CN115676920A - Method for purifying ammonium chloroiridate - Google Patents
Method for purifying ammonium chloroiridate Download PDFInfo
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- CN115676920A CN115676920A CN202211375012.3A CN202211375012A CN115676920A CN 115676920 A CN115676920 A CN 115676920A CN 202211375012 A CN202211375012 A CN 202211375012A CN 115676920 A CN115676920 A CN 115676920A
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Abstract
The invention belongs to the technical field of platinum group metal compound purification. The invention provides a method for purifying ammonium chloroiridate, which comprises the following steps: reacting the ammonium chloroiridate crude product, water and a reducing agent, and filtering through a microporous filter membrane to obtain a solution; and reacting the solution with an oxidant to obtain ammonium chloroiridate. The purification method does not relate to ammonium sulfide, thereby avoiding the generation of sulfide and reducing the pollution to the environment; the method has the advantages of simple operation, short time, high iridium yield, good purity of the ammonium chloroiridate, quality superior to YS/T1322-2019 ammonium chloroiridate industrial standard and suitability for industrial production.
Description
Technical Field
The invention relates to the technical field of platinum group metal compound purification, in particular to a method for purifying ammonium chloroiridate.
Background
Ammonium chloroiridate is a red-black six-sided crystal, is used as an important precursor of iridium and iridium compounds, and has the characteristics of easy purification, high recovery rate and the like. In the literatures of "application of platinum group metal property metallurgical material" and "extraction and refining of precious metal", ammonium chloride iridate is purified by an ammonium sulfide precipitation method, specifically, ammonium chloride iridate and a reducing agent are dissolved in water, ammonium sulfide is used to separate impurity elements in a solution, and finally, an oxidizing agent is used to oxidize, precipitate and filter out the purified ammonium chloride iridate.
Therefore, research and development of a purification method with high iridium yield and good ammonium chloroiridate purity have good application prospect.
Disclosure of Invention
The invention aims to provide a method for purifying ammonium chloroiridate aiming at the defects of the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for purifying ammonium chloroiridate, which comprises the following steps:
1) Reacting the ammonium chloroiridate crude product, water and a reducing agent, and filtering through a microporous filter membrane to obtain a solution;
2) And reacting the solution with an oxidant to obtain ammonium chloroiridate.
Preferably, the content of iridium in the crude ammonium chloroiridate product in the step 1) is 36-43%, and the purity of the crude ammonium chloroiridate product is 90-99.5%.
Preferably, the reducing agent in step 1) is one or two of formic acid, hydroxylamine hydrochloride, oxalic acid, hydrazine hydrate, sodium sulfite and hydrazine hydrochloride.
Preferably, the mass ratio of the crude ammonium iridate chloride, water and the reducing agent in the step 1) is 1:2 to 10:0.05 to 0.5; the aperture of the microporous filter membrane is 0.2-0.3 μm.
Preferably, the reaction temperature in the step 1) is 100-120 ℃, and the reaction time is 5-30 min.
Preferably, the oxidant in the step 2) is chlorine, nitric acid, a sodium chlorate solution, hydrogen peroxide or a sodium hypochlorite solution; the mass concentration of the nitric acid is 60-70%, the mass concentration of the hydrogen peroxide is 25-35%, and the mass concentration of the sodium chlorate solution and the mass concentration of the sodium hypochlorite solution are respectively 5-15%.
Preferably, the mass ratio of the oxidant in the step 2) to the crude ammonium chloroiridate in the step 1) is 0.05-2: 1.
preferably, the iridium concentration in the solution in the step 2) is 40-200 g/L.
Preferably, the reaction temperature in the step 2) is 100-120 ℃, and the reaction time is 10-60 min.
Preferably, after the reaction product is obtained in the step 2), the reaction product is filtered, washed and dried; the filtering time is 40-60 min; the washing reagent is ammonium chloride solution, and the washing times are 2-4 times; the mass concentration of the ammonium chloride solution is 12-15%; the drying temperature is 110-130 ℃, and the drying time is 0.5-1.5 h.
The beneficial effects of the invention include the following:
1) The purification method of ammonium chloroiridate does not relate to ammonium sulfide, avoids the generation of sulfide and reduces the pollution to the environment.
