CN114293022B - Platinum iridium alloy separation method - Google Patents
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Abstract
The invention provides a platinum iridium alloy separation method, which comprises the following steps: (1) Heating platinum iridium alloy with aqua regia until the platinum iridium alloy is completely dissolved, and removing nitrate and acid; (2) Heating the solution, slowly adding a mixed solution of sodium hydroxide and an oxidant, adjusting the pH, cooling, standing and filtering to obtain a filter cake and a filtrate; (3) Heating the filtrate to 70-100 ℃, adding ammonium chloride solid to generate precipitate, standing and filtering, washing the precipitate, and reducing the precipitate with hydrazine hydrate to obtain platinum powder with purity more than or equal to 99.95%; (4) Heating and dissolving the filter cake obtained in the step (2) by using hydrochloric acid, adding ammonium chloride and an oxidant, precipitating solids, cooling, standing and filtering to obtain a filter cake; (5) Adding deionized water into the filter cake for heating, adding nitrite for complete dissolution, standing and cooling, filtering, washing and introducing hydrogen for reduction to obtain iridium powder with purity of more than or equal to 99.95%. The platinum iridium alloy separation method is simple to operate, high in separation efficiency, and the purity of the separated noble metal can reach 99.95% or more.
Description
Technical Field
The invention belongs to the technical field of noble metal purification, and particularly relates to a platinum iridium alloy separation method.
Background
Platinum group metals have many excellent physicochemical properties such as high temperature resistance, oxidation resistance, catalytic properties, corrosion resistance, etc., and have important applications in the fields of aerospace, chemical medicine, electronics, catalysts, etc. At present, few reported separation and purification methods of platinum and iridium are provided, and the main reason is that the physical and chemical properties of platinum and iridium compounds are similar, so that the separation and purification are difficult, and particularly, the purification method of platinum-containing iridium is complex and has low efficiency. The traditional method generally combines a precipitation method, an extraction method and an ion exchange resin method for repeated separation, has complex steps, low separation efficiency and higher cost. Against this background, we developed a simple method of platinum iridium alloy separation.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a platinum-iridium alloy separation method, realizes platinum-iridium separation through different solubilities of platinum and iridium related compounds under different systems, and provides a platinum-iridium alloy purification method with high efficiency and simple operation. The technical scheme adopted by the invention is as follows:
a platinum iridium alloy separation method, wherein: the method comprises the following steps:
(1) Heating 450-550 g of platinum iridium alloy with 2000-3000 mL aqua regia to completely dissolve, and then removing nitrate and acid;
(2) Heating the solution in the step (1) to 70-100 ℃, slowly adding a mixed solution of sodium hydroxide solution and oxidant, adjusting the pH to 8-12, generating a large amount of precipitate, cooling, standing and filtering to obtain a filter cake and filtrate;
(3) Heating the filtrate obtained in the step (2) to 70-100 ℃, adding 250-500 g ammonium chloride solids, generating a large amount of precipitate, standing, filtering, washing the precipitate with ammonium chloride solution to obtain a high-purity platinum compound, and reducing the high-purity platinum compound by hydrazine hydrate to obtain platinum powder with the purity of more than or equal to 99.95%;
(4) Heating and dissolving the filter cake obtained in the step (2) by using hydrochloric acid, adding 50-300 g of ammonium chloride and an oxidant under the stirring condition of 40-100 ℃, precipitating a large amount of solids, cooling, standing and filtering to obtain a filter cake;
(5) Adding deionized water into the filter cake obtained in the step (4), heating, gradually adding 200-400 g of nitrite to dissolve the filter cake, standing and cooling after complete dissolution, precipitating a large amount of solids, washing with cold water, filtering, and reducing to obtain iridium powder with purity more than or equal to 99.95%.
Preferably, the platinum iridium alloy separation method comprises the following steps: the oxidant in the step (2) and the oxidant in the step (4) are selected from one or any combination of hydrogen peroxide, sodium hypochlorite and sodium chlorate, wherein the dosage of the sodium chlorate is 20-50 g, and the dosage of the hydrogen peroxide and the sodium hypochlorite is 30-60 mL.
Preferably, the platinum iridium alloy separation method comprises the following steps: the mass fraction of the sodium hydroxide solution in the step (2) is 5-30%, and the mass ratio of the sodium hydroxide solution to the oxidant is 5-20: 1.
preferably, the platinum iridium alloy separation method comprises the following steps: the mass concentration of the ammonium chloride solution in the step (3) is 5-15%.
Preferably, the platinum iridium alloy separation method comprises the following steps: the cooling temperature in the step (5) is 0-10 ℃ and the cooling time is 2-50 h.
Preferably, the platinum iridium alloy separation method comprises the following steps: the nitrite in step (5) is an easily soluble nitrite, including but not limited to sodium nitrite and potassium nitrite, and may be a mixture of one or more easily soluble nitrites.
Preferably, the platinum iridium alloy separation method comprises the following steps: the step (5) of reduction specifically comprises the following steps: the solid is reduced by introducing hydrogen for 2 to 6 hours at the temperature of 600 to 680 ℃.
The invention has the advantages that:
the platinum-iridium alloy separation method is simple to operate, high in separation efficiency, and the purity of the separated platinum powder and iridium powder can reach 99.95% or more, and other separation methods require complicated steps, so that the purity of the product can reach 99.95% or more.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1
A platinum iridium alloy separation method, wherein: the method comprises the following steps:
(1) Placing 550g platinum-iridium alloy sheet (the iridium content is 10%) into a reaction bottle, then sequentially adding 2L aqua regia, heating until the platinum-iridium alloy sheet is completely dissolved, concentrating the solution to 1L, and then adding 2L hydrochloric acid to remove nitrate and maintaining the volume of the solution to 1L, and adding deionized water to remove acid by 3L;
(2) Heating the solution in the step (1) to 80 ℃, adding a mixed solution of sodium chlorate and sodium hydroxide, adjusting the pH to 10, standing, cooling, and filtering to obtain a blackish brown filter cake and a red filtrate;
(3) Heating the filtrate obtained in the step (2), adding 300g of ammonium chloride solid, standing, filtering, pulping a filter cake by using hot deionized water, slowly adding hydrazine hydrate under a stirring state until the solution is clear, filtering to obtain solid, calcining, introducing hydrogen, and reducing to obtain platinum powder with the purity of 99.95% or more;
(4) Dissolving the black brown filter cake obtained in the step (2) by using hydrochloric acid, adding 150g of ammonium chloride and 25g of sodium chlorate, precipitating a large amount of solid at the moment, standing, cooling and filtering;
(5) And (3) adding water into the filter cake obtained in the step (4) for dissolving, adding 200g of sodium nitrite under heating to dissolve the filter cake, standing at 4 ℃ for cooling for 5 hours after complete dissolution, filtering after a large amount of solids are separated out, washing the solids with cold water at 4 ℃ for three times, and drying the solids, and introducing hydrogen gas into the obtained solids at 650 ℃ for 2 hours to obtain iridium powder with the purity of 99.95% or more.
Example 2
A platinum iridium alloy separation method, wherein: the method comprises the following steps:
(1) Placing 500g platinum-iridium alloy sheets (the iridium content is 12%) into a reaction bottle, then sequentially adding 2.5L aqua regia, heating until the platinum-iridium alloy sheets are completely dissolved, concentrating the solution to 1L, and then adding 1.5L hydrochloric acid to remove nitrate and maintaining the volume of the solution to 1L, and adding 5L deionized water to remove acid;
(2) Heating the solution in the step (1) to 90 ℃, adding a mixed solution of sodium hypochlorite and sodium hydroxide, adjusting the pH to 12, standing, cooling, and filtering to obtain a blackish brown filter cake and a red filtrate;
(3) Heating the filtrate obtained in the step (2), adding 450g of ammonium chloride solid, standing, filtering, pulping a filter cake by using hot deionized water, slowly adding hydrazine hydrate under a stirring state until the solution is clarified, filtering to obtain solid, calcining, introducing hydrogen, and reducing to obtain platinum powder with the purity of 99.95% or more;
(4) Dissolving the black brown filter cake obtained in the step (2) by using hydrochloric acid, adding 250g of ammonium chloride, adding 30ml of 30% hydrogen peroxide solution, precipitating a large amount of solids at the moment, standing, cooling and filtering;
(5) Adding deionized water into the filter cake obtained in the step (4), adding 150g of sodium nitrite and 50g of potassium nitrite under heating to dissolve the filter cake, standing at 2 ℃ and cooling for 20h after complete dissolution, filtering after a large amount of solids are separated out, washing the solids with cold water at 2 ℃ for three times, and drying, and introducing hydrogen into the obtained solids at 600 ℃ for 5h, thereby obtaining the iridium powder with the purity of 99.95% or more.
Example 3
A platinum iridium alloy separation method, wherein: the method comprises the following steps:
(1) Placing 450g platinum-iridium alloy sheet (15% of iridium content) into a reaction bottle, sequentially adding 2.5L aqua regia, heating until the platinum-iridium alloy sheet is completely dissolved, concentrating the solution to 1L, adding 2.5L hydrochloric acid to remove nitrate, and adding deionized water to remove acid under the condition of maintaining the volume of the solution to 1L;
(2) Heating the solution in the step (1) to 85 ℃, adding a mixed solution of sodium chlorate and sodium hydroxide, adjusting the pH to 11, standing, cooling, and filtering to obtain a blackish brown filter cake and a red filtrate;
(3) Heating the filtrate obtained in the step (2), adding 500g of ammonium chloride solid, standing, filtering, pulping a filter cake by using hot deionized water, slowly adding hydrazine hydrate under a stirring state until the solution is clarified, filtering to obtain solid, calcining, introducing hydrogen, and reducing to obtain platinum powder with the purity of 99.95% or more;
(4) Dissolving the black brown filter cake obtained in the step (2) by using hydrochloric acid, adding 280g of ammonium chloride, adding 50ml of sodium hypochlorite solution, precipitating a large amount of solids at the moment, standing, cooling and filtering;
(5) And (3) adding water into the filter cake obtained in the step (4) for dissolving, adding 200g of sodium nitrite under heating to dissolve the filter cake, standing at 6 ℃ for cooling for 50 hours after complete dissolution, filtering after a large amount of solids are separated out, washing the solids with cold water at 6 ℃ for three times, drying, and introducing hydrogen into the obtained solids at 680 ℃ for 4 hours to obtain iridium powder with the purity of 99.95% or more.
