CN103302298A - Method for separating and purifying iridium - Google Patents
Method for separating and purifying iridium Download PDFInfo
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- CN103302298A CN103302298A CN201310216080XA CN201310216080A CN103302298A CN 103302298 A CN103302298 A CN 103302298A CN 201310216080X A CN201310216080X A CN 201310216080XA CN 201310216080 A CN201310216080 A CN 201310216080A CN 103302298 A CN103302298 A CN 103302298A
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Abstract
The invention relates to a method for separating iridium from other platinum group metals and base metals in solution and purifying iridium. The special process comprises the following steps: (1) adjusting pH: controlling the mass concentration of iridium to be 60-100 g/L, and adjusting pH of the solution to be 1-3; (2), reducing: slowly adding aluminite powder in the solution of which pH is adjusted; (3), filtering: cooling, and then filtering and washing the solution after being reduced; (4) removing impurities: keeping the mass concentration of iridium solution after being filtered to be 30-50 g/L, adjusting pH to be 1-1.5, and then removing impurities for 2-4 times through using cation exchange resin to repeatedly exchange, and basically absorbing the base metals by resin; (5) concentrating and drying to obtain IrC13 crystals; and (6), reducing hydrogen: placing the dried IrC13 crystals into a hydrogen reduction furnace to be reduced to obtain iridium powder with the concentration higher than 99.95%. Compared with the prior art, the method to separate and purify iridium solution by adopting aluminium reduction and ion exchange to remove impurities has the advantages as follows: (1) the purity of iridium powder after hydrogen is reduced reaches more than 99.95%; (2), the direct recovery rate of iridium reaches more than 85%, and the total recovery rate of iridium is larger than 97%; and (3) the operation is simple, the use is practical, and the industrialization is easy to realize.
Description
Technical field
The present invention relates to the separation method between iridium and other platinum group metal and the base metal, especially separating-purifying iridium from the noble metal secondary resource waste material that contains iridium.
Background technology
The platinum group metal similar chemical characteristic is arranged so that the platinum group metal be separated from each other very difficult, wherein the separating-purifying of iridium especially the difficulty.The common method of separating-purifying iridium has hydrogen reduction method and precipitation method for refining from the hydrochloric acid solution that contains iridium.
Hydrogen reduction method separating-purifying iridium is divided into pressurization and non-pressure process.Patent CN87104181.2 is expensive from containing, separating-purifying iridium the iridium solution of base-metal ion: the precious metal impurity in the first step pressurized hydrogen Reduced separating iridium, then remove base metal by methods such as ion-exchanges; Second step pressurized hydrogen reduction obtains purity greater than 99.9% pure iridium powder, the rate of recovery of iridium〉99%; Patent CN1626690 adopts hydrogen reduction method from pure iridium rhodium solution rhodium to be reduced into metal under normal pressure and certain temperature, and iridium is not reduced, the purity of iridium behind the separate rhodium〉99.99%.At present, hydrogen reduction method is not realized industrial applications.
Chloride precipitation-ammonium sulfide is refining to be classical iridium method of refining, and patent CN201010567367.3 adopts the precipitate and separate purifying iridium, the steps include: that (1) will contain iridium material dissolving with hydrochloric acid; (2) add nitric acid and NH
4The Cl reaction obtains iridium platinum mixed-ammonium salt; (3) adding hydrazine hydrate makes the platinum reduction separate out black sponge platinum powder and iridium, iron tramp precipitation; (4) add H
2O
2Destroy hydrazine hydrate, add (NH
4)
2S purifies; (5) add Nitric Acid Oxidation and NH
4The Cl precipitation makes iridium generate (NH
4)
2IrCl
6(IV) then adds water slurry, adds hydrazine hydrate reduction, makes (NH
4)
2IrCl
6(IV) becomes (NH
4)
3IrCl
6(III), (NH
4)
3IrCl
6(III) is water-soluble very large, then adds ammonium sulfide precipitation (NH
4)
3IrCl
6Other high and low metal impurities in (III) solution filter, and add ammonium chloride to solution, add nitric acid oxidation, make (NH
4)
2IrCl
6(III) generates (NH
4)
2IrCl
6(IV) precipitation is filtered.So repeated multiple times, until obtain qualified (NH
4)
2IrCl
6(IV) precipitation, at last calcining, hydrogen reduction obtains qualified iridium powder.
