CN103302298B - A kind of method of separating-purifying iridium - Google Patents
A kind of method of separating-purifying iridium Download PDFInfo
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- CN103302298B CN103302298B CN201310216080.XA CN201310216080A CN103302298B CN 103302298 B CN103302298 B CN 103302298B CN 201310216080 A CN201310216080 A CN 201310216080A CN 103302298 B CN103302298 B CN 103302298B
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Abstract
The present invention relates to iridium and the process for separation and purification between other platinum group metal and base metal in solution.Its concrete technology and reaction condition as follows: (1) adjusts pH: controlling the mass concentration of iridium is 60 ~ 100g/L, adjusts pH value of solution to be 1 ~ 3; (2) reduce: in the solution mixing up pH, slowly add aluminium powder; (3) filter: by the solution cooled and filtered after reduction, washing; (4) removal of impurities: the mass concentration of the iridium solution after filtration is remained 30 ~ 50g/L, regulate pH=1 ~ 1.5, then repeatedly exchange 2 ~ 4 removal of impurities with cationic ion-exchange resin, base metal is substantially by resin adsorption; (5) concentrate drying obtains IrCl
3crystal; (6) hydrogen reduction: by the IrCl after oven dry
3crystal put into hydrogen also stove reduction obtain the iridium powder that purity is greater than 99.95%.The present invention adopts aluminium reducing, ion-exchange removal of impurities carries out separating-purifying to iridium solution, compared with prior art has the following advantages: the iridium powder purity that (1) hydrogen reduction obtains reaches more than 99.95%; (2) make the direct yield of iridium reach more than 85%, the total recovery of iridium is greater than 97%; (3) the present invention is simple to operate, practical, is easy to realize industrialization.
Description
Technical field
The present invention relates to iridium and the separation method between other platinum group metal and base metal, especially from separating-purifying iridium the noble metal secondary resource waste containing iridium.
Background technology
It is very difficult that platinum group metal has similar chemical characteristic that platinum group metal is separated from each other, and wherein the separating-purifying of iridium is especially difficult.Hydrogen reduction method and precipitation method for refining is had from containing the common method of separating-purifying iridium the hydrochloric acid solution of iridium.
Hydrogen reduction method separating-purifying iridium is divided into pressurization and non-pressure process.Patent CN87104181.2 is from containing separating-purifying iridium the iridium solution of expensive, base-metal ion: the precious metal impurity in first step pressurized hydrogen Reduced separating iridium, then by method removing base metals such as ion-exchanges; The reduction of second step pressurized hydrogen obtains the pure iridium powder that purity is greater than 99.9%, the rate of recovery >99% of iridium; Patent CN1626690 is under normal pressure and certain temperature, and adopt hydrogen reduction method, from pure iridium rhodium solution, rhodium is reduced into metal, iridium is not reduced, the purity >99.99% of iridium after separate rhodium.At present, hydrogen reduction method does not realize industrial applications.
It is classical iridium method of refining that chloride precipitation-ammonium sulfide is refined, and patent CN201010567367.3 adopts precipitate and separate purifying iridium, the steps include: that (1) will containing iridium material dissolving with hydrochloric acid; (2) nitric acid and NH is added
4cl is obtained by reacting iridium platinum mixed-ammonium salt; (3) adding hydrazine hydrate makes platinum reduction separate out black sponge platinum powder and iridium, iron tramp precipitation; (4) H is added
2o
2destroy hydrazine hydrate, add (NH
4)
2s purifies; (5) Nitric Acid Oxidation and NH is added
4cl precipitation makes iridium generate (NH
4)
2irCl
6(IV), then add water pulp, adds hydrazine hydrate reduction, make (NH
4)
2irCl
6(IV) (NH is become
4)
3irCl
6(III), (NH
4)
3irCl
6(III) water-soluble very large, then add ammonium sulfide precipitation (NH
4)
3irCl
6(III) other high and low metal impurities in solution, filter, add ammonium chloride, add nitric acid oxidation, make (NH to solution
4)
2irCl
6(III) (NH is generated
4)
2irCl
6(IV) precipitate, filter.So repeated multiple times, until obtain qualified (NH
4)
2irCl
6(IV) precipitate, finally calcining, hydrogen reduction obtains qualified iridium powder.