The platinum-iridium alloy separation method is simple to operate and high in separation efficiency, and the purity of the separated platinum powder and iridium powder can reach 99.95% or more.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications and equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and all such modifications and equivalents are intended to be encompassed in the scope of the claims of the present invention.
Claims (5)
1. A platinum iridium alloy separation method is characterized in that: the method comprises the following steps:
(1) Heating 450-550 g of platinum iridium alloy with 2000-3000 mL aqua regia to completely dissolve, and then removing nitrate and acid;
(2) Heating the solution in the step (1) to 70-100 ℃, slowly adding a mixed solution of sodium hydroxide solution and oxidant, adjusting the pH to 8-12, generating a large amount of precipitate, cooling, standing and filtering to obtain a filter cake and filtrate;
(3) Heating the filtrate obtained in the step (2) to 70-100 ℃, adding 250-500 g ammonium chloride solids, generating a large amount of precipitate, standing, filtering, washing the precipitate with ammonium chloride solution to obtain a high-purity platinum compound, and reducing the high-purity platinum compound by hydrazine hydrate to obtain platinum powder with the purity of more than or equal to 99.95%;
(4) Heating and dissolving the filter cake obtained in the step (2) by using hydrochloric acid, adding 50-300 g of ammonium chloride and an oxidant under the stirring condition of 40-100 ℃, precipitating a large amount of solids, cooling, standing and filtering to obtain a filter cake;
(5) Adding deionized water into the filter cake obtained in the step (4), heating, gradually adding 200-400 g of nitrite to dissolve the filter cake, standing and cooling after complete dissolution, precipitating a large amount of solids, washing with cold water, filtering, and reducing to obtain iridium powder with purity more than or equal to 99.95%;
the oxidant in the step (2) and the oxidant in the step (4) are selected from one or any combination of hydrogen peroxide, sodium hypochlorite and sodium chlorate, the dosage of the sodium chlorate is 20-50 g, and the dosage of the hydrogen peroxide and the sodium hypochlorite is 30-60 mL;
the mass ratio of the sodium hydroxide solution to the oxidant is 5-20: 1, a step of;
the cooling temperature in the step (5) is 0-10 ℃ and the cooling time is 2-50 h.
2. The platinum iridium alloy separation method according to claim 1, wherein: and (2) the mass fraction of the sodium hydroxide solution in the step (2) is 5-30%.
3. The platinum iridium alloy separation method according to claim 1, wherein: the mass concentration of the ammonium chloride solution in the step (3) is 5-15%.
4. The platinum iridium alloy separation method according to claim 1, wherein: the nitrite in the step (5) is soluble nitrite.
5. The platinum iridium alloy separation method according to claim 1, wherein: the step (5) of reduction specifically comprises the following steps: the solid is reduced by introducing hydrogen for 2 to 6 hours at the temperature of 600 to 680 ℃.
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Citations (4)
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|---|---|---|---|---|
| US3876747A (en) * | 1972-08-10 | 1975-04-08 | Swarsab Mining | Separation and purification of iridium |
| CN102212696A (en) * | 2010-07-23 | 2011-10-12 | 金属回收科技有限公司 | Process for recovery of precious metals |
| CN109055774A (en) * | 2018-09-13 | 2018-12-21 | 陈永福 | A method of separating platinum, ruthenium and other platinum group metal hydroxide from the solution containing platinum group metal ion |
| CN111926195A (en) * | 2020-06-24 | 2020-11-13 | 重庆材料研究院有限公司 | Method for preparing high-purity platinum from platinum alloy waste |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2062804C1 (en) * | 1993-12-24 | 1996-06-27 | Красноярский завод цветных металлов | Method for extraction of iridium of material containing metals of platinum group |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3876747A (en) * | 1972-08-10 | 1975-04-08 | Swarsab Mining | Separation and purification of iridium |
| CN102212696A (en) * | 2010-07-23 | 2011-10-12 | 金属回收科技有限公司 | Process for recovery of precious metals |
| CN109055774A (en) * | 2018-09-13 | 2018-12-21 | 陈永福 | A method of separating platinum, ruthenium and other platinum group metal hydroxide from the solution containing platinum group metal ion |
| CN111926195A (en) * | 2020-06-24 | 2020-11-13 | 重庆材料研究院有限公司 | Method for preparing high-purity platinum from platinum alloy waste |
Non-Patent Citations (1)
| Title |
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| 余建明编著.贵金属分离与精炼工艺学.化学工业出版社,2016,(第二版),279-288、325-334. * |
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