2) The purification method of ammonium chloroiridate has the advantages of simple operation, short time, high iridium yield, good purity of ammonium chloroiridate, quality superior to YS/T1322-2019 ammonium chloroiridate industrial standard and suitability for industrial production.
Detailed Description
The invention provides a method for purifying ammonium chloroiridate, which comprises the following steps:
1) Reacting the ammonium chloroiridate crude product, water and a reducing agent, and filtering through a microporous filter membrane to obtain a solution;
2) And reacting the solution with an oxidant to obtain ammonium chloroiridate.
In the invention, the content of iridium in the crude ammonium chloroiridate product in the step 1) is preferably 36-43%, more preferably 38-41%, and even more preferably 39-40%; the purity of the crude ammonium chloroiridate is preferably 90 to 99.5%, and more preferably 95 to 99.5%.
In the invention, the reducing agent in the step 1) is preferably one or two of formic acid, hydroxylamine hydrochloride, oxalic acid, hydrazine hydrate, sodium sulfite and hydrazine hydrochloride.
In the invention, the mass ratio of the crude ammonium chloroiridate in the step 1) to water to the reducing agent is preferably 1:2 to 10:0.05 to 0.5, more preferably 1:4 to 8:0.15 to 0.4, more preferably 1:5 to 7:0.25 to 0.3; the pore diameter of the microfiltration membrane is preferably 0.2 to 0.3. Mu.m, more preferably 0.22 to 0.28. Mu.m, and still more preferably 0.24 to 0.26. Mu.m.
In the invention, the adding sequence of the ammonium chloroiridate crude product, water and the reducing agent in the step 1) is as follows: mixing the ammonium chloroiridate crude product with water to obtain a solution I; and (3) adjusting the pH value of the solution I, heating, and adding a reducing agent for reaction.
In the invention, the reagent for adjusting the pH value of the solution I is dilute hydrochloric acid; the mass fraction of the dilute hydrochloric acid is preferably 15 to 25%, more preferably 18 to 22%, and still more preferably 20%; the pH value of the solution I is preferably adjusted to 0 to 3, more preferably 1 to 2, and still more preferably 2; the temperature for heating after adjusting the pH of the solution I is preferably 30 to 50 ℃, more preferably 35 to 45 ℃, and still more preferably 40 ℃.
In the invention, the solution in the step 1) is a transparent dark red solution.
In the invention, the reaction temperature in the step 1) is preferably 100-120 ℃, more preferably 105-115 ℃, and more preferably 110 ℃; the reaction time is preferably 5 to 30min, more preferably 10 to 25min, and still more preferably 15 to 20min.
In the invention, the oxidant in the step 2) is preferably chlorine, nitric acid, a sodium chlorate solution, hydrogen peroxide or a sodium hypochlorite solution; the mass concentration of the nitric acid is preferably 60 to 70%, more preferably 62 to 68%, and even more preferably 64 to 66%; the mass concentration of the hydrogen peroxide is preferably 25 to 35 percent, more preferably 28 to 32 percent, and even more preferably 30 percent; the mass concentration of the sodium chlorate solution and the mass concentration of the sodium hypochlorite solution are independently preferably 5 to 15%, more preferably 8 to 12%, and still more preferably 10%.
In the invention, the mass ratio of the oxidant in the step 2) to the crude ammonium chloroiridate in the step 1) is preferably 0.05-2: 1, more preferably 0.5 to 1.5:1, more preferably 0.8 to 1.2:1.
in the invention, the solution obtained in the step 1) is the solution obtained in the step 2) after the pH value of the solution is adjusted; the reagent for adjusting the pH value of the solution in the step 1) is dilute hydrochloric acid; the mass fraction of the dilute hydrochloric acid is preferably 15 to 25%, more preferably 18 to 22%, and still more preferably 20%; the pH of the solution in step 1) is preferably adjusted to 0 to 3, more preferably 1 to 2, and still more preferably 1.2 to 1.8.
In the present invention, the concentration of iridium in the solution of step 2) is preferably 40 to 200g/L, more preferably 80 to 160g/L, and still more preferably 100 to 140g/L.
In the invention, the iridium concentration in the solution reaches the requirement by adopting a heating and concentrating mode; the temperature for the heating concentration is preferably 100 to 120 ℃, more preferably 105 to 115 ℃, and still more preferably 110 ℃.