The shortcoming of the precipitation method has: (1) adopts (NH
4)
2s method is refined in iridium process, and base metal sulfide precipitation can adsorb a large amount of iridium, reduces the direct yield of iridium; (2) precipitation method adopt in the process of reducing agent reduction iridium (IV) for iridium (III), and other platinum group metal impurity is also reduced to platinum (II), palladium (II), ruthenium (III), the rhodium (III) of lower valency, due to (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 more strict, be difficult to obtain qualified iridium powder product by the precipitation method.Therefore many, the process tedious of the shortcoming number of occurrence of precipitation method separating-purifying iridium, separation are 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 is to provide a kind of method of iridium separating-purifying, realizes the high efficiente callback of iridium in noble metal secondary resource waste.Due to similar chemical characteristic, that platinum group metal is separated from each other is very difficult, and the difficult problem that the separating-purifying of iridium is maximum removes other a small amount of platinum group metal impurity in main body iridium solution.Due to IrCl
6 2-thermodynamic stability and kinetic inertness all higher than other platinum group metal chlorine part, pass through controlled condition, under Low acid, can reduce other platinum group metal in iridium solution with active metal aluminium is metallic state, and iridium (IV) is reduced generation iridium (III), only have a small amount of iridium to be reduced into metal iridium, reach the object that iridium is separated with other platinum group metal.
Embodiment of the present invention design as follows:
(1) adjust pH: the mass concentration keeping the hydrochloric acid solution of iridium is 60 ~ 100g/L, the pH regulating solution is 1 ~ 3;
(2) reduce: in the solution mixing up pH, slowly add granularity is 60 ~ 100 orders, and the aluminium powder that purity is greater than 99.9%, the mass ratio adding iridium in aluminium powder and solution is: m
al: m
ir=0.3 ~ 0.8:1; The reaction condition of aluminum reduction is: solution temperature 80 ~ 95 DEG C, mixing speed 80 ~ 300r/min, 2 ~ 3 hours reaction time; Platinum in solution, palladium, rhodium, ruthenium are reduced to metal, H
2irCl
6(IV) generation H is reduced
3irCl
6(III), solution colour becomes light green from 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 as shown in 1. formula:
3H
2IrCl
6+Al+3HCl→3H
3IrCl
6+AlCl
3①
Platinum group metal represents with M, with aluminium powder generation displacement reaction as shown in 2. formula:
3H
2MCl
6+4Al→3M+4AlCl
3+6HCl②
Inactive base metal is also replaced as metal by aluminium, and the reaction of aluminium displacement base metal is as shown in 3. formula:
3MCl
2+2Al→3M+2AlCl
3③
(3) filter: by the solution cooled and filtered after reduction, washing, filtrate is not containing the iridium solution of other platinum group metal impurity, and residue collection is sorted out, and unification is reclaimed;
(4) removal of impurities: the mass concentration of the iridium solution after filtration is remained 30 ~ 50g/L, regulate pH=1 ~ 1.5, then carry out removal of impurities with cationic ion-exchange resin, repeatedly exchange 2 ~ 4 times, 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
3represent, positive resin R-H represents, cation exchange reaction is as 4. and 5. shown in formula:
MCl
2+R-H→R
2-M+2HCl④
MCl
3+3R-H→3HCl+R
3-M⑤
(5) concentrate drying: by by the iridium solution condensing crystallizing after ion-exchange removal of impurities, then obtain IrCl 90 ~ 130 DEG C of oven dry
3crystal;
(6) hydrogen reduction: by the IrCl after oven dry
3crystal puts into hydrogen also stove, needs to carry out purging 0.5 ~ 2h with nitrogen before passing into hydrogen, and control reduction temperature 650 ~ 850 DEG C, recovery time 1 ~ 3h, logical hydrogen reduction obtains the iridium powder that purity is greater than 99.95%.
The chemical reaction that said process relates to:
2IrCl
3+3H
2→2Ir+6HCl⑥
Above-mentioned, the solution of iridium described in steps A is with H
2irCl
6for main body, containing other platinum group metal a small amount of and base metal impurity.
The mass concentration of iridium should be kept described in steps A to be 60 ~ 100g/L, to regulate pH=1 ~ 3 of solution.
The purity adding aluminium powder described in step B is greater than 99.9%, and granularity is 60 ~ 100 orders, and in aluminium powder and solution, the mass ratio of iridium is: m
al: m
ir=0.3 ~ 0.8:1.
