CN115011807B - Purification method for efficiently separating rhodium iridium with high yield - Google Patents
Purification method for efficiently separating rhodium iridium with high yield Download PDFInfo
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- 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
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- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention belongs to the technical field of precious metal separation and purification, and particularly relates to a purification method for efficiently separating rhodium iridium with high yield. According to the method, the pH value of the solution to be purified containing the impurity iridium is adjusted by adding the alkaline solution, the precipitant is added at a proper temperature, the precipitate is filtered to obtain the rhodium complex precipitate without the impurity iridium, the precipitate is reduced by adding the sodium hydroxide solution to obtain rhodium black, and the rhodium black is calcined through introducing hydrogen to obtain the high-purity rhodium powder.
Description
Technical Field
The invention belongs to the technical field of precious metal separation and purification, and particularly relates to a purification method for efficiently separating rhodium iridium with high yield.
Background
In the separation and purification of noble metal rhodium, the chemical properties of impurity iridium and rhodium are similar, so that the impurity iridium element cannot be effectively removed by utilizing the conventional wet chemical purification methods such as a sodium nitrite mixing method, a vulcanization precipitation method, an ammonia mixing method, an extraction method and the like. At present, rhodium iridium separation generally adopts an ammonium sulfite precipitation method, and the method can separate and purify rhodium and iridium, but the separation and purification process has complicated steps and serious three-waste pollution, such as sodium nitrite precipitation, ammonium sulfite precipitation, hydrochloric acid dissolution, heating reduction, filtrate reprecipitation, hydrochloric acid redissolution and the like. Particularly, when rhodium contains iridium impurity elements with high content (Ir is more than 5%), the impurity iridium is difficult to separate, and the ammonium sulfite method needs repeated purification for more than three times, so that the purification efficiency and recovery rate of rhodium are greatly reduced.
Based on the background, the rhodium-iridium separation and purification process is improved, and the development of a purification method for separating rhodium-iridium with high efficiency and high yield is particularly important.
Disclosure of Invention
Aiming at the technical problems of complicated rhodium-iridium separation process, low yield efficiency and serious three-waste pollution, the invention provides a purification method for efficiently separating rhodium-iridium with high yield. The method realizes the high-efficiency and rapid separation of rhodium and iridium elements, has simple process and convenient operation, ensures the purity of rhodium powder after rhodium and iridium separation, ensures the minimum content of impurity iridium elements to be 0.0005%, ensures the purity of rhodium powder, and simultaneously greatly improves the efficiency and yield of rhodium and iridium separation and purification.
In order to achieve the technical purpose, the technical scheme adopted by the embodiment of the invention is as follows:
a purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
s1, adding a certain amount of alkaline solution into to-be-purified solution containing iridium impurity to adjust the pH value of the to-be-purified solution to be more than or equal to 0.5;
s2, heating the solution in a graphite furnace at 50-100 ℃, adding a precipitant into the solution to be purified, and reacting for 5-90 min until yellow precipitate is not separated out;
s3, filtering and precipitating to remove iridium impurities to obtain a rhodium complex yellow filter cake, and washing the filter cake;
s4, placing the filter cake in pure water, stirring, heating to 50-90 ℃, adjusting the pH of the solution to 10-14, and reducing to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and at 700 o And C, introducing hydrogen and reducing for 1-3h to obtain high-purity rhodium powder, wherein the mass content of iridium impurities is less than 0.01%.
Further, the solution to be purified containing iridium impurities in the step S1 is a chlororhodium acid solution, and the mass fraction of the iridium impurities in the solution to be purified is 0.1% -20%.
Further, the solute in the alkaline solution is one or two of ammonia water, potassium hydroxide, sodium carbonate and sodium bicarbonate, and the pH value of the solution to be purified is regulated to be 0.5-12 by utilizing the alkaline solution.
Further, in the step S2, the precipitant is one or more of hydrazine hydrochloride, hydrazine hydrate, hydrazine sulfate, sodium borohydride and formic acid, and the mass ratio of the precipitant to rhodium is 2-10:1.
further, in step S3, the filter cake is washed with a sodium chloride solution until the washing filtrate is colorless.
Further, the volume of the pure water in the step S4 is 1-5 times of the volume of the filter cake.
Further, in the step S5, the mass content of iridium impurity in the high-purity rhodium powder is 0.0005% -0.01%.
Compared with the prior art, the technical scheme of the embodiment of the invention has the following advantages:
according to the method, the pH value of the iridium-containing solution to be purified is adjusted by adding an alkaline solution into the iridium-containing solution to be purified, a precipitator is added at a proper temperature, rhodium complex precipitate of iridium without impurities is obtained through filtration, the precipitate is reduced by adding a sodium hydroxide solution to obtain rhodium black, and high-purity rhodium powder is obtained after hydrogen-introducing calcination, so that the problems of incomplete removal of iridium elements, complicated purification procedures, low purification efficiency, low yield, serious three-waste pollution and the like in the rhodium purification process in the prior art can be solved.
The method can realize the efficient and rapid separation of rhodium and iridium elements, has simple process and convenient operation, and the mass content of the impurity iridium elements after rhodium purification can reach 0.0005% at the minimum.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in further detail with reference to specific embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
step S1, adding a certain amount of potassium hydroxide into a solution to be purified (100 g containing noble metal rhodium) of chlororhodium containing 0.5% of iridium impurities by mass to adjust the pH of the solution to 1.5;
step S2, placing the solution on a graphite furnace, heating to 60 ℃, adding 300g of hydrazine hydrate into the solution to be purified, and reacting for 8min, wherein yellow precipitate is not separated out any more;
step S3, filtering the yellow precipitate to obtain a yellow rhodium complex filter cake without impurity iridium, and washing the filter cake with a sodium chloride solution until the washing filtrate is colorless;
step S4, placing the filter cake in a beaker, adding pure water with the volume 1 time of the volume of the filter cake, stirring by using a tetrafluoroethylene plastic rod, placing the stirred mixture in a graphite furnace with the set temperature of 90 ℃ for heating, then slowly adding sodium hydroxide solution to adjust the pH value of the solution to be 14, reducing until no obvious bubbles are generated, and carrying out solid-liquid separation to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and setting the heating temperature to be 700 DEG C o C, introducing hydrogen and reducing for 3 hours to obtain high-purity rhodium powder, wherein the content of iridium impurities is 0.0008%.
Example 2
A purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
step S1, adding a certain amount of ammonia water into a solution to be purified (300 g containing noble metal rhodium) of chlororhodium containing 15% of iridium impurities by mass fraction to adjust the pH value of the solution to 6;
step S2, placing the solution into a graphite furnace with the set temperature of 90 ℃ for heating, adding 1000g of hydrazine hydrochloride into the solution to be purified, and reacting for 30min, wherein yellow precipitate is not separated out any more;
step S3, filtering the yellow precipitate to obtain a yellow rhodium complex filter cake without impurity iridium, and washing the filter cake with a sodium chloride solution until the washing filtrate is colorless;
step S4, placing the filter cake in a beaker, adding pure water with the volume being 5 times of the volume of the filter cake, stirring by using a tetrafluoroethylene plastic rod, placing the stirred mixture on a graphite furnace for heating at 80 ℃, then slowly adding sodium hydroxide solution to adjust the pH value of the solution to be 12, reducing until no obvious bubbles are generated, and carrying out solid-liquid separation to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and setting the heating temperature to be 700 DEG C o And C, introducing hydrogen and reducing for 3 hours to obtain high-purity rhodium powder, wherein the content of iridium impurities is 0.0005%.
Example 3
A purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
step S1, adding a certain amount of potassium hydroxide into a solution to be purified (100 g containing noble metal rhodium) of chlororhodium containing 0.1% of iridium impurities by mass fraction to adjust the pH of the solution to 3;
step S2, placing the solution on a graphite furnace, heating to 50 ℃, adding 300g of hydrazine hydrate into the solution to be purified, and reacting for 50min, wherein yellow precipitate is not separated out any more;
step S3, filtering the yellow precipitate to obtain a yellow rhodium complex filter cake without impurity iridium, and washing the filter cake with a sodium chloride solution until the washing filtrate is colorless;
step S4, placing the filter cake in a beaker, adding pure water with the volume being 2 times of the volume of the filter cake, stirring by using a tetrafluoroethylene plastic rod, placing the stirred mixture in a graphite furnace with the set temperature of 70 ℃ for heating, then slowly adding sodium hydroxide solution to adjust the pH value of the solution to be 10, reducing until no obvious bubbles are generated, and carrying out solid-liquid separation to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and setting the heating temperature to be 700 DEG C o C, introducing hydrogen and reducing for 1h to obtain high-purity rhodium powder, wherein the content of iridium impurities is 0.0008%.
Example 4
A purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
step S1, adding a certain amount of potassium hydroxide into a solution to be purified (100 g containing noble metal rhodium) of chlororhodium containing 20% of iridium impurities by mass fraction to adjust the pH of the solution to 2;
step S2, placing the solution on a graphite furnace, heating to 70 ℃, adding 300g of hydrazine hydrate into the solution to be purified, and reacting for 60min, wherein yellow precipitate is not separated out any more;
step S3, filtering the yellow precipitate to obtain a yellow rhodium complex filter cake without impurity iridium, and washing the filter cake with a sodium chloride solution until the washing filtrate is colorless;
step S4, placing the filter cake in a beaker, adding pure water with the volume being 3 times of the volume of the filter cake, stirring by using a tetrafluoroethylene plastic rod, placing the stirred mixture in a graphite furnace with the set temperature of 60 ℃ for heating, then slowly adding sodium hydroxide solution to adjust the pH value of the solution to be 13, reducing until no obvious bubbles are generated, and carrying out solid-liquid separation to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and setting the heating temperature to be 700 DEG C o C, introducing hydrogen and reducing for 3 hours to obtain high-purity rhodium powder, wherein the content of iridium impurities is 0.01%.