The shortcoming of the precipitation method has: (1) adopts (NH
4)
2In the refining iridium process of S method, the base metal sulfide precipitation can be adsorbed a large amount of iridium, reduces the direct yield of iridium; (2) precipitation method employing reducing agent reduction iridium (IV) are in the process of iridium (III), and other platinum group metal impurity also is reduced to platinum (II), palladium (II), ruthenium (III), the rhodium (III) of lower valency, because (NH
4)
3IrCl
6(III) solution main body is iridium, and other platinum group metal impurity only has on a small quantity, (NH
4)
2S meeting preferential precipitation iridium, to other platinum group metal contamination precipitation weak effect, the rate of recovery of iridium is low; (3) because iridium powder product national standard is stricter, be difficult to obtain qualified iridium powder product by the precipitation method.Therefore the shortcoming number of occurrence of precipitation method separating-purifying iridium is many, process is tediously long, separate not thoroughly, the iridium rate of recovery is low, be difficult to obtain qualified iridium product.
Summary of the invention
Main purpose of the present invention provides a kind of method of iridium separating-purifying, realizes the high efficiente callback of iridium in the noble metal secondary resource waste material.Because similar chemical characteristic is so that the platinum group metal is separated from each other very difficultly, the difficult problem of the separating-purifying maximum of iridium is to remove other a small amount of platinum group metal impurity in the main body iridium solution.Because IrCl
6 2-Thermodynamic stability and kinetic inertness all be higher than other platinum group metal chlorine part, pass through controlled condition, under low acidity, can reduce with active metal aluminium that other platinum group metal is metallic state in the iridium solution, and iridium (IV) is reduced generation iridium (III), only have a small amount of iridium to be reduced into metal iridium, reach the purpose that iridium separates with other platinum group metal.
Embodiment of the present invention design as follows:
(1) transfer pH: keeping the mass concentration of the hydrochloric acid solution of iridium is 60～100 g/L, and the pH of regulator solution is 1 ~ 3;
(2) reduction: slowly adding granularity in the solution that mixes up pH is 60～100 orders, and purity is greater than 99.9% aluminium powder, and the mass ratio that adds iridium in aluminium powder and the solution is: m
Al: m
Ir=0.3 ~ 0.8:1; The reaction condition of aluminum reduction is: 80 ~ 95 ℃ of solution temperatures, mixing speed 80 ~ 300 r/min, 2 ~ 3 hours reaction time; Platinum in the solution, palladium, rhodium, ruthenium are reduced to metal, H
2IrCl
6(IV) is reduced and generates H
3IrCl
6(III), solution colour becomes light green by peony, and a small amount of iridium is reduced into metal iridium;
The chemical reaction that said process relates to:
H
2IrCl
6Solution and aluminium powder generation redox reaction are shown in 1. formula:
3H
2IrCl
6 + Al + 3HCl → 3H
3IrCl
6 + AlCl
3 ①
The platinum group metal represents with M, with aluminium powder generation displacement reaction shown in 2. formula:
3H
2MCl
6 + 4Al → 3M + 4AlCl
3 + 6HCl ②
Inactive base metal also is replaced as metal by aluminium, and the reaction of aluminium displacement base metal is shown in 3. formula:
3MCl
2 + 2Al → 3M + 2AlCl
3 ③
(3) filter: the solution cooled and filtered after will reducing, washing, filtrate is not for containing the iridium solution of other platinum group metal impurity, and filter residue is collected and is sorted out, the unified recovery;
(4) removal of impurities: the mass concentration of the iridium solution after will filtering remains 30 ~ 50 g/L, regulates pH=1 ~ 1.5, then carries out removal of impurities with cationic ion-exchange resin, repeatedly exchanges 2 ~ 4 times, and the base metal hydrated cation is substantially by resin adsorption;
Base metal chloride MCl in the chemical reaction process that said process relates to
2And MCl
3Expression, positive resin represents with R-H, cation exchange reaction is as 4. and 5. shown in the formula:
MCl
2 + R-H → R
2-M + 2HCl ④
MCl
3 + 3R-H → 3HCl + R
3-M ⑤
(5) concentrate drying: will by the iridium solution condensing crystallizing after the ion-exchange removal of impurities, then obtain IrCl 90 ~ 130 ℃ of oven dry
3Crystal;
(6) hydrogen reduction: the IrCl after will drying
3Crystal is put into also stove of hydrogen, and passing into needs to purge 0.5 ~ 2 h with nitrogen before the hydrogen, 650 ~ 850 ℃ of control reduction temperatures, and recovery time 1 ~ 3 h, logical hydrogen reduction obtains purity greater than 99.95% iridium powder.
