein the acid liquor is nitric acid or non-nitric acid so as to generate Ag precipitate. And finally, filtering the pickle liquor to obtain filtrate containing In, and purifying the filtrate by using a resin adsorption or extraction method to obtain In. The method can effectively separate three elements of Cd, in and Ag, and simultaneously can recycle the high purity of In and Cd.
Description
Technical Field
The invention belongs to the technical field of isotope medicament preparation, and particularly relates to a method for separating In, cd and Ag In a target.
Background
111 In has a half-life of 2.83 d, emits two gamma rays having energies of 173 keV and 247keV by electron capture decay energy, can be used as a radioisotope for diagnosis, 111 in-labeled radiopharmaceuticals are mainly used for tumor imaging. 111 The production method of In mainly comprises three methods: (1) Proton bombardment by cyclotron 112 Cd is obtained, and the energy of the proton stream is required to be 16-22 MeV; (2) Proton bombardment by cyclotron 111 Cd is obtained, and the energy of the proton stream is required to be 4-15 MeV; (3) By alpha particle striking 109 Ag is obtained, and the energy of the alpha particle stream is required to be 15-30 MeV. Among them, the method (3) has the advantages over the methods (1) and (2) that: the use method (3) can not generate nuclides with long service life and high energy gamma rays 114m In (t=49.5 d), and natural silver can be used as Ag target, which is very convenient, and thus, hit by alpha particles 109 Ag acquisition 111 In is very popular. 111 In preparation, preparing high-purity natural Ag into Ag foil, and placing into reactorOr accelerator, using alpha irradiation of 15-30 MeV to prepare 111 In. However, the prior art lacks a method for separating In, cd and Ag In the target.
Disclosure of Invention
Aiming at the defects, the invention provides a method for separating In, cd and Ag In a target, which has good selectivity and can efficiently separate In, cd and Ag.
The invention provides a method for separating In, cd and Ag In a target, which comprises the following steps:
and heating the target In vacuum, and distilling to remove Cd to obtain a target substrate, wherein the target substrate contains In and Ag.
And (3) placing the target substrate into acid liquor for acid leaching to obtain acid leaching liquor, wherein the acid liquor is nitric acid or non-nitric acid, and when the nitric acid is used for acid leaching, alkali metal halogen salt is required to be added, so that the Ag is separated out in a precipitation form. When the acid leaching is performed using the non-nitric acid, the Ag is converted into a water-insoluble compound.
Filtering the pickle liquor to obtain filtrate containing In, and purifying the filtrate by using a resin adsorption or extraction method to obtain In.
Further, the vacuum degree of the vacuum heating is 5-50 Pa, the temperature of the vacuum heating is 700-800 ℃, and the time of the vacuum heating is 2-3 hours.
Further, the non-nitric acid is selected from HC, HBr and H 2 SO 4 One of them.
Further, the alkali metal halide salt is selected from one of NaCl, naBr, KCl and KBr.
Further, the concentration of the acid liquor is 4-8 mol/L, the temperature of the acid leaching is 50-90 ℃, the stirring rate of the acid leaching is 200-600 r/min, and the time of the acid leaching is 1-6 h.
Further, the resin selected in the resin adsorption step is cation exchange resin or chelating resin.
Further, the extractant of the extraction step is selected from one of a neutral extractant, an amine extractant and an acidic extractant.
Further, the neutral extractant is TBP. The amine extractant is N235. The acidic extractant is P507.
The beneficial effects are that:
according to the invention, through vacuum heating of the target, the principle of boiling point difference of Cd, in and Ag is effectively utilized, cd is directly removed, separation of In and Cd is realized, the separation efficiency is high, the method belongs to physical separation, and the loss of In and Cd is less. According to the invention, the target substrate is subjected to acid leaching, nitric acid and alkali metal halogen salt are used or non-nitric acid is used to convert Ag into precipitate, and the precipitate is filtered and removed, so that the effective separation of In and Ag is realized. The method can effectively separate three elements of Cd, in and Ag, and simultaneously can recycle the high purity of In and Cd.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Wherein:
FIG. 1 is a flow chart of a method for separating In, cd, and Ag from a target using non-nitric acid leaching In one embodiment of the invention;
FIG. 2 is a flow chart of a method for separating In, cd, and Ag from a target using nitric acid leaching In one embodiment of the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-2, the invention provides a method for separating In, cd and Ag In a target, comprising the following steps:
the target is vacuum heated, and a micro distillation device can be selected for vacuum heating, wherein the micro distillation device is made of quartz, zirconia, magnesia and other materials and is provided with a cold end, so that condensation distillation of distilled metal is facilitated. And distilling to remove Cd to obtain a target substrate, wherein the target substrate contains In and Ag.
