CN113215405B - Method for recovering rare and precious metals from waste three-way catalyst - Google Patents
Method for recovering rare and precious metals from waste three-way catalyst Download PDFInfo
- Publication number
- CN113215405B CN113215405B CN202110439270.2A CN202110439270A CN113215405B CN 113215405 B CN113215405 B CN 113215405B CN 202110439270 A CN202110439270 A CN 202110439270A CN 113215405 B CN113215405 B CN 113215405B
- Authority
- CN
- China
- Prior art keywords
- powder
- silver
- palladium
- platinum
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- 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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/026—Recovery of noble metals from waste materials from spent catalysts
-
- 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
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
-
- 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
- C22B11/06—Chloridising
-
- 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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
- C22B13/00—Obtaining lead
- C22B13/06—Refining
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for recovering rare and precious metals from waste three-way catalysts, which comprises the following steps: crushing; adding hydrochloric acid and oxidant into the crushed material in the second step, and then performing filter pressing; step three: strong reduction is carried out after aluminum replacement, and then silver electrolysis is carried out; step four: mixing the leached slag with lead and silver slag for smelting; step five: electrolyzing silver after vacuum distillation; step six: adding nitric acid into silver anode mud obtained by silver electrolysis for decomposition, adding sodium chloride to obtain silver chloride, reducing the silver chloride into silver powder, replacing filtrate to obtain palladium black powder solution, adding ammonium chloride into the palladium black powder to obtain palladium red powder, adding ammonia water and hydrochloric acid into the red powder for precipitation to obtain palladium yellow powder, and adding ammonia water into the yellow powder for reduction to obtain palladium powder; step seven: adding aqua regia into the platinum-rhodium solid after the silver anode slime is decomposed to obtain rhodium powder; step eight: and seventhly, reducing and replacing the solution containing the aqua regia to obtain platinum black powder, precipitating the platinum black powder to obtain platinum yellow powder, washing and filtering the platinum yellow powder, and then reducing and replacing to obtain platinum powder. The invention has high recovery rate, saves processing cost, has high benefit and little pollution and is beneficial to environmental protection.
Description
Technical Field
The invention relates to the technical field of rare and precious metal recovery, in particular to a method for recovering rare and precious metals from a waste three-way catalyst.
Background
Harmful gases such as CO, HC and NOx discharged by automobile exhaust are converted into harmless carbon dioxide, water and nitrogen through the oxidation and reduction of three-way catalysis. The surface of the carrier of the three-way catalytic converter is coated with a thin catalyst coating, and the platinum group precious metals (platinum Pt, rhodium Rh and palladium Pd) directly play a catalytic role in the coating. The three-way catalyst mainly comprises the following components: more than 98 percent of aluminum oxide, 3000-10000 g/ton of palladium, 150-1000 g/ton of platinum and 150-600 g/ton of rhodium. The conventional technologies for recovering rare and precious metals from waste three-way catalysts in the prior art are basically two types:
1. fire method: ball-milling the three-way catalyst into powder, then mixing with lead soot and lead-silver slag for granulation, putting the mixture into a blast furnace for smelting and enrichment to obtain crude lead, removing ash and blowing, blowing ash to obtain silver-palladium-platinum-rhodium alloy, separating silver and palladium from alloy nitric acid, precipitating and separating silver and palladium from solution, separating platinum from solid by aqua regia, extracting platinum from the solution, and obtaining rhodium powder as aqua regia insoluble solid. However, in the method, because the content of the three-way catalyst is higher, lead and silver are not ideal for enriching platinum group metals, two-time enrichment is needed, and the melting slag has too high tail leakage; the enriched crude lead ash blowing also has the defects of high grade, lead oxide and ash blowing slag escaping, secondary crude lead ash blowing, long process, slow period, large pollution, low recovery rate, high processing cost, unfavorable environmental protection and unsatisfactory economic benefit.
2. And (2) wet method: the ternary catalyst is ball-milled into powder, and is put into a reaction kettle to be leached in a hydrochloric acid medium by an aqueous solution chlorination method, and a solution sodium nitrite complexation method. The method needs secondary leaching, the leaching solution affects the recovery of precious metals too much, the leaching residue is not completely leached, the residue recovery value is economical and not cost-effective, the process is long, the nitrous acid complexation method needs to be circulated for many times to separate platinum, palladium and rhodium, the labor intensity is high, the reagent cost is high, a large amount of waste gas and waste water are generated, precious metals are carried in the hydrolysis of base metals, when rhodium, platinum and palladium are separated, platinum and palladium carry rhodium, and rhodium carries platinum and palladium, so that the control is not good, the operation difficulty is large, although the method can directly recover and separate platinum, palladium and rhodium, the recovery rate is low, the cost is high, the waste gas and waste water treatment capacity is large, and the method is not beneficial to environmental protection.
