CN110218867B - Method for separating rhodium and ruthenium from noble metal mixed liquor - Google Patents
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Abstract
The invention discloses a method for separating rhodium and ruthenium from a noble metal mixed solution, which comprises the following steps: dissolving waste materials containing rhodium and ruthenium in aqua regia to prepare mixed solution containing rhodium and ruthenium, adding a rhodium precipitation agent, stirring, precipitating, filtering, and collecting precipitate and precipitate tail liquid; dissolving the precipitate with aqua regia, and adding analytically pure hydrochloric acid for denitration treatment to obtain denitration mixed solution containing rhodium and ruthenium; adding a rhodium precipitation agent into the denitration mixed solution containing rhodium and ruthenium, stirring and precipitating, then filtering, and collecting precipitate and precipitate tail liquid; dissolving the precipitate with aqua regia, adding analytically pure hydrochloric acid, performing denitration treatment to obtain a secondary denitration rhodium-and ruthenium-containing liquid, adding a rhodium precipitation agent, precipitating, collecting precipitate, recovering rhodium, collecting the precipitate, adding zinc powder, and reducing and recovering ruthenium. The method is simple to operate and low in cost.
Description
The technical field is as follows:
the invention relates to the field of precious metal separation, in particular to a method for separating rhodium and ruthenium from a precious metal mixed solution.
Background art:
platinum group metals have excellent physicochemical properties, are important raw materials for modern industrial development, and are widely applied to the fields of aerospace materials, microelectronics, automobile manufacturing, catalysis, electrochemistry and the like. However, the reserves of the platinum group metals are limited, and how to obtain the platinum group metals from smelting byproducts in colleges and universities and how to recover the platinum group metals from industrial waste materials are important issues concerning the development of industrialization. Among them, rhodium and ruthenium are important platinum group metals, and it is also very important to separate rhodium and ruthenium in a noble metal mixed solution.
Rhodium is hard and is not corroded by acid, can be used for preparing catalysts, thermocouples, platinum-rhodium alloys and the like, is also commonly plated on searchlights and reflectors, and can also be used as a bright and hard coating film of other metals. In addition, it is used as a polishing machine for gemstones and as an electrical contact element. Ruthenium is a hard, brittle, light gray polyvalent rare metal element that is an excellent catalyst for hydrogenation, isomerization, oxidation, and reforming reactions. Pure metallic ruthenium is of little use. It is an effective hardener for platinum and palladium. It is used to make electric contact alloy and hard-grinding hard alloy. Therefore, it is critical to separate and extract rhodium and ruthenium metals with high efficiency.
At present, the extraction of noble metal rhodium generally adopts a medium-temperature chlorination method and a sodium bisulfate melting method, a sodium nitrite complexing method or an extraction method. The patent with the application number of 201310004627.X discloses a method for efficiently separating and purifying rhodium and ruthenium, which sequentially comprises pretreatment of rhodium and ruthenium alloy waste, moderate-temperature chlorination, separation of rhodium and ruthenium and refining of rhodium and ruthenium.
The invention content is as follows:
the invention aims to solve the technical problems of high energy consumption, secondary pollution to the environment and complex process in the prior art, and provides a method for separating rhodium and ruthenium from a noble metal mixed solution.
In order to better solve the technical problems, the invention adopts the following technical scheme:
a method for separating rhodium and ruthenium from a noble metal mixed solution comprises the following steps:
(1) adding the noble metal mixed solution into a PP (polypropylene) barrel, adding a rhodium precipitation agent, stirring and precipitating for 30min, standing for 1h, collecting precipitate, washing, placing in a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to obtain a denitrated mixed solution containing rhodium and ruthenium;
(2) adding the denitrated mixed solution containing rhodium and ruthenium obtained in the step (1) into a PP (polypropylene) barrel, continuously adding a rhodium precipitation agent, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentration of Rh and Ru in the precipitation tail solution by adopting an ICP (inductively coupled plasma) technology;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia for dissolution, cooling to room temperature after complete dissolution to obtain rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the rhodium-ruthenium-containing liquid;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation agent for stirring and precipitation, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), then adding zinc powder, stirring and reducing, and collecting ruthenium.
Preferably, in the above-mentioned technical means, the noble metal mixed solution is prepared by dissolving a rhodium-and ruthenium-containing solid with aqua regia.
Preferably, in the step (1), the mixed solution of noble metals has an Rh content of 8.3g/L and an Ru content of 0.103 g/L. The Rh content in the precipitation tail liquid after the rhodium precipitation agent is added for precipitation is 0.025g/L, and the ruthenium content is 0.083 g/L.
Preferably, the mass concentration of the rhodium deposition agent is 50%, and during the precipitation, 500-550ml of rhodium deposition agent is added into 1kg of rhodium, and more preferably 500ml of rhodium deposition agent is added into 1kg of rhodium.
Preferably, the concentrations of Rh and Ru in the precipitation tail liquid in the step (2) are 0.021g/L and 0.011g/L respectively.
Preferably, in the above technical solution, the concentrations of Rh and Ru in the rhodium-and ruthenium-containing liquid after the secondary denitration are respectively: 21.3g/L and 0.001 g/L.
Preferably, in the step (4), the adding amount of the zinc powder is five times of the ruthenium content in the precipitation tail liquid.
Preferably, in the step (4), the zinc powder needs to be ground before being added, and is sieved by a 150-mesh and 200-mesh sieve.
Compared with the prior art, the invention has the following advantages:
in order to improve the separation purity of rhodium, the invention adds aqua regia to dissolve solid containing rhodium and ruthenium, then continuously adds rhodium precipitating agent to precipitate and enrich precious metal rhodium until the concentration of Ru in precipitation tail liquid is detected to be 0.001g/L, which has no influence on the purity of recovered rhodium, then collects the precipitation tail liquid of each stage, and adds zinc powder to reduce, thereby achieving the purpose of separating rhodium from ruthenium. In the separation process, aqua regia is adopted for dissolution, rhodium precipitating agent is added into the dissolved liquid for precipitation and enrichment of metal rhodium, and separation of rhodium and ruthenium is achieved after filtration. The invention adopts a rhodium precipitation reagent, and adds zinc powder as a reducing agent, thereby greatly reducing the separation cost of rhodium and ruthenium, and the invention can obtain rhodium powder and ruthenium powder with the purity of more than 99 percent.
The specific implementation mode is as follows:
in order that the invention may be better understood, the invention is further illustrated by the following examples, which are intended to be illustrative only and are not to be construed as limiting the invention in any way.
Example 1
A method for separating rhodium and ruthenium from a noble metal mixed solution comprises the following steps:
(1) dissolving a rhodium-and-ruthenium-containing solid by aqua regia to prepare a rhodium-and-ruthenium-containing mixed solution, wherein the content of rhodium (Rh) in the mixed solution is 8.3g/L, and the content of ruthenium (Ru) in the mixed solution is 0.103g/L, adding the rhodium-and-ruthenium-containing mixed solution into a PP (polypropylene) barrel, then adding a rhodium precipitation reagent solution, adding 500ml of rhodium precipitation reagent into 1kg of rhodium, stirring and precipitating for 30min, standing for 1h, collecting precipitate and precipitation tail liquid, washing the precipitate, placing the precipitate into a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to prepare a denitrified rhodium-and-ruthenium-containing mixed solution; ICP detection shows that Rh content in the precipitation tail liquid is 0.025g/L, and ruthenium content is 0.083 g/L;
(2) adding the mixed solution containing rhodium and ruthenium obtained in the step (1) after denitration into a PP barrel, continuously adding a rhodium precipitation reagent solution, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentrations of Rh and Ru in the precipitation tail solution to be 0.021g/L and 0.011g/L respectively by adopting an ICP (inductively coupled plasma) technology;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia to dissolve the precipitate, cooling the precipitate to room temperature to prepare rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the liquid to respectively obtain the concentrations of Rh and Ru of 21.3g/L and 0.001 g/L;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation reagent solution, stirring and precipitating, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), adding zinc powder, stirring and reducing, and collecting ruthenium, wherein the addition amount of the zinc powder is 5 times of the content of ruthenium.
Example 2
A method for separating rhodium and ruthenium from a noble metal mixed solution comprises the following steps:
(1) dissolving a rhodium-and-ruthenium-containing solid by aqua regia to prepare a rhodium-and-ruthenium-containing mixed solution, wherein the content of rhodium (Rh) in the mixed solution is 8.3g/L, and the content of ruthenium (Ru) in the mixed solution is 0.103g/L, adding the rhodium-and-ruthenium-containing mixed solution into a PP (polypropylene) barrel, then adding a rhodium precipitation reagent, adding 510ml of rhodium precipitation reagent into 1kg of rhodium, stirring and precipitating for 30min, standing for 1h, collecting precipitate and precipitation tail liquid, washing the precipitate, placing the precipitate into a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to prepare a denitrified rhodium-and-ruthenium-containing mixed solution; ICP detection shows that Rh content in the precipitation tail liquid is 0.025g/L, and ruthenium content is 0.083 g/L;
(2) adding the mixed solution containing rhodium and ruthenium obtained in the step (1) after denitration into a PP barrel, continuously adding a rhodium precipitation reagent solution, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentrations of Rh and Ru in the precipitation tail solution to be 0.021g/L and 0.011g/L respectively by adopting an ICP (inductively coupled plasma) technology;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia to dissolve the precipitate, cooling the precipitate to room temperature to prepare rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the liquid to respectively obtain the concentrations of Rh and Ru of 21.3g/L and 0.001 g/L;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation reagent solution, stirring and precipitating, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), adding zinc powder, stirring and reducing, and collecting ruthenium, wherein the addition amount of the zinc powder is 5 times of the content of ruthenium.
Example 3
A method for separating rhodium and ruthenium from a noble metal mixed solution comprises the following steps:
(1) dissolving a rhodium-and-ruthenium-containing solid by aqua regia to prepare a rhodium-and-ruthenium-containing mixed solution, wherein the content of rhodium (Rh) in the mixed solution is 8.3g/L, and the content of ruthenium (Ru) in the mixed solution is 0.103g/L, adding the rhodium-and-ruthenium-containing mixed solution into a PP (polypropylene) barrel, then adding a rhodium precipitation reagent, adding 520ml of rhodium into 1kg of rhodium, stirring and precipitating for 30min, standing for 1h, collecting precipitate and precipitate tail solution, washing the precipitate, placing the precipitate into a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to prepare a denitrified rhodium-and-ruthenium-containing mixed solution; ICP detection shows that Rh content in the precipitation tail liquid is 0.025g/L, and ruthenium content is 0.083 g/L;
(2) adding the mixed solution containing rhodium and ruthenium obtained in the step (1) after denitration into a PP barrel, continuously adding a rhodium precipitation reagent solution, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentrations of Rh and Ru in the precipitation tail solution to be 0.021g/L and 0.011g/L respectively by adopting an ICP (inductively coupled plasma) technology;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia to dissolve the precipitate, cooling the precipitate to room temperature to prepare rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the liquid to respectively obtain the concentrations of Rh and Ru of 21.3g/L and 0.001 g/L;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation reagent solution, stirring and precipitating, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), adding zinc powder, stirring and reducing, and collecting ruthenium, wherein the addition amount of the zinc powder is 5 times of the content of ruthenium.
Example 4
A method for separating rhodium and ruthenium from a noble metal mixed solution comprises the following steps:
(1) dissolving a rhodium-and-ruthenium-containing solid by aqua regia to prepare a rhodium-and-ruthenium-containing mixed solution, wherein the content of rhodium (Rh) in the mixed solution is 8.3g/L, and the content of ruthenium (Ru) in the mixed solution is 0.103g/L, adding the rhodium-and-ruthenium-containing mixed solution into a PP (polypropylene) barrel, then adding a rhodium precipitation reagent, adding 530ml of rhodium precipitation reagent into 1kg of rhodium, stirring and precipitating for 30min, standing for 1h, collecting precipitate and precipitation tail liquid, washing the precipitate, placing the precipitate into a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to prepare a denitrified rhodium-and-ruthenium-containing mixed solution; ICP detection shows that Rh content in the precipitation tail liquid is 0.025g/L, and ruthenium content is 0.083 g/L;
(2) adding the mixed solution containing rhodium and ruthenium obtained in the step (1) after denitration into a PP barrel, continuously adding a rhodium precipitation reagent solution, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentrations of Rh and Ru in the precipitation tail solution to be 0.021g/L and 0.011g/L respectively by adopting an ICP (inductively coupled plasma) technology;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia to dissolve the precipitate, cooling the precipitate to room temperature to prepare rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the liquid to respectively obtain the concentrations of Rh and Ru of 21.3g/L and 0.001 g/L;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation reagent solution, stirring and precipitating, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), adding zinc powder, stirring and reducing, and collecting ruthenium, wherein the addition amount of the zinc powder is 5 times of the content of ruthenium.
Example 5
A method for separating rhodium and ruthenium from a noble metal mixed solution comprises the following steps:
(1) dissolving a rhodium-and-ruthenium-containing solid by aqua regia to prepare a rhodium-and-ruthenium-containing mixed solution, wherein the content of rhodium (Rh) in the mixed solution is 8.3g/L, and the content of ruthenium (Ru) in the mixed solution is 0.103g/L, adding the rhodium-and-ruthenium-containing mixed solution into a PP (polypropylene) barrel, then adding a rhodium precipitation reagent, adding 540ml of rhodium precipitation reagent into 1kg of rhodium, stirring and precipitating for 30min, standing for 1h, collecting precipitate and precipitation tail liquid, washing the precipitate, placing the precipitate into a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to prepare a denitrified rhodium-and-ruthenium-containing mixed solution; ICP detection shows that Rh content in the precipitation tail liquid is 0.025g/L, and ruthenium content is 0.083 g/L;
(2) adding the mixed solution containing rhodium and ruthenium obtained in the step (1) after denitration into a PP barrel, continuously adding a rhodium precipitation reagent solution, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentrations of Rh and Ru in the precipitation tail solution to be 0.021g/L and 0.011g/L respectively by adopting an ICP (inductively coupled plasma) technology;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia to dissolve the precipitate, cooling the precipitate to room temperature to prepare rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the liquid to respectively obtain the concentrations of Rh and Ru of 21.3g/L and 0.001 g/L;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation reagent solution, stirring and precipitating, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), adding zinc powder, stirring and reducing, and collecting ruthenium, wherein the addition amount of the zinc powder is 5 times of the content of ruthenium.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (4)
1. A method for separating rhodium and ruthenium from a noble metal mixed solution is characterized by comprising the following steps:
(1) adding the noble metal mixed solution into a PP (polypropylene) barrel, adding a rhodium precipitation agent, stirring and precipitating for 30min, standing for 1h, collecting precipitate, washing, placing in a porcelain jar, slowly dropwise adding aqua regia, stirring until the precipitate is dissolved, and cooling to room temperature to obtain a denitrated mixed solution containing rhodium and ruthenium;
the precious metal mixed solution is prepared by dissolving rhodium and ruthenium-containing solid by aqua regia, wherein the Rh content in the precious metal mixed solution is 8.3g/L, and the Ru content is 0.103 g/L;
the Rh content in the precipitation tail liquid after the rhodium precipitation agent is added for precipitation is 0.025g/L, and the Ru content is 0.083 g/L;
the mass concentration of the rhodium precipitation agent is 50%, and during precipitation, 500-550ml of rhodium precipitation agent is added into 1kg of rhodium;
the aqua regia is prepared by mixing hydrochloric acid with the mass concentration of 31% and nitric acid with the mass concentration of 65% according to the volume ratio of 1: 3;
(2) adding the denitrated mixed solution containing rhodium and ruthenium obtained in the step (1) into a PP (polypropylene) barrel, continuously adding a rhodium precipitation agent, stirring and precipitating for 30min, standing for 1h, collecting precipitate, and testing the concentration of Rh and Ru in the precipitation tail solution by adopting an ICP (inductively coupled plasma) technology;
the concentrations of Rh and Ru in the precipitation tail liquid are 0.021g/L and 0.011g/L respectively;
(3) washing the precipitate collected in the step (2), adding the precipitate into a porcelain jar, slowly adding aqua regia for dissolution, cooling to room temperature after complete dissolution to obtain rhodium-ruthenium-containing liquid subjected to secondary denitration, and performing ICP (inductively coupled plasma) test on the rhodium-ruthenium-containing liquid;
the concentration of Rh and Ru in the rhodium-and ruthenium-containing liquid after the secondary denitration is respectively as follows: 21.3g/L and 0.001 g/L;
(4) and (3) adding the liquid containing rhodium and ruthenium obtained after the secondary denitration in the step (3) into a PP (polypropylene) barrel, adding a rhodium precipitation agent for stirring and precipitation, filtering and recovering rhodium after precipitation, collecting precipitation tail liquid in the steps (1) and (2), then adding zinc powder, stirring and reducing, and collecting ruthenium.
2. The method for separating rhodium and ruthenium from a mixed solution of noble metals as claimed in claim 1, wherein in the step (1), 500ml of rhodium precipitating agent is added to 1kg of rhodium during precipitation.
3. The method for separating rhodium and ruthenium from mixed solution of noble metals as claimed in claim 1, wherein in step (4), the zinc powder is added in an amount which is five times of the ruthenium content in the precipitation tail solution.
4. The method as claimed in claim 1, wherein in step (4), the zinc powder is ground and sieved through a 150-200 mesh sieve before being added.
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| CN101748284A (en) * | 2008-12-22 | 2010-06-23 | 财团法人工业技术研究院 | Method for recovering precious metal |
| CN103014322A (en) * | 2013-01-07 | 2013-04-03 | 郴州高鑫铂业有限公司 | Method for efficiently separating and purifying rhodium and ruthenium |
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| CN101748284A (en) * | 2008-12-22 | 2010-06-23 | 财团法人工业技术研究院 | Method for recovering precious metal |
| CN103014322A (en) * | 2013-01-07 | 2013-04-03 | 郴州高鑫铂业有限公司 | Method for efficiently separating and purifying rhodium and ruthenium |
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