And (3) placing the target substrate into acid liquor for acid leaching to obtain acid leaching liquor, wherein the acid liquor is nitric acid or non-nitric acid, and when the acid leaching is carried out by using nitric acid, alkali metal halogen salt is required to be added, so that Ag is separated out in a precipitation form. When acid leaching is performed using non-nitric acid, ag is converted into water-insoluble compounds.
Filtering the pickle liquor to obtain filtrate containing In, and purifying the filtrate by using a resin adsorption or extraction method to obtain In.
According to the invention, through vacuum heating of the target, the principle of boiling point difference of Cd, in and Ag is effectively utilized, cd is directly removed, separation of In and Cd is realized, the separation efficiency is high, the method belongs to physical separation, and the loss of In and Cd is less. According to the invention, the target substrate is subjected to acid leaching, nitric acid and alkali metal halogen salt are used or non-nitric acid is used to convert Ag into precipitate, and the precipitate is filtered and removed, so that the effective separation of In and Ag is realized. The method can effectively separate three elements of Cd, in and Ag, and simultaneously can recycle the high purity of In and Cd.
In one embodiment, the vacuum degree of the vacuum heating is 5-50 Pa, the temperature of the vacuum heating is 700-800 ℃, and the time of the vacuum heating is 2-3 hours.
In one embodiment, the non-nitric acid is selected from HC, HBr, and H 2 SO 4 One of them.
In a specific embodiment, the alkali metal halide salt is selected from one of NaCl, naBr, KCl and KBr.
In a specific embodiment, the concentration of the acid solution is 4-8 mol/L, the acid leaching temperature is 50-90 ℃, the stirring rate of the acid leaching is 200-600 r/min, and the acid leaching time is 1-6 h.
In one embodiment, the resin selected for the resin adsorption step is a cation exchange resin or a chelating resin. The resin is preferably a Dowex 1*4 type resin column.
In a specific embodiment, the extractant of the extraction step is selected from one of a neutral extractant, an amine extractant, and an acidic extractant.
In one embodiment, the neutral extractant is TBP. The amine extractant is N235. The acidic extractant is P507.
The following are specific examples.
The separation method is element separation and non-isotope separation, namely, the separation of different isotopes of the same element and different isotopes of another element is applicable to the process of the invention, so that the non-radioactive isotope can be used for a simulated cold experiment to replace a real radioactive isotope separation experiment.
Example 1
The experimental target was cooled using a natural Ag target with a purity of 6N and doped with 100 ppm In and 10 ppm Cd. The total weight of the target was 500 mg.
Placing the target in a high-purity quartz tray, and then placing the tray in a vacuum distillation furnace; firstly, introducing high-purity Ar gas (purity is more than 6N) into a vacuum distillation furnace for 10 min, closing a gas valve, and pumping the vacuum distillation furnace chamber to a vacuum degree of 5 Pa; the Ar gas was repeatedly introduced and evacuated to 5 Pa, and this step was repeated three times. Argon is again introduced to maintain the pressure in the chamber at 20 Pa. Heating to 750 ℃ by electrifying, and preserving heat for 2 h; in this step, the condensing section was cooled with circulating water and Cd condensate was collected. The target was removed and placed in 6 mol/L HCl solution, heated to 80℃and stirred at 500 r/min, maintaining 3 h. Filtering to obtain a filtrate which is a salt solution containing In, passing the filtrate through a Dowex 1*4 type resin column for three times, eluting with 0.05 mol/L hydrochloric acid, obtaining the eluted solution which is a high-purity In-containing solution, and reducing filter residues which are AgCl to obtain the metal Ag.
Through detection, the total content of impurities In the obtained In solution is less than 50 ppm, the content of Ag is less than 10 ppm, and the content of impurity Cd is less than 4 ppm.
Example 2
The experimental target was cooled using a natural Ag target with a purity of 6N and doped with 100 ppm In and 10 ppm Cd. The total weight of the target was 500 mg.
Placing the target in a high-purity quartz tray, and then placing the tray in a vacuum distillation furnace; high purity Ar gas (purity)>6N) introducing the mixture into a vacuum distillation furnace for 10 min, closing a gas valve, and pumping the vacuum distillation furnace chamber to a vacuum degree of 5 Pa; the Ar gas was repeatedly introduced and evacuated to 5 Pa, and this step was repeated three times. Argon is again introduced to maintain the pressure in the chamber at 20 Pa. Heating to 750 ℃ by electrifying, and preserving heat for 2 h; in this step, the condensing section was cooled with circulating water and Cd condensate was collected. Taking out the target, and placing the target at HNO of 6 mol/L 3 In the process, the mixture was heated to 85℃and stirred at a rate of 400 r/min. After the target is completely dissolved, adding a proper amount of NaBr, filtering to obtain a filtrate which is a salt solution containing In, extracting the indium In the solution for three times by using a P507 extractant, carrying out back extraction by using 1 mol/L HCl acid to obtain the salt solution of In, wherein filter residues are AgBr, and reducing to obtain the metal Ag.
Through detection, the total content of impurities In the obtained In solution is less than 70 ppm, the content of Ag is less than 40 ppm, and the content of impurity Cd is less than 5 ppm.
The foregoing disclosure is illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (8)
1. A method for separating In, cd and Ag from a target, comprising the steps of:
vacuum heating a target, and distilling to remove Cd to obtain a target substrate, wherein the target substrate contains In and Ag;
acid leaching is carried out on the target substrate by putting acid liquor into the target substrate to obtain acid leaching liquor, wherein the acid liquor is nitric acid or non-nitric acid, and alkali metal halogen salt is required to be added when the nitric acid is used for acid leaching, so that the Ag is separated out in a precipitation form; upon acid leaching with the non-nitric acid, the Ag is converted to a water-insoluble compound;
filtering the pickle liquor to obtain filtrate containing In, and purifying the filtrate by using a resin adsorption or extraction method to obtain In.
2. The method for separating In, cd and Ag from a target according to claim 1, wherein the vacuum degree of vacuum heating is 5 to 50pa, the temperature of vacuum heating is 700 to 800 ℃, and the time of vacuum heating is 2 to 3 hours.
3. The method of separating In, cd and Ag In a target according to claim 1, wherein said non-nitric acid is selected from the group consisting of HC, HBr and H 2 SO 4 One of them.
4. The method of claim 1, wherein the alkali metal halide salt is selected from one of NaCl, naBr, KCl and KBr.
5. The method for separating In, cd and Ag from a target according to claim 1, wherein the concentration of the acid solution is 4-8 mol/L, the temperature of the acid leaching is 50-90 ℃, the stirring rate of the acid leaching is 200-600 r/min, and the time of the acid leaching is 1-6 h.
6. The method of separating In, cd and Ag from a target according to claim 1, wherein the resin selected In the resin adsorption step is a cation exchange resin or a chelate resin.
7. The method of separating In, cd and Ag from a target according to claim 1, wherein the extractant of the extraction step is one selected from the group consisting of neutral extractants, amine extractants and acidic extractants.
8. The method of separating In, cd and Ag from a target of claim 7, wherein the neutral extractant is TBP; the amine extractant is N235; the acidic extractant is P507.
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| CN202311349745.4A CN117385177A (en) | 2023-10-18 | 2023-10-18 | Method for separating In, cd and Ag In target |
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| CN202311349745.4A CN117385177A (en) | 2023-10-18 | 2023-10-18 | Method for separating In, cd and Ag In target |
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Application publication date: 20240112 |