The chemical reaction that said process relates to:
2IrCl
3 + 3H
2 → 2Ir + 6HCl ⑥
Above-mentioned, the solution of iridium described in the steps A is with H
2IrCl
6Be main body, contain a small amount of other platinum group metal and base metal impurity.
The mass concentration that should keep iridium described in the steps A is 60 ~ 100 g/L, the pH of regulator solution=1 ~ 3.
The purity that adds aluminium powder described in the step B is greater than 99.9%, and granularity is 60 ~ 100 orders, and the mass ratio of iridium is in aluminium powder and the solution: m
Al: m
Ir=0.3 ~ 0.8:1.
The reaction condition of aluminum reduction described in the step B is: 80 ~ 95 ℃ of solution temperatures, mixing speed 80 ~ 300 r/min, 2 ~ 3 hours reaction time.
There are platinum, palladium, rhodium, ruthenium in the platinum group metal that aluminium powder described in the step B can reduce, and the iridium of trace.
The used ion exchange resin of the removal of impurities of ion-exchange described in the step D is one or more in 001 * 1,001 * 2,001 * 3,001 * 4,001 * 7,002 * 7,003 * 7,004 * 7,001 * 8,001 * 14.5 strongly acidic styrene type cation exchange resin.
The mass concentration of the iridium solution among the step D before the removal of impurities should keep 30 ~ 50 g/L.
Bake out temperature described in the step e should remain on 90 ~ 130 ℃.
Hydrogen reduction condition described in the step F is: 650 ~ 850 ℃ of reduction temperatures, and recovery time 1 ~ 3 h, passing into hydrogen needs to purge 0.5 ~ 2 h with nitrogen before.
The present invention adopts aluminium reducing, ion-exchange removal of impurities that iridium solution is carried out separating-purifying, compared with prior art has the following advantages: the iridium powder purity that (1) hydrogen reduction obtains reaches more than 99.95%; (2) direct yield of iridium is reached more than 85%, the total recovery of iridium is greater than 97%; (3) the present invention is simple to operate, and practicality is easy to realize industrialization.
Description of drawings
Fig. 1 is process chart of the present invention.
The specific embodiment
The present invention is described in further detail and verifies its effect below in conjunction with the drawings and specific embodiments.
Embodiment one
Contain iridium solution 1000 ml, Ir 65.51 g/L, Ru 1.73 g/L, Cu 0.65 g/L, Fe 0.32 g/L, Pb 0.29 g/L, Al 1.82 g/L, transfer pH=1 with NaOH solution, then the solution that mixes up pH is put into the there-necked flask of 2000 ml, electric jacket is heated to 80 ℃, slowly adds while stirring 40 grams, 99.9%, 80 purpose aluminium powders, 2 hours reaction time, cooled and filtered, washing, filtrate is not for containing the iridium solution of ruthenium, the unified recovery after filter residue is collected.Iridium solution concentration after filtering is controlled at 40 g/L, and transfer pH=1.5, and repeatedly exchanging 3 times with 001 * 7 type cationic ion-exchange resin, the base metal hydrated cation is substantially by resin adsorption, to by the iridium solution condensing crystallizing after the ion-exchange removal of impurities, then obtain IrCl 120 ℃ of oven dry
3Crystal; With the IrCl after the oven dry
3Crystal is put into also stove of hydrogen, and 750 ℃ of logical hydrogen reductions obtained the 99.95% iridium powder of 57.46g in 2 hours, and the direct yield of iridium is 87.7%, and total recovery is greater than 97%.
Embodiment two
Contain iridium solution 1000 ml, Ir 77.47 g/L, Pt 0.83 g/L, Zn 0.48 g/L, Fe 0.55 g/L, Pb 0.35 g/L, Al 0.92 g/L, transfer pH=1.5 with NaOH solution, then the solution that mixes up pH is put into the there-necked flask of 2000 ml, electric jacket is heated to 90 ℃, slowly adds while stirring 46 grams, 99.9%, 80 purpose aluminium powders, 2 hours reaction time, cooled and filtered, washing, filtrate are the iridium solution of not platiniferous, the unified recovery after filter residue is collected.Iridium solution concentration after filtering is controlled at 40 g/L, and transfer pH=1.5, and repeatedly exchanging 4 times with 001 * 7 type cationic ion-exchange resin, the base metal hydrated cation is substantially by resin adsorption, to by the iridium solution condensing crystallizing after the ion-exchange removal of impurities, then obtain IrCl 120 ℃ of oven dry
3Crystal; With the IrCl after the oven dry
3Crystal is put into also stove of hydrogen, and 750 ℃ of logical hydrogen reductions obtained the 99.95% iridium powder of 68.41g in 3 hours, and the direct yield of iridium is 88.3%, and total recovery is greater than 97%.
Embodiment three
Contain iridium solution 1000 ml, Ir 64.45 g/L, Ru 1.07 g/L, Rh 0.49 g/L, Cu 0.68 g/L, Fe 0.59 g/L, Pb 0.55 g/L, Al 0.87 g/L, transfer pH=1 with NaOH solution, then the solution that mixes up pH is put into the there-necked flask of 2000 ml, electric jacket is heated to 90 ℃, slowly adds while stirring 38 grams, 99.9%, 80 purpose aluminium powders, 2 hours reaction time, cooled and filtered, washing, filtrate are the iridium solution of not rhodium-containing, ruthenium, the unified recovery after filter residue is collected.Iridium solution concentration after filtering is controlled at 40 g/L, and transfer pH=1.5, and repeatedly exchanging 4 times with 001 * 7 type cationic ion-exchange resin, the base metal hydrated cation is substantially by resin adsorption, to by the iridium solution condensing crystallizing after the ion-exchange removal of impurities, then obtain IrCl 120 ℃ of oven dry
3Crystal; With the IrCl after the oven dry
3Crystal is put into also stove of hydrogen, and 750 ℃ of logical hydrogen reductions obtained the 99.95% iridium powder of 56.01g in 2 hours, and the direct yield of iridium is 86.9%, and total recovery is greater than 97%.
Embodiment four
Contain iridium solution 1000 ml, Ir 82.47 g/L, Ru 1.84 g/L, Pt 0.69 g/L, Pd 1.72 g/L, Rh 0.52 g/L, Cu 0.47 g/L, Fe 0.83 g/L, Zn 0.19 g/L, Al 0.62 g/L, transfer pH=1.5 with NaOH solution, then the solution that mixes up pH is put into the there-necked flask of 2000 ml, electric jacket is heated to 85 ℃, slowly add while stirring 50 grams, 99.9%, 80 purpose aluminium powders, 3 hours reaction time, cooled and filtered, washing, filtrate is the iridium solution of not platiniferous, palladium, rhodium, ruthenium, the unified recovery after filter residue is collected.Iridium solution concentration after filtering is controlled at 40 g/L, and transfer pH=1.5, and repeatedly exchanging 4 times with 001 * 7 type cationic ion-exchange resin, the base metal hydrated cation is substantially by resin adsorption, to by the iridium solution condensing crystallizing after the ion-exchange removal of impurities, then obtain IrCl 120 ℃ of oven dry
3Crystal; With the IrCl after the oven dry
3Crystal is put into also stove of hydrogen, and 750 ℃ of logical hydrogen reductions obtained the 99.95% iridium powder of 72.17g in 3 hours, and the direct yield of iridium is 87.5%, and total recovery is greater than 97%.
Claims (9)
1. the method for a separating-purifying iridium is characterized in that carrying out successively as follows:
A, accent pH: the pH that will contain the hydrochloric acid solution of iridium is adjusted to 1 ~ 3;
B, reduction: in the solution that mixes up pH, slowly add aluminium powder, then H
2IrCl
6(IV) is reduced and generates H
3IrCl
6(III), solution colour becomes light green by peony, and a small amount of iridium is reduced into metal iridium;
C, filtration: the solution cooled and filtered after will reducing, washing, filtrate is not for containing the iridium solution of other platinum group metal impurity, and filter residue is collected and is sorted out, the unified recovery;
D, removal of impurities: it is 1 ~ 1.5 that the iridium solution after will filtering is regulated its pH, then carries out removal of impurities with cationic ion-exchange resin, repeatedly exchanges 2 ~ 4 times, and the base metal hydrated cation is substantially by resin adsorption;
E, concentrate drying: will be by the iridium solution condensing crystallizing after the ion-exchange removal of impurities, then oven dry obtains IrCl
3Crystal;
F, hydrogen reduction: the IrCl after will drying
3Crystal is put into also stove of hydrogen, and under 650 ~ 850 ℃, logical hydrogen reduction obtains purity greater than 99.95% iridium powder.
2. the method for separating-purifying iridium according to claim 1, the hydrochloric acid solution that it is characterized in that iridium described in the steps A is with H
2IrCl
6Be main body, contain a small amount of other platinum group metal and base metal impurity.
3. the method for separating-purifying iridium according to claim 1, it is characterized in that should keeping described in the steps A mass concentration of the hydrochloric acid solution of iridium is 60 ~ 100 g/L.
4. the method for separating-purifying iridium according to claim 1 is characterized in that the purity of the aluminium powder of adding described in the step B greater than 99.9%, and granularity is 60 ~ 100 orders, and the mass ratio of iridium is in aluminium powder and the solution: m
Al: m
Ir=0.3 ~ 0.8:1.
5. the method for separating-purifying iridium according to claim 1 is characterized in that the reaction condition of aluminum reduction described in the step B is: 80 ~ 95 ℃ of solution temperatures, mixing speed 80 ~ 300 r/min, 2 ~ 3 hours reaction time.
6. the method for separating-purifying iridium according to claim 1 is characterized in that the used ion exchange resin of ion-exchange removal of impurities described in the step D is one or more in 001 * 1,001 * 2,001 * 3,001 * 4,001 * 7,002 * 7,003 * 7,004 * 7,001 * 8,001 * 14.5 strongly acidic styrene type cation exchange resin.
7. the method for separating-purifying iridium according to claim 1 is characterized in that the mass concentration of the iridium solution before the removal of impurities among the step D should keep 30 ~ 50 g/L.
8. the method for separating-purifying iridium according to claim 1 is characterized in that the bake out temperature described in the step e should remain on 90 ~ 130 ℃.
9. the method for separating-purifying iridium according to claim 1, the hydrogen reduction condition described in the step F that it is characterized in that is: 650 ~ 850 ℃ of reduction temperatures, recovery time 1 ~ 3 h needs to purge 0.5 ~ 2 h with nitrogen before passing into hydrogen.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104259483A (en) * | 2014-09-12 | 2015-01-07 | 昆明贵金属研究所 | Method for recycling iridum-rhodium alloy waste material |
| CN106319240A (en) * | 2016-08-29 | 2017-01-11 | 金川集团股份有限公司 | Method for removing noble metal impurities from iridium-containing material liquid |
| CN108405881A (en) * | 2018-02-02 | 2018-08-17 | 贵研铂业股份有限公司 | A kind of preparation method of high pure spherical ruthenium powder |
| CN108421986A (en) * | 2018-05-17 | 2018-08-21 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity iridium powder |
| 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 |
| CN115536081A (en) * | 2022-11-04 | 2022-12-30 | 郴州高鑫材料有限公司 | Method for preparing chloroiridic acid from multi-platinum group metal material |
| CN115571931A (en) * | 2022-11-04 | 2023-01-06 | 郴州高鑫材料有限公司 | Method for preparing chloroiridic acid from pure iridium powder |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104259483A (en) * | 2014-09-12 | 2015-01-07 | 昆明贵金属研究所 | Method for recycling iridum-rhodium alloy waste material |
| CN106319240A (en) * | 2016-08-29 | 2017-01-11 | 金川集团股份有限公司 | Method for removing noble metal impurities from iridium-containing material liquid |
| CN106319240B (en) * | 2016-08-29 | 2018-04-10 | 金川集团股份有限公司 | The removal methods of precious metal impurity in a kind of feed liquid containing iridium |
| CN108405881A (en) * | 2018-02-02 | 2018-08-17 | 贵研铂业股份有限公司 | A kind of preparation method of high pure spherical ruthenium powder |
| CN108421986A (en) * | 2018-05-17 | 2018-08-21 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity iridium powder |
| CN108421986B (en) * | 2018-05-17 | 2021-06-08 | 贵研铂业股份有限公司 | Preparation method of high-purity iridium powder |
| 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 |
| CN115536081A (en) * | 2022-11-04 | 2022-12-30 | 郴州高鑫材料有限公司 | Method for preparing chloroiridic acid from multi-platinum group metal material |
| CN115571931A (en) * | 2022-11-04 | 2023-01-06 | 郴州高鑫材料有限公司 | Method for preparing chloroiridic acid from pure iridium powder |
| CN115536081B (en) * | 2022-11-04 | 2023-09-15 | 郴州高鑫材料有限公司 | Method for preparing chloroiridium acid from multiple platinum group metal materials |
| CN115571931B (en) * | 2022-11-04 | 2024-05-28 | 郴州高鑫材料有限公司 | Method for preparing chloroiridic acid from pure iridium powder |
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