Therefore, it is necessary to develop a method for recovering rare and precious metals from waste three-way catalysts to solve the above problems.
Disclosure of Invention
The invention aims to provide a method for recovering rare and precious metals from waste three-way catalysts, which has the advantages of high recovery rate, processing cost saving, high benefit, little pollution and environmental protection.
In order to achieve the above purpose, the invention provides the following technical scheme: a method for recovering rare and precious metals from waste three-way catalysts comprises the following steps:
the method comprises the following steps: putting the three-way catalyst into an ultrafine grinder to grind to 200 meshes;
step two: putting the crushed material in the first step into a steel-lined tetrafluoro reaction kettle, and adding a raw material 1:1, continuously injecting an oxidant, introducing steam, heating to 100-120 ℃, fully and completely reacting at high temperature and normal pressure for 8 hours, then adding water for washing, and performing filter pressing twice by using a filter press;
step three: performing aluminum replacement on the filter liquor subjected to filter pressing in the step two to obtain palladium-platinum-rhodium alloy powder, adding No. 1 silver powder into the palladium-platinum-rhodium alloy powder, putting the palladium-platinum-rhodium alloy powder and the No. 1 silver powder into a high-temperature small intermediate frequency furnace for strong reduction smelting to obtain a silver-platinum-palladium-rhodium alloy ingot, and then feeding the silver ingot to silver electrolysis;
step four: the leached slag after the leaching of the ternary catalyst is mixed with lead and silver slag and put into a high-temperature intermediate frequency furnace for smelting to obtain crude lead-silver noble metal alloy containing palladium, platinum, rhodium and silver;
step five: feeding the crude lead-silver noble metal alloy obtained in the step four into a vacuum furnace for vacuum distillation to obtain crude lead, and feeding the obtained silver palladium platinum rhodium alloy ingot into a silver electrolysis furnace;
step six: electrolyzing the silver in the fifth step to obtain No. 1 silver powder and silver anode mud, adding nitric acid into the silver anode mud to decompose the silver anode mud to obtain a silver palladium solution, adding sodium chloride into the silver palladium solution to obtain a silver chloride precipitate, filter-pressing the silver chloride precipitate by using a filter press to obtain silver chloride and filtrate, adding sodium chloride and hydrazine hydrate to reduce the silver chloride into silver powder, adding sodium chloride and hydrazine hydrate to replace the filtrate to obtain a palladium black powder solution, filtering the palladium black powder solution to obtain filtrate and palladium black powder, adding aqua regia into the palladium black powder to dissolve the palladium black powder, filtering the filtrate, adding ammonium chloride into the filtrate to obtain palladium red powder, filtering the palladium red powder to obtain red powder and filtrate, adding ammonia into the red powder to dissolve the red powder to obtain a palladium solution, filtering the palladium solution, adding hydrochloric acid into the filtrate to precipitate to obtain palladium yellow powder, filtering the palladium yellow powder to obtain yellow powder and filtrate, adding ammonia into the yellow powder to dissolve the palladium solution to obtain a palladium solution, filtering the filtrate, and adding hydrazine hydrate to reduce the filtrate to obtain 99.95% palladium powder;
step seven: adding aqua regia to decompose the platinum-rhodium solid after the silver anode slime is decomposed in the sixth step to obtain rhodium powder serving as the solid in the obtained solution, and obtaining 99.85% rhodium powder;
step eight: and seventhly, adding sodium hydroxide and hydrazine hydrate into the aqua regia-containing solution for reduction and displacement to obtain platinum black powder and a solution, adding hydrochloric acid and hydrogen peroxide into the platinum black powder for dissolution to obtain a platinum solution, filtering the platinum solution, adding ammonium chloride into the filtrate, precipitating, filtering to obtain platinum yellow powder, washing the platinum yellow powder with 10% diluted hydrochloric acid, filtering, and adding sodium hydroxide and hydrazine hydrate for reduction and displacement to obtain 99.95% platinum powder.
Preferably, the oxidizing agent in the second step is nitric acid or hydrofluoric acid.