In the invention, the reaction temperature in the step 2) is preferably 100-120 ℃, more preferably 105-115 ℃, and more preferably 110 ℃; the reaction time is preferably 10 to 60min, more preferably 20 to 50min, and still more preferably 30 to 40min.
In the invention, after the reaction in the step 2) is carried out to obtain a reaction product, the reaction product is filtered, washed and dried; the filtering time is preferably 40-60 min, more preferably 45-55 min, and even more preferably 50min; the washing reagent is preferably an ammonium chloride solution; the number of washing is preferably 2 to 4, more preferably 3; the mass concentration of the ammonium chloride solution is preferably 12 to 15%, more preferably 12.5 to 14.5%, and still more preferably 13 to 14%; the drying temperature is preferably 110-130 ℃, more preferably 115-125 ℃, and more preferably 120 ℃; the drying time is preferably 0.5 to 1.5 hours, more preferably 0.8 to 1.2 hours, and still more preferably 1 hour.
In the invention, the reaction product in the step 2) is cooled to room temperature and then filtered to obtain crystals, and then the crystals are washed and dried.
In the invention, the ammonium chloroiridate in the step 2) is a red black granular crystal.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
999.94g of crude ammonium chloroiridate (iridium content 42.45% and purity of crude ammonium chloroiridate 98.71%) and 3000g of deionized water were mixed to obtain solution I; adjusting the pH value of the solution I to 1 by using 20% by mass of dilute hydrochloric acid, heating to 40 ℃, adding 70g of formic acid, reacting at 100 ℃ for 10min, and filtering by using a microporous filter membrane with the aperture of 0.2 mu m to obtain a transparent dark red solution.
Adjusting the pH value of the transparent dark red solution to 0.4 by using 20% by mass of dilute hydrochloric acid, heating and concentrating the solution at 100 ℃ until the concentration of iridium is 121.28g/L, stopping heating, adding 550g of hydrogen peroxide (in hydrogen peroxide, the mass concentration of hydrogen peroxide is 25%), and reacting for 10min at 110 ℃ to obtain a reaction product; cooling the reaction product to room temperature, and filtering within 50min to obtain crystals; and washing the crystals for 3 times by adopting an ammonium chloride solution with the mass concentration of 14%, and then drying in an oven at the temperature of 120 ℃ for 0.5h to obtain red-black granular ammonium chloroiridate.
The ammonium chloroiridate prepared by the embodiment has the iridium content of 43.03% of 962.1g, the iridium yield of 97.53%, the purity of the ammonium chloroiridate detected to be 99.97%, and the quality superior to the YS/T1322-2019 ammonium chloroiridate industrial standard.
Example 2
1000.11g of crude ammonium chloroiridate (iridium content is 41.44%, purity of crude ammonium chloroiridate is 96.38%) and 4000g of deionized water are mixed to obtain solution I; adjusting the pH value of the solution I to 2 by using 15% by mass of dilute hydrochloric acid, heating to 30 ℃, adding 80g of hydroxylamine hydrochloride, reacting at 120 ℃ for 5min, and filtering by using a microporous filter membrane with the aperture of 0.3 mu m to obtain a transparent dark red solution.
Adjusting the pH value of the transparent dark red solution to 0.5 by using dilute hydrochloric acid with the mass fraction of 15%, heating and concentrating the solution at 120 ℃ until the concentration of iridium is 103.61g/L, stopping heating, then adding 400g of nitric acid aqueous solution (in the nitric acid aqueous solution, the mass concentration of nitric acid is 60%), and reacting for 20min at 120 ℃ to obtain a reaction product; cooling the reaction product to room temperature, and filtering within 40min to obtain crystals; and washing the crystals for 4 times by adopting an ammonium chloride solution with the mass concentration of 15%, and then drying in an oven at 110 ℃ for 1.5h to obtain red-black granular ammonium chloroiridate.
The ammonium chloroiridate 919.63g with the iridium content of 43.07% is prepared in the embodiment, the iridium yield is 95.57%, the purity of the ammonium chloroiridate is 99.96% through detection, and the quality of the ammonium chloroiridate is superior to the industrial standard of YS/T1322-2019 ammonium chloroiridate.