The reaction condition of aluminum reduction described in step B is: solution temperature 80 ~ 95 DEG C, mixing speed 80 ~ 300r/min, 2 ~ 3 hours reaction time.
There are platinum, palladium, rhodium, ruthenium in the platinum group metal that aluminium powder described in step B can reduce, and the iridium of trace.
The removal of impurities of ion-exchange described in step D ion exchange resin used 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 in step D before removal of impurities should keep 30 ~ 50g/L.
Bake out temperature described in step e should remain on 90 ~ 130 DEG C.
Hydrogen reduction condition described in step F is: reduction temperature 650 ~ 850 DEG C, recovery time 1 ~ 3h, needs to carry out purging 0.5 ~ 2h with nitrogen before passing into hydrogen.
The present invention adopts aluminium reducing, ion-exchange removal of impurities carries out separating-purifying to iridium solution, compared with prior art has the following advantages: the iridium powder purity that (1) hydrogen reduction obtains reaches more than 99.95%; (2) make the direct yield of iridium reach more than 85%, the total recovery of iridium is greater than 97%; (3) the present invention is simple to operate, practical, is easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments the present invention be described in further detail and verify its effect.
embodiment one
Containing iridium solution 1000ml, Ir65.51g/L, Ru1.73g/L, Cu0.65g/L, Fe0.32g/L, Pb0.29g/L, Al1.82g/L, pH=1 is adjusted by NaOH solution, then the solution mixing up pH is put into the there-necked flask of 2000ml, electric jacket is heated to 80 DEG C, slowly adds 40 gram 99.9%, 80 object aluminium powders while stirring, 2 hours reaction time, cooled and filtered, washing, filtrate is not containing the iridium solution of ruthenium, unified recovery after residue collection.Iridium solution concentration after filtering is controlled at 40g/L, and adjust pH=1.5, repeatedly exchange 3 times with 001 × 7 type cationic ion-exchange resin, base metal hydrated cation is substantially by resin adsorption, by by the iridium solution condensing crystallizing after ion-exchange removal of impurities, then obtain IrCl 120 DEG C of oven dry
3crystal; By the IrCl after oven dry
3crystal puts into hydrogen also stove, and 750 DEG C of logical hydrogen reductions obtain the 99.95% iridium powder of 57.46g for 2 hours, and the direct yield of iridium is 87.7%, and total recovery is greater than 97%.
embodiment two
Containing iridium solution 1000ml, Ir77.47g/L, Pt0.83g/L, Zn0.48g/L, Fe0.55g/L, Pb0.35g/L, Al0.92g/L, pH=1.5 is adjusted by NaOH solution, then the solution mixing up pH is put into the there-necked flask of 2000ml, electric jacket is heated to 90 DEG C, slowly adds 46 gram 99.9%, 80 object aluminium powders while stirring, 2 hours reaction time, cooled and filtered, washing, filtrate is the iridium solution of not platiniferous, unified recovery after residue collection.Iridium solution concentration after filtering is controlled at 40g/L, and adjust pH=1.5, repeatedly exchange 4 times with 001 × 7 type cationic ion-exchange resin, base metal hydrated cation is substantially by resin adsorption, by by the iridium solution condensing crystallizing after ion-exchange removal of impurities, then obtain IrCl 120 DEG C of oven dry
3crystal; By the IrCl after oven dry
3crystal puts into hydrogen also stove, and 750 DEG C of logical hydrogen reductions obtain the 99.95% iridium powder of 68.41g for 3 hours, and the direct yield of iridium is 88.3%, and total recovery is greater than 97%.
embodiment three
Containing iridium solution 1000ml, Ir64.45g/L, Ru1.07g/L, Rh0.49g/L, Cu0.68g/L, Fe0.59g/L, Pb0.55g/L, Al0.87g/L, pH=1 is adjusted by NaOH solution, then the solution mixing up pH is put into the there-necked flask of 2000ml, electric jacket is heated to 90 DEG C, slowly adds 38 gram 99.9%, 80 object aluminium powders while stirring, 2 hours reaction time, cooled and filtered, washing, filtrate is the iridium solution of not rhodium-containing, ruthenium, unified recovery after residue collection.Iridium solution concentration after filtering is controlled at 40g/L, and adjust pH=1.5, repeatedly exchange 4 times with 001 × 7 type cationic ion-exchange resin, base metal hydrated cation is substantially by resin adsorption, by by the iridium solution condensing crystallizing after ion-exchange removal of impurities, then obtain IrCl 120 DEG C of oven dry
3crystal; By the IrCl after oven dry
3crystal puts into hydrogen also stove, and 750 DEG C of logical hydrogen reductions obtain the 99.95% iridium powder of 56.01g for 2 hours, and the direct yield of iridium is 86.9%, and total recovery is greater than 97%.