Example 5
A purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
step S1, adding a certain amount of potassium hydroxide into a solution to be purified (100 g containing noble metal rhodium) of chlororhodium containing 15% of iridium impurities by mass fraction to adjust the pH of the solution to 7;
step S2, placing the solution on a graphite furnace, heating to 80 ℃, adding 300g of hydrazine hydrate into the solution to be purified, and reacting for 90min, wherein yellow precipitate is not separated out any more;
step S3, filtering the yellow precipitate to obtain a yellow rhodium complex filter cake without impurity iridium, and washing the filter cake with a sodium chloride solution until the washing filtrate is colorless;
step S4, placing the filter cake in a beaker, adding pure water with the volume 4 times of the volume of the filter cake, stirring by using a tetrafluoroethylene plastic rod, placing the stirred mixture in a graphite furnace with the set temperature of 90 ℃ for heating, then slowly adding sodium hydroxide solution to adjust the pH value of the solution to be 11, reducing until no obvious bubbles are generated, and carrying out solid-liquid separation to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and setting the heating temperature to be 700 DEG C o And C, introducing hydrogen and reducing for 3 hours to obtain high-purity rhodium powder, wherein the content of iridium impurities is 0.0006%.
Example 6
A purification method for efficiently separating rhodium iridium with high yield comprises the following steps:
step S1, adding a certain amount of potassium hydroxide into a solution to be purified (100 g containing noble metal rhodium) of chlororhodium containing 10% of iridium impurities by mass fraction to adjust the pH of the solution to 8;
step S2, placing the solution on a graphite furnace, heating to 75 ℃, adding 300g of hydrazine hydrate into the solution to be purified, and reacting for 45min, wherein yellow precipitate is not separated out;
step S3, filtering the yellow precipitate to obtain a yellow rhodium complex filter cake without impurity iridium, and washing the filter cake with a sodium chloride solution until the washing filtrate is colorless;
step S4, placing the filter cake in a beaker, adding pure water with the volume being 2.5 times of the volume of the filter cake, stirring by using a tetrafluoroethylene plastic rod, heating in a graphite furnace with the set temperature of 70 ℃ after stirring uniformly, then slowly adding a sodium hydroxide solution to adjust the pH value of the solution to be 12, reducing until no obvious bubbles are generated, and carrying out solid-liquid separation to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, and setting the heating temperature to be 700 DEG C o And C, introducing hydrogen and reducing for 2 hours to obtain high-purity rhodium powder, wherein the content of iridium impurities is 0.001%.
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. The purification method for efficiently separating rhodium iridium with high yield is characterized by comprising the following steps:
s1, adding an alkaline solution into a solution to be purified containing iridium impurity to adjust the pH value of the solution to be purified to be more than or equal to 0.5;
s2, heating the solution in a graphite furnace at 50-100 ℃, adding a precipitant into the solution to be purified, and reacting for 5-90 min until yellow precipitate is not separated out;
s3, filtering and precipitating to remove iridium impurities to obtain a rhodium complex yellow filter cake, and washing the filter cake;
s4, placing the filter cake in pure water, stirring, heating to 50-90 ℃, adjusting the pH of the solution to 10-14, and reducing to obtain high-purity rhodium black;
s5, placing rhodium black in a hydrogen introducing furnace, introducing hydrogen at 700 ℃ for reduction for 1-3 hours to obtain high-purity rhodium powder, wherein the mass content of iridium impurities is less than 0.01%;
the solution to be purified containing iridium impurities in the step S1 is a chlororhodium acid solution, and the mass fraction of the iridium impurities in the solution to be purified is 0.1% -20%;
in the step S2, the precipitant is one or more of hydrazine hydrochloride, hydrazine hydrate, hydrazine sulfate, sodium borohydride and formic acid, and the mass ratio of the precipitant to rhodium is 2-10:1.
2. the purification method for efficiently separating rhodium iridium with high yield according to claim 1, wherein:
the solute in the alkaline solution is one or two of ammonia water, potassium hydroxide, sodium carbonate and sodium bicarbonate, and the pH value of the solution to be purified is regulated to be 0.5-12 by using the alkaline solution.
3. The purification method for efficiently separating rhodium iridium with high yield according to claim 1, wherein:
in the step S3, the filter cake is washed by adopting sodium chloride solution until the washing filtrate is colorless.
4. The purification method for efficiently separating rhodium iridium with high yield according to claim 1, wherein:
the volume of the pure water in the step S4 is 1-5 times of the volume of the filter cake.
5. The purification method for efficiently separating rhodium iridium with high yield according to claim 1, wherein:
in the step S5, the mass content of the impurity iridium in the high-purity rhodium powder is 0.0005% -0.01%.
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