CN108330291B - Platinum separation and purification process - Google Patents
Platinum separation and purification process Download PDFInfo
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- CN108330291B CN108330291B CN201810053056.1A CN201810053056A CN108330291B CN 108330291 B CN108330291 B CN 108330291B CN 201810053056 A CN201810053056 A CN 201810053056A CN 108330291 B CN108330291 B CN 108330291B
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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
- C22B11/042—Recovery of noble metals from waste materials
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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
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B3/409—Mixtures at least one compound being an organo-metallic compound
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Abstract
The invention relates to the technical field of precious metal separation and purification, in particular to a platinum separation and purification process, which comprises base metal impurity removal treatment, extraction treatment, back extraction treatment and reduction treatment. The separation and purification method greatly improves the extraction efficiency of the platinum and also improves the purity of the platinum.
Description
Technical Field
The invention relates to the technical field of precious metal purification, in particular to a platinum separation and purification process.
Background
Platinum is also called platinum, has excellent chemical property stability, can be used as jewelry ornaments or artware, and can also be used as a catalyst in advanced chemical vessels, platinum crucibles, electrodes or chemical reactions; in addition, in the field of special materials, platinum can be used as an important raw material for producing high-temperature thermocouples.
At present, precipitation and solvent extraction methods are commonly used for separating and purifying platinum. The precipitation method has the advantages of long extraction process, low yield, high cost, simple solvent extraction process, high applicability and flexibility to various materials and large processing capacity, so the precipitation method is widely popularized and applied; however, the solvent extraction method has some problems when the platinum is extracted, the existing extraction system has low extraction efficiency on the platinum, and when the concentration of the platinum is increased, an association system formed by the platinum and an extracting agent has high concentration, the extraction system is turbid, and the phase separation speed is slow. Therefore, the development of a new extraction process is an important research direction of the technology.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of the prior art, the platinum separation and purification process is provided, the extraction efficiency of platinum can be improved by utilizing the process, and the purity of platinum is also improved.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a process for the separation and purification of platinum, said purification process comprising the steps of:
(1) adding concentrated nitric acid into the platinum waste, heating and stirring, adding an oxidant, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) adding the platinum concentrated solution obtained in the step (2) into an organic phase, uniformly stirring, adjusting the pH, heating, standing for phase splitting, and respectively collecting a water phase and an extract liquor;
(4) taking the extraction liquid in the step (3), regulating the acidity of the extraction liquid by hydrochloric acid, performing back extraction, standing for phase splitting, and collecting back extraction liquid;
(5) and (4) adding a reducing agent into the back extraction solution obtained in the step (4), boiling, filtering to obtain black precipitates, washing, calcining and cooling to obtain the spongy platinum.
As an improved technical scheme, the concentrated nitric acid in the step (1) is 60-80 wt% of concentrated nitric acid, and the oxidant is sodium peroxide or hydrogen peroxide.
As an improved technical proposal, the temperature of the heating in the step (1) is controlled between 95 and 105 ℃.
As an improved technical scheme, the organic phase in the step (3) comprises an extracting agent and a diluting agent, wherein the extracting agent comprises N-2-chlorphenyl-N' -benzoyl thiourea and tributyl phosphate; the diluent is toluene, n-octane, isoamyl alcohol or n-dodecane.
As a preferable technical scheme, the concentration of the N-2-chlorphenyl-N' -benzoyl thiourea is 0.012-0.018 mol/L.
As an improved technical scheme, the pH value is controlled to be 4-5 during the extraction in the step (3), and the temperature is controlled to be 80-85 ℃ during the heating.
As an improved technical scheme, the back extraction in the step (4) is carried out by using 0.5-0.8 wt% of thiourea.
As an improved technical scheme, the hydrochloric acid concentration used for adjusting the acidity of the extraction liquid in the step (4) is 0.8 mol/L-1.2 mol/L.
As an improved technical scheme, the reducing agent in the step (5) is hydrazine hydrochloride or hydrazine hydrate or formaldehyde.
After the technical scheme is adopted, the invention has the beneficial effects that:
(1) according to the invention, the platinum-containing waste is dissolved by using high-concentration nitric acid, and then the oxidizing agent is added for treatment, so that base metals such as copper, iron, magnesium and the like in the platinum waste can be effectively removed, and the purity of platinum is improved;
(2) the invention adopts N-2-chlorphenyl-N '-benzoyl thiourea and tributyl phosphate as extracting agents, and the extracting agents are diluted by toluene, N-octane, isoamylol or N-dodecane and then used as organic phase to extract platinum, the N-2-chlorphenyl-N' -benzoyl thiourea and tributyl phosphate composite extracting agent has better extraction capability to platinum, and the purpose of separating and extracting the platinum from other noble metals is realized through phase splitting. The phase separation time of the extraction system is short, the primary extraction rate of platinum can reach 99.999%, the extraction separation effect is good, the purity of the obtained platinum powder can reach 99.9989%, and the obtained platinum powder can be used as a raw material of a thermocouple, a high-grade chemical vessel or a catalyst in chemical reaction, so that the use cost of platinum is greatly reduced.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A separation and purification process of platinum comprises the following steps:
(1) adding 68 wt% of concentrated nitric acid into platinum waste, controlling the heating temperature at 96 ℃, stirring, adding an oxidant (sodium peroxide) accounting for 0.15% of the weight of the platinum waste, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) taking the platinum concentrated solution in the step (2), adding an organic phase (0.012 mol/L of N-2-chlorphenyl-N' -benzoyl thiourea, tributyl phosphate and toluene according to the volume ratio of 1:1: 2) according to the proportion of 1:1 of O/A, uniformly stirring, adjusting the pH value to 4.2, controlling the heating temperature to 80 ℃, standing for phase separation, and respectively collecting a water phase and an extract;
(4) taking the extract liquor obtained in the step (3), adjusting the acidity of the extract liquor by using 0.8 mol/L hydrochloric acid, adding 0.5 wt% of thiourea according to the proportion of 1:1 of O/A, performing back extraction, standing for phase separation, and collecting back extract liquor;
(5) and (4) adding a reducing agent (formaldehyde) into the stripping solution obtained in the step (4), boiling, filtering to obtain black precipitate, washing, calcining and cooling to obtain the spongy platinum.
Under the process conditions, the purity of the platinum is 99.9983%, and the extraction rate of the platinum is 99.995%.
Example 2
A separation and purification process of platinum comprises the following steps:
(1) adding 70 wt% of concentrated nitric acid into platinum waste, controlling the heating temperature at 98 ℃, stirring, adding an oxidant (sodium peroxide) accounting for 0.2% of the weight of the platinum waste, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) adding the platinum concentrated solution obtained in the step (2) into an organic phase (0.014 mol/L N-2-chlorphenyl-N' -benzoyl thiourea, tributyl phosphate and N-octane according to the volume ratio of 1.5:1:2) according to the O/A ratio of 1:1.2, uniformly stirring, adjusting the pH value to 4.5, controlling the heating temperature to 82 ℃, standing for phase separation, and respectively collecting a water phase and an extract;
(4) taking the extract liquor obtained in the step (3), adjusting the acidity of the extract liquor by using 0.9 mol/L hydrochloric acid, adding 0.6 wt% of thiourea according to the proportion of 1:1.5 of O/A, carrying out back extraction, standing for phase separation, and collecting back extract liquor;
(5) and (4) adding a reducing agent (hydrazine hydrochloride or hydrazine hydrate or formaldehyde) into the stripping solution obtained in the step (4), boiling, filtering, washing black precipitates, calcining and cooling to obtain the spongy platinum.
Under the process condition, the purity of the platinum is 99.9984%, and the extraction rate of the platinum is 99.996%.
Example 3
A separation and purification process of platinum comprises the following steps:
(1) adding 78 wt% of concentrated nitric acid into platinum waste, heating at 102 ℃, stirring, adding an oxidant (hydrogen peroxide) accounting for 0.35% of the weight of the platinum waste, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) adding the platinum concentrated solution obtained in the step (2) into an organic phase (N-2-chlorphenyl-N' -benzoyl thiourea, tributyl phosphate and isoamylol in a volume ratio of 1.8:1.2:3 of 0.016 mol/L) according to the proportion that O/A is 1:1.8, uniformly stirring, adjusting the pH value to 4.8, controlling the heating temperature to 83 ℃, standing for phase separation, and respectively collecting a water phase and an extract;
(4) taking the extract liquor obtained in the step (3), adjusting the acidity of the extract liquor by using 1 mol/L hydrochloric acid, adding 0.75 wt% of thiourea according to the proportion of 1:1.8 of O/A, performing back extraction, standing for phase separation, and collecting back extract liquor;
(5) and (4) adding a reducing agent (hydrazine hydrochloride) into the stripping solution obtained in the step (4), boiling, filtering to obtain black precipitates, washing, calcining and cooling to obtain the spongy platinum.
Under the process condition, the purity of the platinum is 99.9989%, and the extraction rate of the platinum is 99.999%.
Example 4
A separation and purification process of platinum comprises the following steps:
(1) adding 80 wt% of concentrated nitric acid into platinum waste, heating to 105 ℃, stirring, adding an oxidant (sodium peroxide or hydrogen peroxide) accounting for 0.5 wt% of the platinum waste, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) adding the platinum concentrated solution obtained in the step (2) into an organic phase (0.018 mol/L of N-2-chlorphenyl-N' -benzoyl thiourea, tributyl phosphate and N-dodecane according to the volume ratio of 2:1.5: 3) according to the O/A ratio of 1:2, uniformly stirring, adjusting the pH value to 5, controlling the heating temperature to 85 ℃, standing for phase separation, and respectively collecting a water phase and an extract;
(4) taking the extract liquor obtained in the step (3), adjusting the acidity of the extract liquor by using 1.2 mol/L hydrochloric acid, adding 0.8 wt% of thiourea according to the proportion of 1:2 of O/A, performing back extraction, standing for phase separation, and collecting back extract liquor;
(5) and (4) adding a reducing agent (hydrazine hydrate) into the stripping solution obtained in the step (4), boiling, filtering to obtain black precipitates, washing, calcining and cooling to obtain the spongy platinum.
Under the process condition, the purity of the platinum is 99.9986%, and the extraction rate of the platinum is 99.997%.
Example 5
A separation and purification process of platinum comprises the following steps:
(1) adding 80 wt% of concentrated nitric acid into platinum waste, heating to 105 ℃, stirring, adding an oxidant (sodium peroxide or hydrogen peroxide) accounting for 0.5 wt% of the platinum waste, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) adding the platinum concentrated solution obtained in the step (2) into an organic phase (0.018 mol/L of N-2-chlorphenyl-N' -benzoyl thiourea and paraffin according to the volume ratio of 1.5: 3) according to the O/A ratio of 1:2, stirring and uniformly mixing, adjusting the pH value to 5, controlling the heating temperature to 85 ℃, standing and phase splitting, and respectively collecting a water phase and an extract;
(4) taking the extraction liquid in the step (3), regulating the acidity of the extraction liquid by using 1 mol/L hydrochloric acid, adding 0.8 wt% of thiourea according to the proportion of 1:2 of O/A, performing back extraction, standing for phase separation, and collecting a back extraction liquid;
(5) and (4) adding a reducing agent (hydrazine hydrate) into the stripping solution obtained in the step (4), boiling, filtering to obtain black precipitates, washing, calcining and cooling to obtain the spongy platinum.
Under the process condition, the purity of the platinum is more than 99.9988%, and the extraction rate of the platinum is 99.998%.
Claims (7)
1. A separation and purification process of platinum is characterized by comprising the following steps:
(1) adding concentrated nitric acid into the platinum waste, heating and stirring, adding an oxidant, stirring, filtering after the reaction is finished, and collecting platinum slag;
(2) taking the platinum slag obtained in the step (1), adding excessive aqua regia, heating and dissolving, removing concentrated nitric acid, and concentrating to obtain a platinum concentrated solution;
(3) adding the platinum concentrated solution obtained in the step (2) into an organic phase, uniformly stirring, adjusting the pH, heating, standing for phase splitting, and respectively collecting a water phase and an extract liquor; wherein the organic phase comprises an extractant and a diluent, and the extractant comprises N-2-chlorphenyl-N' -benzoyl thiourea and tributyl phosphate; the diluent is toluene, n-octane, isoamylol or n-dodecane; controlling the pH value to be 4-5 during extraction and controlling the temperature to be 80-85 ℃ during heating;
(4) taking the extraction liquid in the step (3), regulating the acidity of the extraction liquid by hydrochloric acid, performing back extraction, standing for phase splitting, and collecting back extraction liquid;
(5) and (4) adding a reducing agent into the back extraction solution obtained in the step (4), boiling, filtering to obtain black precipitates, washing, calcining and cooling to obtain the spongy platinum.
2. The process for separating and purifying platinum according to claim 1, wherein: the concentrated nitric acid in the step (1) is 60-80 wt% of concentrated nitric acid, and the oxidant is sodium peroxide or hydrogen peroxide.
3. The process for separating and purifying platinum according to claim 1, wherein: the temperature is controlled to be 95-105 ℃ when the step (1) is heated.
4. The process for separating and purifying platinum as claimed in claim 1, wherein the concentration of the N-2-chlorphenyl-N' -benzoyl thiourea is 0.012-0.018 mol/L.
5. The process for separating and purifying platinum according to claim 1, wherein: and (4) carrying out back extraction by using 0.5-0.8 wt% of thiourea during the back extraction.
6. The process for separating and purifying platinum as claimed in claim 1, wherein the hydrochloric acid concentration used in the step (4) for adjusting the acidity of the extraction solution is 0.8 mol/L-1.2 mol/L.
7. The process for separating and purifying platinum according to claim 1, wherein: in the step (5), the reducing agent is hydrazine hydrochloride or hydrazine hydrate or formaldehyde.
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| CN111321299B (en) * | 2020-03-23 | 2021-12-14 | 紫金矿业集团股份有限公司 | Method for efficiently separating silver, platinum and palladium from silver anode mud |
| CN111575497A (en) * | 2020-06-24 | 2020-08-25 | 广东金正龙科技有限公司 | Method for accelerating platinum dissolution |
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| CN102220494B (en) * | 2011-06-08 | 2012-08-29 | 西北师范大学 | Method for separating palladium and copper from solution containing copper, cobalt and nickel by taking acylthiourea as extractant |
| CN102731392B (en) * | 2012-07-06 | 2014-02-26 | 云南民族大学 | Platinum characteristic complexing agent, preparation method and application for extracting, and enriching and testing platinum |
| CN103468967B (en) * | 2013-09-04 | 2015-07-15 | 重庆材料研究院有限公司 | Extraction method of platinum in high-concentration platinum solution |
| CN103468968B (en) * | 2013-09-04 | 2015-07-29 | 重庆材料研究院有限公司 | The extracting method of platinum rhodium in a kind of platinum rhodium mixed liquor |
| CN103805784B (en) * | 2014-03-03 | 2016-01-13 | 北京工业大学 | A kind of synergistic extraction method of fetching receipts platinum based on Recovery by Solvent Extraction Methold |
| CN105256144B (en) * | 2015-11-18 | 2017-10-03 | 金川集团股份有限公司 | A kind of technique that refined platinum is purified in the strip liquor from platinum |
| CN106756085B (en) * | 2016-12-22 | 2019-02-05 | 邝贤语 | A kind of smelting process of platinum concentrate |
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