Preferably, the wastewater from the aluminum substitution in the third step is subjected to wastewater treatment.
Preferably, the smelting slag in the fourth step is sent to a cement plant without value, and the crude lead obtained in the fifth step can be sold.
Preferably, the silver powder No. 1 obtained by electrolyzing the silver obtained in the sixth step is sent to a high-temperature small intermediate frequency furnace to be enriched with platinum, palladium and rhodium or sold for sale, and the silver powder reduced by adding sodium hydroxide and hydrazine hydrate to silver chloride is sent to the high-temperature small intermediate frequency furnace to be enriched with platinum, palladium and rhodium.
Preferably, in the sixth step, the filtrate obtained by filtering the palladium black powder solution, the filtrate obtained by filtering the palladium red powder, and the filtrate obtained by filtering the palladium yellow powder are subjected to water treatment.
Preferably, in the sixth step, filter residues obtained by filtering after dissolving the palladium black powder in aqua regia and filter residues obtained by filtering twice through palladium solution are returned to the high-temperature small intermediate frequency furnace.
Preferably, the platinum solution in the step eight is filtered, the filter residue is returned to the high-temperature small intermediate frequency furnace, and the washing water of the platinum yellow powder and the filtered filtrate are subjected to water treatment.
In the technical scheme, the invention has the following technical effects and advantages:
1. the invention has high recovery rate: the recovery rate of palladium, platinum and rhodium is over 99.5 percent, the process is short, the effect is quick, and the problems of large control difficulty, large odor pollution, low recovery rate and the like of the traditional technology are solved.
2. The silver powder and the filter residue obtained in the processing process can be fed into a high-temperature small intermediate frequency furnace to enrich platinum, palladium and rhodium, and the crude lead, the silver powder and the like can be sold, so that the processing cost is saved, and the benefit is high.
3. The washing water and the filtration in the processing process of the invention are both used for water treatment, the pollution is little, and the invention is beneficial to environmental protection.
Drawings
In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to these drawings.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a process flow diagram of the present invention;
Detailed Description
In order to make the technical solutions of the present invention better understood, those skilled in the art will now describe the present invention in further detail with reference to the accompanying drawings.
The invention provides a method for recovering rare and precious metals from waste ternary catalysts (the main components of the ternary catalysts are more than 98 percent of aluminum oxide, 3000-10000 g/ton of palladium, 150-1000 g/ton of platinum and 150-600 g/ton of rhodium) as shown in figures 1-2, which comprises the following steps:
the method comprises the following steps: the three-way catalyst is put into an ultrafine grinder to be ground to more than 200 meshes, the ground meshes of the ultrafine grinder are uniform, dust and pollution are avoided through cyclone collection, and the leaching rate is high;
step two: putting the crushed material obtained in the first step into a steel-lined tetrafluoro reaction kettle, wherein the steel-lined tetrafluoro reaction kettle is high in high temperature resistance, wear resistance, corrosion resistance and safety and suitable for various mixed acids, and then adding 1:1, continuously injecting an oxidant, namely nitric acid and hydrofluoric acid, introducing steam, heating to 100-120 ℃, fully and completely reacting at high temperature and normal pressure for 8 hours, then adding water, washing, and performing filter pressing twice by using a filter press, wherein the leaching rate reaches 95% of platinum, 98% of palladium and 85% of rhodium;
step three: performing aluminum replacement on the filter liquor subjected to filter pressing in the step two to obtain palladium-platinum-rhodium alloy powder, performing wastewater treatment on the aluminum-replaced wastewater, adding No. 1 silver powder into the palladium-platinum-rhodium alloy powder, putting the palladium-platinum-rhodium alloy powder into a high-temperature small intermediate frequency furnace for strong reduction smelting to obtain silver-platinum-palladium-rhodium alloy ingots, and then feeding the silver ingots for electrolysis, wherein no dissolution loss is generated when rhodium is decomposed by weak acid;