embodiment four
Containing iridium solution 1000ml, Ir82.47g/L, Ru1.84g/L, Pt0.69g/L, Pd1.72g/L, Rh0.52g/L, Cu0.47g/L, Fe0.83g/L, Zn0.19g/L, Al0.62g/L, pH=1.5 is adjusted by NaOH solution, then the solution mixing up pH is put into the there-necked flask of 2000ml, electric jacket is heated to 85 DEG C, slowly add 50 gram 99.9%, 80 object aluminium powders while stirring, 3 hours reaction time, cooled and filtered, washing, filtrate is the iridium solution of not platiniferous, palladium, rhodium, ruthenium, unified recovery after residue collection.Iridium solution concentration after filtering is controlled at 40g/L, and adjust pH=1.5, repeatedly exchange 4 times with 001 × 7 type cationic ion-exchange resin, base metal hydrated cation is substantially by resin adsorption, by by the iridium solution condensing crystallizing after ion-exchange removal of impurities, then obtain IrCl 120 DEG C of oven dry
3crystal; By the IrCl after oven dry
3crystal puts into hydrogen also stove, and 750 DEG C of logical hydrogen reductions obtain the 99.95% iridium powder of 72.17g for 3 hours, and the direct yield of iridium is 87.5%, and total recovery is greater than 97%.
Claims (1)
1. a method for separating-purifying iridium, is characterized in that carrying out successively as follows:
A, tune pH: the pH of the hydrochloric acid solution containing iridium is adjusted to 1 ~ 3;
B, reduction: in the solution mixing up pH, slowly add aluminium powder, then H
2irCl
6(IV) generation H is reduced
3irCl
6(III), solution colour becomes light green from peony, and a small amount of iridium is reduced into metal iridium;
C, filtration: by the solution cooled and filtered after reduction, washing, filtrate is not containing the iridium solution of other platinum group metal impurity, and residue collection is sorted out, unified recovery;
D, removal of impurities: regulate its pH to be 1 ~ 1.5 the iridium solution after filtering, then carry out removal of impurities with cationic ion-exchange resin, repeatedly exchange 2 ~ 4 times, base metal hydrated cation is substantially by resin adsorption;
E, concentrate drying: by by the iridium solution condensing crystallizing after ion-exchange removal of impurities, then dry and obtain IrCl
3crystal;
F, hydrogen reduction: by the IrCl after oven dry
3crystal puts into hydrogen also stove, and at 650 ~ 850 DEG C, logical hydrogen reduction obtains the iridium powder that purity is greater than 99.95%,
The hydrochloric acid solution of iridium described in steps A is with H
2irCl
6for main body, containing other platinum group metal a small amount of and base metal impurity,
The mass concentration of the hydrochloric acid solution of iridium described in steps A is 60 ~ 100g/L,
The purity adding aluminium powder described in step B is greater than 99.9%, and granularity is 60 ~ 100 orders, and in aluminium powder and solution, the mass ratio of iridium is: m
al: m
ir=0.3 ~ 0.8:1,
The reaction condition of aluminum reduction described in step B is: solution temperature 80 ~ 95 DEG C, mixing speed 80 ~ 300r/min, 2 ~ 3 hours reaction time,
The removal of impurities of ion-exchange described in step D ion exchange resin used 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 in step D before removal of impurities should keep 30 ~ 50g/L,
Bake out temperature described in step e should remain on 90 ~ 130 DEG C,
Hydrogen reduction condition described in step F is: reduction temperature 650 ~ 850 DEG C, recovery time 1 ~ 3h, needs to carry out purging 0.5 ~ 2h with nitrogen before passing into hydrogen.
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Families Citing this family (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 |
| 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 |
| 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 |
| 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 |
| 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 |
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