Example 3
Mixing 1000g of crude ammonium chloroiridate (the iridium content is 40.94%, and the purity of the crude ammonium chloroiridate is 95.22%) with 2000g of deionized water to obtain a solution I; adjusting the pH value of the solution I to 3 by using dilute hydrochloric acid with the mass fraction of 25%, heating to 50 ℃, adding 50g of sodium sulfite, reacting at 110 ℃ for 20min, and filtering by using a microporous filter membrane with the aperture of 0.25 mu m to obtain a transparent dark red solution.
Adjusting the pH value of a transparent dark red solution to 1 by using 20% by mass of dilute hydrochloric acid, heating and concentrating the transparent dark red solution at 110 ℃ until the iridium concentration is 163.76g/L, stopping heating, adding 50g of a sodium chlorate solution (the mass concentration of sodium chlorate in the sodium chlorate solution is 15%), and reacting for 60min at 100 ℃ to obtain a reaction product; cooling the reaction product to room temperature, and filtering within 50min to obtain crystals; and washing the crystals for 2 times by adopting an ammonium chloride solution with the mass concentration of 12%, and then drying in an oven at the temperature of 130 ℃ for 1h to obtain red-black granular ammonium chloroiridate.
The ammonium chloroiridate 907.64g with the iridium content of 42.97% is prepared in the embodiment, the iridium yield is 95.26%, the purity of the ammonium chloroiridate is 99.97% through detection, and the quality of the ammonium chloroiridate is superior to the YS/T1322-2019 ammonium chloroiridate industrial standard.
Example 4
1000.06g of crude ammonium chloroiridate (iridium content 39.68% and purity 92.27%) and 5000g of deionized water were mixed to obtain a solution I; adjusting the pH value of the solution I to 2 by using 20% by mass of dilute hydrochloric acid, heating to 40 ℃, adding 120g of hydrazine hydrochloride, reacting at 115 ℃ for 30min, and filtering by using a microporous filter membrane with the aperture of 0.28 mu m to obtain a transparent dark red solution.
Adjusting the pH value of the transparent dark red solution to 1 by using 20% by mass of dilute hydrochloric acid, heating and concentrating the solution at 120 ℃ until the iridium concentration is 132.27g/L, stopping heating, adding 200g of sodium hypochlorite solution (the mass concentration of sodium hypochlorite in the sodium hypochlorite solution is 5%), and reacting at 115 ℃ for 40min to obtain a reaction product; cooling the reaction product to room temperature, and filtering within 50min to obtain crystals; and washing the crystals for 3 times by adopting an ammonium chloride solution with the mass concentration of 14%, and then drying in an oven at 125 ℃ for 0.8h to obtain red-black granular ammonium chloroiridate.
The ammonium chloroiridate 877.45g with the iridium content of 42.97% is prepared in the embodiment, the iridium yield is 95.01%, the purity of the ammonium chloroiridate is 99.96% through detection, and the quality of the ammonium chloroiridate is superior to the YS/T1322-2019 ammonium chloroiridate industrial standard.
Example 5
1000.18g of crude ammonium chloroiridate (the iridium content is 36.51%, and the purity of the crude ammonium chloroiridate is 95.37%) and 4000g of deionized water are mixed to obtain a solution I; adjusting the pH value of the solution I to 2 by using 20% by mass of dilute hydrochloric acid, heating to 35 ℃, adding 200g of oxalic acid and 100g of hydrazine hydrate, reacting at 105 ℃ for 25min, and filtering by using a microporous filter membrane with the aperture of 0.3 mu m to obtain a transparent dark red solution.
Adjusting the pH value of the transparent dark red solution to 2 by using 20% by mass of dilute hydrochloric acid, heating and concentrating the solution at 100 ℃ until the concentration of iridium is 121.72g/L, stopping heating, adding 500g of hydrogen peroxide (in hydrogen peroxide, the mass concentration of hydrogen peroxide is 35%), and reacting for 35min at 120 ℃ to obtain a reaction product; cooling the reaction product to room temperature, and filtering within 50min to obtain crystals; and washing the crystals for 3 times by adopting an ammonium chloride solution with the mass concentration of 15%, and then drying in an oven at 115 ℃ for 0.5h to obtain red-black granular ammonium chloroiridate.
The ammonium chloroiridate 889.76g with the iridium content of 40.25% is prepared in the embodiment, the iridium yield is 98.07%, the purity of the ammonium chloroiridate is 99.95% through detection, and the quality of the ammonium chloroiridate is superior to the industrial standard of YS/T1322-2019 ammonium chloroiridate.