step four: the leached slag after the leaching of the ternary catalyst is mixed with lead and silver slag and put into a high-temperature intermediate frequency furnace for smelting, the low-grade leached slag is completely smelted and enriched, and the smelted slag is sent to a cement plant without value to obtain crude lead-silver noble metal alloy containing palladium, platinum, rhodium and silver;
step five: conveying the crude lead-silver precious metal alloy obtained in the step four to a vacuum furnace for vacuum distillation, wherein the vacuum furnace for vacuum distillation is dust-free, noise-free and pollution-free to obtain crude lead (sold for sale), and conveying the obtained silver-palladium-platinum-rhodium alloy ingot to silver electrolysis;
step six: electrolyzing the silver in the step five to obtain No. 1 silver powder and silver anode mud, feeding the No. 1 silver powder into a high-temperature small intermediate frequency furnace to enrich platinum, palladium and rhodium or sell the silver anode mud, adding nitric acid to decompose the silver anode mud to obtain a silver palladium solution, adding sodium chloride to the silver palladium solution to obtain a silver chloride precipitate, performing filter pressing on the silver chloride precipitate by using a filter press to obtain silver chloride and filtrate, reducing the silver chloride by adding sodium hydroxide and hydrazine hydrate to obtain silver powder, feeding the silver powder into the high-temperature small intermediate frequency furnace to enrich platinum, rhodium, replacing the filtrate (palladium solution) by adding sodium hydroxide and hydrazine hydrate to obtain a palladium black powder solution, filtering the palladium black powder solution to obtain filtrate and palladium black powder, performing water treatment on the filtrate, adding ammonia to decompose the red powder to obtain a palladium solution, filtering the palladium solution, returning the filter residue to the high-temperature small intermediate frequency furnace, adding hydrochloric acid to precipitate to obtain yellow powder, filtering the palladium yellow powder to obtain yellow powder and filtrate, performing water treatment on the filtrate, adding ammonia to dissolve the red powder to obtain a palladium solution, filtering the filter residue, and reducing the filter residue to obtain a high-temperature small intermediate frequency furnace to obtain a filter residue, and 99% reduction solution;
step seven: adding aqua regia to decompose the platinum-rhodium solid after the silver anode slime is decomposed in the sixth step to obtain solid in the solution, namely rhodium powder;
step eight: and seventhly, adding sodium hydroxide and hydrazine hydrate into the aqua regia-containing solution to perform reduction and replacement to obtain platinum black powder and solution, removing nitrate from aqua regia in the traditional technology, controlling difficulty and odor pollution to be high, precipitating platinum by ammonium chloride incompletely, treating the solution type water, dissolving the platinum black powder by adding hydrochloric acid and hydrogen peroxide to obtain platinum solution, completely precipitating platinum by ammonium chloride, filtering the platinum solution, returning filter residues to a high-temperature small intermediate frequency furnace, adding ammonium chloride into filtrate to precipitate, filtering to obtain platinum powder, washing the platinum powder by 10% diluted hydrochloric acid, filtering, performing water treatment on washing water and filtered filtrate, and performing reduction and replacement on the platinum powder by adding sodium hydroxide and hydrazine hydrate to obtain 99.95% platinum powder.
The invention has high recovery rate: the recovery rate of palladium, platinum and rhodium is more than 99.5 percent, the flow is short, the effect is quick, and the problems of great control difficulty, great odor pollution, low recovery rate and the like of the traditional technology are solved.
The silver powder and the filter residue obtained in the processing process can be fed into a high-temperature small intermediate frequency furnace to enrich platinum, palladium and rhodium, and the crude lead, the silver powder and the like can be sold, so that the processing cost is saved, and the benefit is high.
The washing water and the filtration in the processing process of the invention are both used for water treatment, the pollution is little, and the invention is beneficial to environmental protection.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.
