CN114672659A - Method for preparing rhodium iodide from iridium-rhodium alloy leaching solution - Google Patents
Method for preparing rhodium iodide from iridium-rhodium alloy leaching solution Download PDFInfo
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- CN114672659A CN114672659A CN202210351655.8A CN202210351655A CN114672659A CN 114672659 A CN114672659 A CN 114672659A CN 202210351655 A CN202210351655 A CN 202210351655A CN 114672659 A CN114672659 A CN 114672659A
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- KXAHUXSHRWNTOD-UHFFFAOYSA-K rhodium(3+);triiodide Chemical compound [Rh+3].[I-].[I-].[I-] KXAHUXSHRWNTOD-UHFFFAOYSA-K 0.000 title claims abstract description 51
- SXRIPRHXGZHSNU-UHFFFAOYSA-N iridium rhodium Chemical compound [Rh].[Ir] SXRIPRHXGZHSNU-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002386 leaching Methods 0.000 title claims abstract description 46
- 229910000629 Rh alloy Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 49
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 46
- 239000010948 rhodium Substances 0.000 claims abstract description 46
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims abstract description 46
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 14
- 229910000575 Ir alloy Inorganic materials 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 238000006722 reduction reaction Methods 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 54
- 239000000047 product Substances 0.000 description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- XJUCCGJZENLZSA-UHFFFAOYSA-M [Rh]Cl Chemical compound [Rh]Cl XJUCCGJZENLZSA-UHFFFAOYSA-M 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 230000020477 pH reduction Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021639 Iridium tetrachloride Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- IZJHFJOSJRYLBF-UHFFFAOYSA-N azanium;iridium;chloride Chemical compound [NH4+].[Cl-].[Ir] IZJHFJOSJRYLBF-UHFFFAOYSA-N 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- LFWGHOQHYGPAKO-UHFFFAOYSA-K rhodium trichloroiridium Chemical compound [Ir](Cl)(Cl)Cl.[Rh] LFWGHOQHYGPAKO-UHFFFAOYSA-K 0.000 description 1
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/005—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution, and belongs to the field of comprehensive utilization of secondary resources of precious metals. Adding a reducing agent into an iridium-rhodium alloy leaching solution to carry out a reduction reaction to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolyzed tin-removed solution of the rhodium-iridium alloy leaching solution; adding potassium iodide into the reaction system A, stirring and reacting for 1-4h at the temperature of 60-80 ℃, carrying out solid-liquid separation, and washing and vacuum drying the solid in sequence to obtain rhodium iodide. The method can prepare high-quality rhodium iodide from the iridium-rhodium alloy leaching solution, simultaneously realizes the further enrichment of iridium, and is beneficial to the subsequent separation of rhodium and iridium.
Description
Technical Field
The invention relates to a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution, and belongs to the field of comprehensive utilization of secondary resources of precious metals.
Background
The iridium-rhodium alloy has good oxidation resistance at high temperature, is an important material for manufacturing a high-temperature thermocouple, can measure the high temperature of 2000 ℃ in an oxidation atmosphere, and is an extremely important temperature measuring tool in high-temperature experiments, rocket technology, aviation and aerospace technology. The rhodium-iridium alloy waste is generated in the thermocouple preparation and processing processes, and needs to be separated, purified and recycled due to high value. The leaching rates of rhodium and iridium in aqua regia respectively reach 75 percent, 85 percent and above after the iridium and rhodium alloy waste is subjected to alloy crushing, tin is one of metals with good crushing treatment effects of the iridium and rhodium alloy waste, the pH value of a solution after the aqua regia is leached is adjusted to 2-3 by adopting a hydrolysis method, the tin in the solution can be effectively removed, the solution after the tin removal is an acidic rhodium and iridium chloride complex solution, and the molar ratio of rhodium to iridium is 1-3.
For a solution system with the rhodium content and the iridium content which are not greatly different, the efficient separation of the rhodium and the iridium is one of the world problems in the metallurgical industry. The solution system is generally prepared by separating most of iridium or rhodium through various chemical precipitation methods to obtain a solution system containing a large amount of rhodium and a small amount of iridium or containing a large amount of iridium and a small amount of rhodium, and then separating rhodium from iridium through an ion exchange method, a solvent extraction method and the like. For the tin-removed liquid, the content of rhodium and iridium is not greatly different, ammonium chloride is usually adopted to deposit iridium, most of iridium is separated and enriched in the form of ammonium chloroiridate, and the ammonium chlororhodanate solution taking rhodium as a main body is obtained. Because part of rhodium is coprecipitated while the iridium is precipitated by ammonium chloride, the iridium needs to be purified and refined subsequently; the iridium cannot be completely removed by ammonium chloride iridium precipitation, the ammonium chlororhodate solution taking rhodium as a main body also contains a large amount of iridium, and rhodium and iridium separation and purification treatment is required to be carried out subsequently. The conventional process flow for separating rhodium from iridium in the tin-removed liquid is complicated, and the rhodium content in the intermediate product chloroiridic acid ammonia is high, so that the intermediate product chloroiridic acid ammonia cannot be used in a value-added manner as a product.
Disclosure of Invention
The invention provides a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution, aiming at the problem of rhodium and iridium separation and extraction in the iridium-rhodium alloy leaching solution, rhodium and iridium in the solution after tin removal exist in the form of chloride complex ions, the rhodium iodide is directly prepared from the solution to carry out crude separation of rhodium and iridium, the rhodium content in the solution is greatly reduced, rhodium iodide with higher purity is prepared, meanwhile, iridium enrichment is realized, tail solution containing a small amount of rhodium and a large amount of iridium is obtained after treatment, the method is favorable for subsequently separating and recovering the residual small amount of rhodium by adopting an ion exchange method or a solvent extraction method, and the efficient separation of rhodium and iridium is realized.
A method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution comprises the following specific steps:
(1) adding a reducing agent into the iridium-rhodium alloy leaching solution for reduction reaction to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolyzed tin-removed solution of the rhodium-iridium alloy leaching solution;
(2) adding potassium iodide into the reaction system A, stirring and reacting for 1-4h at the temperature of 60-80 ℃, carrying out solid-liquid separation, and carrying out ultrasonic washing and vacuum drying on the solid in sequence to obtain rhodium iodide.
The rhodium concentration in the iridium-rhodium alloy leaching solution is 0.1-0.3mol/L, and the molar ratio of rhodium to iridium is 1-3: 1.
The reducing agent in the step (1) is ascorbic acid, and the addition amount of the ascorbic acid is 1-4 times of the molar amount of iridium in the iridium-rhodium alloy leaching solution.
The temperature of the reduction reaction in the step (1) is room temperature to 60 ℃, and the reaction time is 15 to 60 min.
The addition amount of the potassium iodide in the step (2) is 3-9 times of the molar amount of rhodium in the iridium-rhodium alloy leaching solution in the step (1).
Preferably, the time of ultrasonic washing in the step (2) is 0.5-2.0 h; the temperature of vacuum drying is 50-80 ℃, and the time is 8-15 h.
The reaction principle is as follows:
adding a reducing agent into the liquid after tin removal to ensure that rhodium and iridium chloride complex ions maintain the valence of +3, wherein the reaction product of the iridium chloride complex ions with the valence of +3 and potassium iodide has better water solubility; and the rhodium chloride complex ion with the valence of +3 reacts with potassium iodide to obtain rhodium iodide, the rhodium iodide is insoluble in water, and the rhodium iodide is separated by utilizing the solubility difference, and the reaction equation is as follows:
[RhCl(OH2)5]2++3KI→RhI3↓+5H2O+3KCl
[IrCl4(OH2)2]-+3I-→IrI3+2H2O+4Cl-
the method can prepare rhodium iodide with higher quality, can greatly reduce the rhodium content in a mixed system, and realizes iridium enrichment.
The invention has the beneficial effects that:
(1) according to the method, rhodium iodide is directly prepared from the hydrolyzed detinned solution of the rhodium-iridium alloy leaching solution to carry out crude separation of rhodium and iridium, so that the content of rhodium in the solution is greatly reduced, rhodium iodide with higher purity is prepared, meanwhile, enrichment of iridium is realized, the operation is simple, the yield of rhodium iodide is high, and the loss amount of iridium in the solution is extremely small;
(2) the method is suitable for preliminary separation of rhodium and iridium in the rhodium-iridium-chloride complex ion mixed solution, and can separate and remove at least 96% of rhodium in the form of rhodium iodide and enrich iridium;
(3) the rhodium iodide obtained by the method has high purity, and the residual liquid after the reaction can be returned to a chlororhodium/iridium acid (salt) system only by acidification and oxidation, so that the subsequent further removal of a small amount of rhodium in the solution is facilitated, and the efficient separation of rhodium and iridium is realized.
Drawings
FIG. 1 is an X-ray diffraction pattern of the rhodium triiodide product of example 1;
FIG. 2 is an X-ray diffraction pattern of the rhodium triiodide product of example 4;
FIG. 3 is an X-ray diffraction pattern of a rhodium iodide product meeting national standards.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution comprises the following specific steps:
(1) adding 2.47g (0.014mol) of reducing agent (ascorbic acid) into 100mL of iridium-rhodium alloy leaching solution, and carrying out reduction reaction at 60 ℃ for 30min to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolysis detinning solution of the rhodium-iridium alloy leaching solution, the rhodium concentration is 0.1mol/L, the iridium concentration is 0.05mol/L, and the pH value is 2-3;
(2) adding 7.55g (0.045mol) of potassium iodide into a reaction system A, stirring and reacting for 2h at the temperature of 80 ℃, cooling to room temperature, carrying out solid-liquid separation to obtain a solid and a tail liquid, washing the solid by ultrasonic oscillation for 1h, and then placing the solid at the temperature of 50 ℃ for vacuum drying for 15h to obtain 4.71g of a rhodium iodide product;
the X-ray diffraction pattern of the rhodium iodide product of this example is shown in fig. 1, and as can be seen by comparing fig. 1 and fig. 3, the diffraction peak angles of the X-ray diffraction patterns of the obtained product and standard rhodium iodide are completely consistent, and the obtained product can be identified as rhodium iodide;
in the rhodium iodide product of the embodiment, the rhodium content is 21.05%, the iridium content is 0.017%, the content of other impurities reaches the standard, the yield of rhodium iodide is 96.35%, and the iridium loss is less than 0.084%; after the tail liquid is concentrated, hydrochloric acid is used for acidification, and a small amount of hydrogen peroxide is added for removing iodine, so that the solution can be recovered to be in the forms of chlororhodium and iridate.
Example 2: a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution comprises the following specific steps:
(1) adding 1.77g (0.01mol) of reducing agent (ascorbic acid) into 100mL of iridium-rhodium alloy leaching solution, and carrying out reduction reaction for 38min at the temperature of 45 ℃ to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolysis detinning solution of the rhodium-iridium alloy leaching solution, the rhodium concentration is 0.15mol/L, the iridium concentration is 0.05mol/L, and the pH value is 2-3;
(2) adding 7.55g (0.045mol) of potassium iodide into a reaction system A, stirring and reacting for 3h at the temperature of 70 ℃, cooling to room temperature, carrying out solid-liquid separation to obtain a solid and a tail liquid, washing the solid by ultrasonic oscillation for 0.8h, and then placing the washed solid at the temperature of 60 ℃ for vacuum drying for 12h to obtain 6.99g of a rhodium iodide product;
in the embodiment, the rhodium iodide product contains 21.02 percent of rhodium, 0.011 percent of iridium and other impurities up to the standard, the yield of rhodium iodide is 96.42 percent, and the loss of iridium is less than 0.090 percent; after the tail liquid is concentrated, hydrochloric acid is used for acidification, and a small amount of hydrogen peroxide is added for removing iodine, so that the solution can be recovered to be in the forms of chlororhodium and iridate.
Example 3: a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution comprises the following specific steps:
(1) adding 10.58g (0.06mol) of reducing agent (ascorbic acid) into 200mL of iridium-rhodium alloy leaching solution, and carrying out reduction reaction for 60min at the temperature of 35 ℃ to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolysis detinning solution of the rhodium-iridium alloy leaching solution, the rhodium concentration is 0.2mol/L, the iridium concentration is 0.08mol/L, and the pH value is 2-3;
(2) adding 53.12g (0.32mol) of potassium iodide into the reaction system A, stirring and reacting for 4h at the temperature of 60 ℃, cooling to room temperature, carrying out solid-liquid separation to obtain a solid and a tail liquid, washing the solid for 1.2h by ultrasonic oscillation, and carrying out vacuum drying at the temperature of 50 ℃ for 15h to obtain 18.58g of a rhodium iodide product;
in the rhodium iodide product of the embodiment, the rhodium content is 21.01%, the iridium content is 0.017%, the contents of other impurities reach the standard, the rhodium iodide yield is 96.07%, and the iridium loss is less than 0.083%; after the tail liquid is concentrated, hydrochloric acid is used for acidification, and a small amount of hydrogen peroxide is added for removing iodine, so that the solution can be recovered to be in the forms of chlororhodium and iridate.
Example 4: a method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution comprises the following specific steps:
(1) adding 17.65g (0.1mol) of reducing agent (ascorbic acid) into 500mL of iridium-rhodium alloy leaching solution, and carrying out reduction reaction at 55 ℃ for 20min to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolysis detinning solution of the rhodium-iridium alloy leaching solution, the rhodium concentration is 0.15mol/L, the iridium concentration is 0.15mol/L, and the pH value is 2-3;
(2) adding 112.05g (0.675mol) of potassium iodide into the reaction system A, stirring and reacting for 2h at the temperature of 80 ℃, cooling to room temperature, carrying out solid-liquid separation to obtain a solid and a tail liquid, washing the solid by ultrasonic oscillation for 1.5h, and then placing the solid at the temperature of 80 ℃ for vacuum drying for 10h to obtain 34.88g of a rhodium iodide product;
the X-ray diffraction pattern of the rhodium iodide product of the present example is shown in fig. 2, and as can be seen from the comparison of fig. 2 and fig. 3, the diffraction peak angles of the X-ray diffraction patterns of the obtained product and the standard rhodium iodide are completely consistent, and the obtained product can be identified as rhodium iodide;
in the rhodium iodide product of the embodiment, the rhodium content is 21.03%, the iridium content is 0.019%, the contents of other impurities reach the standard, the yield of rhodium iodide is 96.16%, and the iridium loss is less than 0.093%; after the tail liquid is concentrated, hydrochloric acid is used for acidification, and a small amount of hydrogen peroxide is added for removing iodine, so that the solution can be recovered to be in the forms of chlororhodium and iridate.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. A method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution is characterized by comprising the following specific steps:
(1) adding a reducing agent into the iridium-rhodium alloy leaching solution for reduction reaction to obtain a reaction system A; wherein the iridium-rhodium alloy leaching solution is a hydrolyzed tin-removed solution of the rhodium-iridium alloy leaching solution;
(2) adding potassium iodide into the reaction system A, stirring and reacting for 1-4h at the temperature of 60-80 ℃, carrying out solid-liquid separation, and carrying out ultrasonic washing and vacuum drying on the solid in sequence to obtain rhodium iodide.
2. The method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution according to claim 1, which is characterized in that: the rhodium concentration in the iridium-rhodium alloy leaching solution is 0.1-0.3mol/L, and the molar ratio of rhodium to iridium is 1-3: 1.
3. The method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution according to claim 1, which is characterized in that: the reducing agent in the step (1) is ascorbic acid, and the addition amount of the ascorbic acid is 1-4 times of the molar amount of iridium in the iridium-rhodium alloy leaching solution.
4. The method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution according to claim 1, which is characterized in that: the temperature of the reduction reaction in the step (1) is room temperature to 60 ℃, and the reaction time is 15 to 60 min.
5. The method for preparing rhodium iodide from an iridium-rhodium alloy leaching solution according to claim 1, which is characterized in that: the adding amount of the potassium iodide in the step (2) is 3-9 times of the molar amount of rhodium in the iridium-rhodium alloy leaching solution in the step (1).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010043895A1 (en) * | 2000-05-18 | 2001-11-22 | Haldor Topsoe A/S | Method for the preparation of rhodium containing solutions |
| CN1769187A (en) * | 2004-10-29 | 2006-05-10 | 中国石油化工股份有限公司 | Rhodium triiodid preparation method |
| WO2020006584A1 (en) * | 2018-06-29 | 2020-01-02 | Lessing Francesca Sarah | Pgm beneficiation |
| CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
| CN113618076A (en) * | 2021-07-21 | 2021-11-09 | 无锡威孚环保催化剂有限公司 | Sponge rhodium powder and preparation method thereof |
-
2022
- 2022-04-02 CN CN202210351655.8A patent/CN114672659A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010043895A1 (en) * | 2000-05-18 | 2001-11-22 | Haldor Topsoe A/S | Method for the preparation of rhodium containing solutions |
| CN1769187A (en) * | 2004-10-29 | 2006-05-10 | 中国石油化工股份有限公司 | Rhodium triiodid preparation method |
| WO2020006584A1 (en) * | 2018-06-29 | 2020-01-02 | Lessing Francesca Sarah | Pgm beneficiation |
| CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
| CN113618076A (en) * | 2021-07-21 | 2021-11-09 | 无锡威孚环保催化剂有限公司 | Sponge rhodium powder and preparation method thereof |
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Application publication date: 20220628 |