From examples 1 to 5, it can be seen that: the purification method of ammonium chloroiridate can obtain high-yield iridium and high-purity ammonium chloroiridate, and the quality of the ammonium chloroiridate is superior to the industry standard of YS/T1322-2019 ammonium chloroiridate, and the purification method is suitable for industrial production.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for purifying ammonium chloroiridate is characterized by comprising the following steps:
1) Reacting the ammonium chloroiridate crude product, water and a reducing agent, and filtering through a microporous filter membrane to obtain a solution;
2) And reacting the solution with an oxidant to obtain the ammonium iridate chloride.
2. The purification method of claim 1, wherein the iridium content in the crude ammonium chloroiridate of step 1) is 36 to 43% and the purity of the crude ammonium chloroiridate is 90 to 99.5%.
3. The purification method according to claim 1 or 2, wherein the reducing agent in step 1) is one or two of formic acid, hydroxylamine hydrochloride, oxalic acid, hydrazine hydrate, sodium sulfite and hydrazine hydrochloride.
4. The purification process according to claim 3, wherein the mass ratio of the crude ammonium iridate chloride, water and the reducing agent in step 1) is 1:2 to 10:0.05 to 0.5; the aperture of the microporous filter membrane is 0.2-0.3 μm.
5. The purification method according to claim 4, wherein the reaction temperature in step 1) is 100 to 120 ℃ and the reaction time is 5 to 30min.
6. The purification method according to claim 4 or 5, wherein the oxidant in step 2) is chlorine gas, nitric acid, a sodium chlorate solution, hydrogen peroxide or a sodium hypochlorite solution; the mass concentration of the nitric acid is 60-70%, the mass concentration of the hydrogen peroxide is 25-35%, and the mass concentration of the sodium chlorate solution and the mass concentration of the sodium hypochlorite solution are respectively 5-15%.
7. The purification method according to claim 6, wherein the mass ratio of the oxidant in step 2) to the crude ammonium chloroiridate in step 1) is 0.05-2: 1.
8. the purification method according to claim 7, wherein the concentration of iridium in the solution of step 2) is 40 to 200g/L.
9. The purification method according to claim 7 or 8, wherein the reaction temperature in step 2) is 100 to 120 ℃ and the reaction time is 10 to 60min.
10. The purification method according to claim 9, wherein after the reaction of step 2) to obtain the reaction product, the reaction product is filtered, washed and dried; the filtering time is 40-60 min; the washing reagent is ammonium chloride solution, and the washing times are 2-4 times; the mass concentration of the ammonium chloride solution is 12-15%; the drying temperature is 110-130 ℃, and the drying time is 0.5-1.5 h.
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| CN202211375012.3A CN115676920A (en) | 2022-11-04 | 2022-11-04 | Method for purifying ammonium chloroiridate |
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| CN202211375012.3A CN115676920A (en) | 2022-11-04 | 2022-11-04 | Method for purifying ammonium chloroiridate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR973009A (en) * | 1947-10-06 | 1951-02-06 | Mond Nickel Company | Iridium refining process |
| CN109055738A (en) * | 2018-08-27 | 2018-12-21 | 浙江特力再生资源有限公司 | Noble metal recoverying and utilizing method in a kind of osmium iridium ruthenium mine |
| CN111112637A (en) * | 2020-02-27 | 2020-05-08 | 贵研铂业股份有限公司 | Method for preparing 5N-grade high-purity iridium powder |
| CN113477939A (en) * | 2021-06-30 | 2021-10-08 | 安徽拓思贵金属有限公司 | Preparation method of high-purity iridium powder |
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2022
- 2022-11-04 CN CN202211375012.3A patent/CN115676920A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR973009A (en) * | 1947-10-06 | 1951-02-06 | Mond Nickel Company | Iridium refining process |
| CN109055738A (en) * | 2018-08-27 | 2018-12-21 | 浙江特力再生资源有限公司 | Noble metal recoverying and utilizing method in a kind of osmium iridium ruthenium mine |
| CN111112637A (en) * | 2020-02-27 | 2020-05-08 | 贵研铂业股份有限公司 | Method for preparing 5N-grade high-purity iridium powder |
| CN113477939A (en) * | 2021-06-30 | 2021-10-08 | 安徽拓思贵金属有限公司 | Preparation method of high-purity iridium powder |
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