Claims (8)
1. A method for recovering rare noble metals from waste three-way catalysts is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: putting the three-way catalyst into an ultrafine grinder to grind to 200 meshes;
step two: putting the crushed material in the first step into a steel lining tetrafluoro reaction kettle, and adding a raw material of 1:1, continuously injecting an oxidant, introducing steam, heating to 100-120 ℃, fully and completely reacting at high temperature and normal pressure for 8 hours, then adding water for washing, and performing filter pressing twice by using a filter press;
step three: performing aluminum replacement on the filter liquor subjected to filter pressing in the step two to obtain palladium-platinum-rhodium alloy powder, adding No. 1 silver powder into the palladium-platinum-rhodium alloy powder, putting the palladium-platinum-rhodium alloy powder and the No. 1 silver powder into a high-temperature small intermediate frequency furnace for strong reduction smelting to obtain a silver-platinum-palladium-rhodium alloy ingot, and then feeding the silver ingot to silver electrolysis;
step four: mixing the leached slag with lead and silver slag to smelt in high temperature intermediate frequency furnace to obtain lead-silver alloy containing Pd, pt, rh and Ag;
step five: feeding the crude lead-silver noble metal alloy obtained in the step four into a vacuum furnace for vacuum distillation to obtain crude lead, and feeding the obtained silver palladium platinum rhodium alloy ingot into a silver electrolysis furnace;
step six: electrolyzing silver in the fifth step to obtain No. 1 silver powder and silver anode mud, adding nitric acid into the silver anode mud to decompose the silver anode mud to obtain a silver palladium solution, adding sodium chloride into the silver palladium solution to obtain silver chloride precipitates, filter-pressing the silver chloride precipitates by using a filter press to obtain silver chloride and filtrate, adding sodium chloride and hydrazine hydrate to reduce the silver chloride into silver powder, adding sodium hydroxide and hydrazine hydrate to replace the filtrate to obtain a palladium black powder solution, filtering the palladium black powder solution to obtain filtrate and palladium black powder, adding aqua regia into the palladium black powder to dissolve the palladium black powder, filtering the filtrate, adding ammonium chloride into the filtrate to obtain palladium red powder, filtering the palladium red powder to obtain red powder and filtrate, adding ammonia into the red powder to dissolve the red powder to obtain a palladium solution, filtering the palladium solution, adding hydrochloric acid into the filtrate to precipitate to obtain palladium yellow powder, filtering the palladium yellow powder to obtain yellow powder and filtrate, adding ammonia into the yellow powder to dissolve to obtain a palladium solution, filtering the palladium solution, and adding hydrazine hydrate into the filtrate to reduce the palladium powder to obtain 99.95 percent;
step seven: adding aqua regia to decompose the platinum-rhodium solid after the silver anode slime is decomposed in the sixth step to obtain rhodium powder serving as the solid in the obtained solution, and obtaining 99.85 percent rhodium powder;
step eight: and seventhly, adding sodium hydroxide and hydrazine hydrate into the aqua regia-containing solution for reduction and displacement to obtain platinum black powder and a solution, adding hydrochloric acid and hydrogen peroxide into the platinum black powder for dissolution to obtain a platinum solution, filtering the platinum solution, adding ammonium chloride into the filtrate for precipitation, filtering to obtain platinum yellow powder, washing the platinum yellow powder with 10% dilute hydrochloric acid water, filtering, and adding sodium hydroxide and hydrazine hydrate for reduction and displacement to obtain 99.95% platinum powder.
2. The method for recovering rare and precious metals from waste three-way catalysts according to claim 1, characterized in that: and the oxidizing agent in the second step is nitric acid and hydrofluoric acid.
3. The method for recovering rare and precious metals from waste three-way catalysts according to claim 1, characterized in that: and (3) performing wastewater treatment on the wastewater subjected to aluminum replacement in the third step.
4. The method for recovering rare noble metals from waste three-way catalysts according to claim 1, characterized in that: and the smelting slag in the fourth step is worthless to be sent to a cement plant, and the crude lead obtained in the fifth step can be sold.
5. The method for recovering rare noble metals from waste three-way catalysts according to claim 1, characterized in that: and feeding the silver powder No. 1 obtained by electrolyzing the silver obtained in the step six into a high-temperature small intermediate frequency furnace for enriching platinum, palladium and rhodium or selling the silver powder, and feeding the silver powder reduced by adding sodium hydroxide and hydrazine hydrate into the high-temperature small intermediate frequency furnace for enriching platinum, palladium and rhodium.
6. The method for recovering rare noble metals from waste three-way catalysts according to claim 1, characterized in that: and in the sixth step, filtering the palladium black powder solution to obtain a filtrate, filtering the palladium red powder to obtain a filtrate, and filtering the palladium yellow powder to obtain a filtrate, and performing water treatment on the filtrate.
7. The method for recovering rare noble metals from waste three-way catalysts according to claim 1, characterized in that: and in the sixth step, filter residues obtained by filtering the palladium black powder after being dissolved by adding aqua regia and filter residues obtained by filtering the palladium solution twice are returned to the high-temperature small intermediate frequency furnace.
8. The method for recovering rare noble metals from waste three-way catalysts according to claim 1, characterized in that: and step eight, filtering the platinum solution, returning filter residues to the high-temperature small intermediate frequency furnace, and performing water treatment on washing water of the platinum yellow powder and filtered filtrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110439270.2A CN113215405B (en) | 2021-04-23 | 2021-04-23 | Method for recovering rare and precious metals from waste three-way catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110439270.2A CN113215405B (en) | 2021-04-23 | 2021-04-23 | Method for recovering rare and precious metals from waste three-way catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113215405A CN113215405A (en) | 2021-08-06 |
| CN113215405B true CN113215405B (en) | 2022-12-20 |
Family
ID=77088753
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110439270.2A Active CN113215405B (en) | 2021-04-23 | 2021-04-23 | Method for recovering rare and precious metals from waste three-way catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113215405B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114231749B (en) * | 2021-12-28 | 2023-11-21 | 金川集团股份有限公司 | Method for recovering platinum and rhodium from platinum and rhodium-containing waste liquid |
| CN114574708B (en) * | 2022-02-18 | 2024-01-26 | 武汉理工大学 | Method for recovering metal platinum from waste automobile tail gas three-way catalyst |
| CN115522055B (en) * | 2022-09-26 | 2023-07-21 | 湖南省金润碲业有限公司 | Environment-friendly platinum palladium rhodium precious metal smelting process and device |
| CN115558793B (en) * | 2022-11-02 | 2023-08-04 | 无锡威孚环保催化剂有限公司 | Method for separating and purifying platinum, palladium and rhodium from platinum-palladium-rhodium-containing solution |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090106067A (en) * | 2008-04-04 | 2009-10-08 | 주식회사 동방이엠티 | Precious metal collection method from scrap metals by dental technician |
| CN102041393A (en) * | 2010-12-30 | 2011-05-04 | 郴州市金贵银业股份有限公司 | Silver anode mud treatment process |
| CN105112670A (en) * | 2015-09-08 | 2015-12-02 | 云南锡业集团（控股）有限责任公司铅业分公司 | Comprehensive recovery method for platinum and palladium in silver electrolyte |
| CN106119554B (en) * | 2016-08-18 | 2018-01-16 | 紫金矿业集团股份有限公司 | High Purity Gold and the method for being enriched with silver, platinum and palladium are prepared from silver anode slime |
-
2021
- 2021-04-23 CN CN202110439270.2A patent/CN113215405B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113215405A (en) | 2021-08-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113215405B (en) | Method for recovering rare and precious metals from waste three-way catalyst | |
| CN102534244A (en) | Method for concentrating precious metal from low-grade precious metal material | |
| CN112981105B (en) | Method for recovering noble metal from waste alumina carrier noble metal catalyst | |
| CN112695200B (en) | Method for recovering selenium, gold and silver from copper anode slime | |
| CN111606308A (en) | Method for efficiently separating and recycling tellurium from copper anode slime copper separation slag | |
| CN112458288A (en) | Method for recovering and preparing silver material from silver-containing waste material | |
| CN111850300B (en) | Method for efficiently enriching platinum and palladium from low-concentration platinum-palladium nitric acid system solution | |
| CN111304457A (en) | Efficient activation dissolving method for rhodium powder | |
| CN109971962B (en) | Treatment process for copper, mercury, selenium, lead and gold and silver in copper smelting lead filter cake | |
| CN111996386B (en) | Method for recovering rhodium from rhodium-containing homogeneous phase waste catalyst | |
| CN111893313B (en) | Dissolving method of iron-platinum group metal alloy obtained by plasma smelting enrichment | |
| CN112442600A (en) | Method for recovering platinum group metal from waste three-way catalyst | |
| CN113151677B (en) | Method for leaching cobalt intermediate product by sulfate without acid | |
| JP4281534B2 (en) | Treatment method for platinum group-containing materials | |
| JP4269586B2 (en) | Methods for separating platinum group elements | |
| CN114107690A (en) | Method for extracting noble metal of three-way catalyst | |
| CN113564379A (en) | Method for recovering precious metal from spent automobile catalyst | |
| CN112267025A (en) | Method for extracting palladium from low-grade failure alumina carrier catalyst | |
| CN113005301A (en) | Method for recovering rare and precious metals from waste petrochemical catalyst | |
| CN114807605B (en) | Method for updating silver electrolyte by hydrogen peroxide | |
| CN116477679B (en) | Method for preparing chloroiridium acid by recycling and purifying iridium catalyst with alumina carrier | |
| CN115074533B (en) | Oxygen pressure green circulation gold leaching method for spent gold carbon catalyst | |
| CN114574708B (en) | Method for recovering metal platinum from waste automobile tail gas three-way catalyst | |
| CN114921814A (en) | Electrochemical recovery method of palladium in waste palladium catalyst | |
| CN114934180B (en) | Method for enriching ruthenium in alumina-based waste ruthenium-loaded catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |