CN108823418B - Method for synergistically recovering precious metals from spent automobile catalyst - Google Patents
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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
- 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
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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
- C22B11/02—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
- C22B11/028—Recovery of noble metals from waste materials from spent catalysts using solid sorbents, e.g. getters or catchment gauzes
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- 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 relates to the field of comprehensive utilization of secondary resources of precious metals, in particular to a method for synergistically recovering precious metals from a spent automobile catalyst. The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of: A. preparing and treating materials; B. preparing and mixing materials; C. smelting; D. and (4) sampling and analyzing slag. The method has the advantages of high recovery rate of noble metal, energy conservation, loss reduction, economic benefit increase, simple operation, clean production process and environmental friendliness.
Description
Technical Field
The invention relates to the field of comprehensive utilization of secondary resources of precious metals, in particular to a method for synergistically recovering precious metals from a spent automobile catalyst.
Background
Because of the specific purifying capacity of noble metals of platinum, palladium and rhodium to automobile exhaust, over 60 percent of platinum, palladium and rhodium are used for producing automobile three-way catalysts every year. As far as 2016, the quantity of automobiles in China is up to 1.94 hundred million, and 600-700 million automobiles are scrapped every year. According to the automobile sales in 2001-2013 and the service life of the automobile catalyst, the amount of the automobile catalyst which is lost in China market is about 1800 tons/year, and about 3 tons of precious metal can be recovered. Although many organizations are researching new catalysts to replace or reduce the amount of precious metals, the amount of precious metals used in the automotive industry is increasing due to the increase in the number of automobiles and the improvement in environmental standards. The number of the vehicles in China is estimated to exceed 3 hundred million in 2020, the number of recoverable spent catalysts of the vehicles is 7900-8000 tons, the precious metal content is about 15 tons, and the value is about 30 hundred million yuan. The dead automobile catalyst is one of the largest target markets of precious metal secondary resources.
There are many types of automotive catalysts, the earliest being gamma-Al2O3Currently, cordierite (2 MgO.2Al) is the most commonly used particulate catalyst as a carrier2O3·5SiO2) The honeycomb catalyst is a carrier, and because the size and the model of an automobile are different, the content of noble metal in the automobile exhaust catalyst is greatly different. The total content of the three noble metals of platinum, palladium and rhodium is 1000-3000 ppm. Many manufacturers of automobiles, carsThe types and the discharge capacities are diversified, so that the content of noble metals in the invalid automobile catalyst is different, the invalid automobile catalyst is crushed, ball-milled into powder and then enters an evaluation system of the invalid automobile catalyst, and public, transparent and fair transactions are realized.
The research and technical routes for recovering noble metals from the spent automobile catalyst are various, and wet and fire processes are applied in production. The wet process has the problems of low recovery rate of noble metals, large amount of waste water and the like, and is gradually eliminated. The pyrometallurgical technology is rich in precious metals, strong in material adaptability, high in recovery rate, capable of greatly improving the processing capacity and more environment-friendly, and the reagent dosage is reduced.
The main methods for treating the failure automobile catalyst by the pyrogenic process technology include a plasma high-temperature smelting iron trapping method, an electric arc furnace high-temperature smelting copper trapping method and the like. The high-temperature smelting copper trapping method has the advantages that the amount of copper or copper oxide added as a trapping element is large, about 60 percent, the trapping effect is good, the method is known as a rose technology, the recovery rate of noble metals is more than 99 percent, but the separation difficulty of copper and noble metals in later-stage noble metal-containing copper alloy is large, the technical route is long, the equipment investment is large, and the industrialization is not realized in China at present. The method for recovering noble metals from the spent automobile catalyst by adopting a plasma furnace or an electric arc furnace high-temperature smelting iron trapping method is a main process technology of industrial production in China.
At present, precious metals are recovered from a spent automobile catalyst by adopting a high-temperature smelting technology, and the recovery rate of platinum, palladium and rhodium is about 98%. The rest 2 percent of platinum, palladium and rhodium enter the slag, the content of noble metal in the slag is low, the recovery difficulty is high, and the cost is high.
The invention of CN200910094112.7 relates to a method for recovering precious metals from a spent automobile catalyst, which comprises the following steps: (1) mixing the spent automobile catalyst with a reducing agent, an additive and a trapping agent; (2) putting the mixed materials into a clay graphite crucible, and placing the clay graphite crucible into an electric furnace or smelting the clay graphite crucible in the electric furnace to obtain a noble metal phase; (3) selectively leaching base metals in the precious metal phase to obtain a precious metal concentrate, and refining the precious metal concentrate to produce a platinum, palladium and rhodium product.
But the additive and the trapping agent are used in large amount, and the energy consumption is large.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for synergistically recovering precious metals from a spent automobile catalyst, which has the advantages of high precious metal recovery rate, energy conservation, loss reduction, economic benefit increase, simplicity in operation, clean production process and environmental friendliness.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the total content of platinum, palladium and rhodium is 1000-3000 ppm, and the particle size of the catalyst is crushed to 40-200 meshes; the collector is hematite, Fe2O3The content of the coarse powder is more than 60 percent, and the coarse powder is crushed into 40 to 100 meshes; the synergistic trapping agent is chemically pure tin dioxide and chemically pure antimony trioxide which are both in powder form; the reducing agent is metallurgical coke, the content of C is 80%, and the reducing agent is crushed into 20-100 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percent, and the industrial lime is crushed into 20 to 100 meshes; crushing common glass into 20-100 mesh;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 100 parts of spent automobile catalyst, 2-10 parts of hematite, 1-5 parts of synergistic trapping agent, 1-10 parts of metallurgical coke, 10-20 parts of lime and 5-10 parts of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly raising the temperature at 180 ℃/h within 150-; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after smelting, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase from the metal phase, and weighing the slag phase;
D. sampling and analyzing slag: and C, crushing the slag obtained in the step C to 20-60 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, and calculating the recovery rate of the noble metal according to the content of the noble metal in the slag.
The synergistic trapping agent is a mixture of tin dioxide and antimony trioxide in any mass ratio.
The invention has the beneficial effects that:
1. the invention adopts the synergistic trapping agent, and in the process of recovering noble metals by smelting the main trapping agent iron at high temperature, 1 or 2 synergistic trapping agents are added, so that the recovery rate of the noble metals in the spent automobile catalyst can be improved, and the recovery rate of the noble metals is high and is more than 99%.
2. The invention adopts a synergistic trapping technology to assist the main trapping agent in recovering precious metals from the failed automobile catalyst, reduces the consumption of additives and trapping agents, saves energy, reduces loss and increases economic benefits.
3. The whole process of the invention does not need to add new equipment, has simple operation and is easy to realize industrialized production.
4. The smelting slag produced by the invention is inert slag, is non-toxic and harmless, and can be used as aggregate in the building industry and auxiliary material for building roads.
5. The invention has clean production process and is environment-friendly.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the content of palladium is 800ppm, the content of platinum is 120ppm, the content of rhodium is 80ppm, and the granularity of the catalyst is crushed to 40 meshes; the collector is hematite, Fe2O3Is 75%, and the granularity is crushed to 40 meshes; the synergistic trapping agent is chemically pure tin dioxide powder; the reducing agent is metallurgical coke, the content of C is 80%, and the granularity of the reducing agent is crushed to 20 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percentThe granularity is crushed to 20 meshes; common glass, the granularity of which is crushed to 20 meshes;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 5000 grams of spent automotive catalyst, 150 grams of hematite, 50 grams of chemically pure tin dioxide powder, 50 grams of metallurgical coke, 500 grams of lime and 250 grams of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly heating to 1500 ℃ at the speed of 150 ℃/h, and preserving heat for 60 minutes; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after the smelting is finished, turning off a power supply of the intermediate frequency furnace, pouring the melt into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase from the metal phase, weighing the slag phase, and weighing the slag with the weight of 5600 g;
D. sampling and analyzing slag: c, crushing the slag obtained in the step C to 20 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, wherein the content of palladium in the slag is 5.0ppm, the content of platinum in the slag is 1.56ppm, and the content of rhodium in the slag is 0.21 ppm; the recovery rate is calculated by the content of noble metals in the slag, the recovery rate of palladium is 99.30 percent, the recovery rate of platinum is 98.54 percent, the recovery rate of rhodium is 98.16 percent, and the total recovery rate of platinum, palladium and rhodium is 99.19 percent.
Example 2
The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the content of palladium is 1000ppm, the content of platinum is 180ppm, the content of rhodium is 110ppm, and the granularity of the catalyst is crushed to 80 meshes; the collector is hematite, Fe2O3Is 75 percent, and the granularity is crushed to 60 meshes; the synergistic trapping agent is chemically pure tin dioxide powder; the reducing agent is metallurgical coke, the content of C is 80%, and the granularity of the reducing agent is crushed to 40 meshes; the slag former is industrial lime and common glassThe CaO content in the lime is 70 percent, and the lime is crushed into 40 meshes in granularity; common glass, the granularity of which is crushed to 40 meshes;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 5000 grams of spent automobile catalyst, 150 grams of hematite, 50 grams of chemically pure antimony trioxide powder, 100 grams of metallurgical coke, 600 grams of lime and 250 grams of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly heating to 1500 ℃ at a speed of 160 ℃/h, and preserving heat for 60 minutes; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after the smelting is finished, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase from the metal phase, weighing the slag phase, and weighing 5650 g of slag;
D. sampling and analyzing slag: c, crushing the slag obtained in the step C to 20 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, wherein the content of palladium in the slag is 5.2ppm, the content of platinum is 1.65ppm and the content of rhodium is 0.25 ppm; the recovery rate is calculated by the content of noble metals in the slag, the recovery rate of palladium is 99.41 percent, the recovery rate of platinum is 98.96 percent, the recovery rate of rhodium is 98.72 percent, and the total recovery rate of platinum, palladium and rhodium is 99.33 percent.
Example 3
The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the content of palladium is 1200ppm, the content of platinum is 250ppm, the content of rhodium is 130ppm, and the granularity of the catalyst is crushed to 100 meshes; the collector is hematite, Fe2O3The content of (b) is 70%, and the particle size is crushed to 80 meshes; the synergistic trapping agent is chemically pure tin dioxide and chemically pure antimony trioxide which are both in powder form; the reducing agent is metallurgical coke with a C content of 80 percentCrushing the particle size to 60 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percent, and the industrial lime is crushed into 60 meshes; crushing common glass into 60 meshes in granularity;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 5000 grams of spent automobile catalyst, 200 grams of hematite, 40 grams of chemically pure tin dioxide powder, 60 grams of chemically pure antimony trioxide powder, 200 grams of metallurgical coke, 650 grams of lime and 300 grams of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly raising the temperature to 1550 ℃ at 170 ℃/h, and keeping the temperature for 90 minutes; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after the smelting is finished, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase from the metal phase, weighing the slag phase, and weighing 5850 g of slag;
D. sampling and analyzing slag: c, crushing the slag obtained in the step C to 40 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, wherein the content of palladium in the slag is 5.4ppm, the content of platinum in the slag is 1.86ppm, and the content of rhodium in the slag is 0.27 ppm; the recovery rate is calculated by the content of noble metals in the slag, the recovery rate of palladium is 99.47 percent, the recovery rate of platinum is 99.13 percent, the recovery rate of rhodium is 98.99 percent, and the total recovery rate of platinum, palladium and rhodium is 99.41 percent.
Example 4
The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the content of palladium is 1300ppm, the content of platinum is 340ppm, the content of rhodium is 150ppm, and the granularity of the catalyst is crushed to 120 meshes; the collector is hematite, Fe2O3The content of (b) is 70%, and the particle size is crushed to 80 meshes; the co-trapping agent is chemically pureTin dioxide and chemically pure antimony trioxide, both in powder form; the reducing agent is metallurgical coke, the content of C is 80%, and the granularity of the reducing agent is crushed to 60 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percent, and the industrial lime is crushed into 60 meshes; crushing common glass into 60 meshes in granularity;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 5000 grams of spent automobile catalyst, 250 grams of hematite, 60 grams of chemically pure tin dioxide powder, 40 grams of chemically pure antimony trioxide powder, 300 grams of metallurgical coke, 750 grams of lime and 350 grams of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly raising the temperature to 1550 ℃ at 170 ℃/h, and keeping the temperature for 90 minutes; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after smelting, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase and the metal phase, weighing the slag phase, and weighing 6050 g of slag;
D. sampling and analyzing slag: c, crushing the slag obtained in the step C to 40 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, and sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, wherein the content of palladium in the slag is 5.6ppm, the content of platinum in the slag is 1.98ppm, and the content of rhodium in the slag is 0.29 ppm; the recovery rate is calculated by the content of noble metals in the slag, the recovery rate of palladium is 99.48 percent, the recovery rate of platinum is 99.30 percent, the recovery rate of rhodium is 99.10 percent, and the total recovery rate of platinum, palladium and rhodium is 99.43 percent.
Example 5
The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the content of palladium is 1400ppm, the content of platinum is 550ppm, the content of rhodium is 300ppm, and the granularity of the catalyst is crushed to 150 meshes; the trapping agent is redIron ore, Fe2O3The content of (b) is 65%, and the particle size is crushed to 100 meshes; the synergistic trapping agent is chemically pure tin dioxide and chemically pure antimony trioxide which are both in powder form; the reducing agent is metallurgical coke, the content of C is 80 percent, and the granularity of the reducing agent is crushed to 80 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percent, and the industrial lime is crushed into 80 meshes in granularity; crushing common glass into 80 mesh;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 5000 grams of spent automobile catalyst, 400 grams of hematite, 80 grams of chemically pure tin dioxide powder, 70 grams of chemically pure antimony trioxide powder, 400 grams of metallurgical coke, 800 grams of lime and 400 grams of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly heating to 1600 ℃ at a speed of 180 ℃/h, and preserving heat for 120 minutes; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after smelting is finished, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase from the metal phase, weighing the slag phase, and weighing 6350 g of slag;
D. sampling and analyzing slag: c, crushing the slag obtained in the step C to 60 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, wherein the content of palladium in the slag is 5.8ppm, the content of platinum in the slag is 2.21ppm, and the content of rhodium in the slag is 0.33 ppm; the recovery rate is calculated by the content of noble metals in the slag, the recovery rate of palladium is 99.47 percent, the recovery rate of platinum is 99.49 percent, the recovery rate of rhodium is 99.50 percent, and the total recovery rate of platinum, palladium and rhodium is 99.48 percent.
Example 6
The method for synergistically recovering the noble metal from the spent automobile catalyst comprises the following steps of:
A. material preparation and treatment: the raw material is failure steamThe catalyst is prepared by crushing a catalyst carrier with the palladium content of 2000ppm, the platinum content of 600ppm and the rhodium content of 400ppm to 200 meshes; the collector is hematite, Fe2O3The content of (b) is 65%, and the particle size is crushed to 100 meshes; the synergistic trapping agent is chemically pure tin dioxide and chemically pure antimony trioxide which are both in powder form; the reducing agent is metallurgical coke, the content of C is 80%, and the granularity of the reducing agent is crushed to 100 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percent, and the industrial lime is crushed into 100 meshes; crushing common glass into 100 meshes in granularity;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 5000 grams of spent automobile catalyst, 500 grams of hematite, 150 grams of chemically pure tin dioxide powder, 100 grams of chemically pure antimony trioxide powder, 500 grams of metallurgical coke, 1000 grams of lime and 500 grams of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly heating to 1650 ℃ at a speed of 180 ℃/h, and preserving heat for 120 minutes; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after smelting, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase and the metal phase, weighing the slag phase, and weighing 6850 g of slag;
D. sampling and analyzing slag: c, crushing the slag obtained in the step C to 60 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, wherein the content of palladium in the slag is 6.0ppm, the content of platinum in the slag is 2.25ppm, and the content of rhodium in the slag is 0.35 ppm; the recovery rate is calculated by the content of noble metals in the slag, the recovery rate of palladium is 99.59 percent, the recovery rate of platinum is 99.49 percent, the recovery rate of rhodium is 99.70 percent, and the total recovery rate of platinum, palladium and rhodium is 99.57 percent.
Claims (2)
1. The method for synergistically recovering the noble metal from the spent automobile catalyst is characterized by comprising the following steps in sequence:
A. material preparation and treatment: the raw material is a spent automobile catalyst, the total content of platinum, palladium and rhodium is 1000-3000 ppm, and the particle size of the catalyst is crushed to 40-200 meshes; the collector is hematite, Fe2O3The content of the coarse powder is more than 60 percent, and the coarse powder is crushed into 40 to 100 meshes; the synergistic trapping agent is chemically pure tin dioxide and chemically pure antimony trioxide which are both in powder form; the reducing agent is metallurgical coke, the content of C is 80%, and the reducing agent is crushed into 20-100 meshes; the slag former is industrial lime and common glass, the CaO content in the industrial lime is 70 percent, and the industrial lime is crushed into 20 to 100 meshes; crushing common glass into 20-100 mesh;
B. material preparation and material mixing: b, mixing the materials obtained in the step A according to the mass parts: 100 parts of spent automobile catalyst, 2-10 parts of hematite, 1-5 parts of synergistic trapping agent, 1-10 parts of metallurgical coke, 10-20 parts of lime and 5-10 parts of common glass; putting all the materials into a mixer to be uniformly mixed;
C. smelting: b, putting the uniformly mixed material obtained in the step B into an intermediate frequency furnace graphite crucible; starting a power supply of the intermediate frequency furnace, slowly raising the temperature at 180 ℃/h within 150-; in the smelting process, the reducing agent metallurgical coke reduces the trapping agent ferric oxide, the synergistic trapping agent stannic oxide and antimony trioxide into metallic iron, tin and antimony, the noble metal is trapped by iron, and the tin or antimony assists the iron to trap the noble metal together; after smelting, turning off a power supply of the intermediate frequency furnace, pouring the molten material into a cast iron mold, layering a metal phase and a slag phase in the cast iron mold, cooling to room temperature, separating the slag phase from the metal phase, and weighing the slag phase;
D. sampling and analyzing slag: and C, crushing the slag obtained in the step C to 20-60 meshes, uniformly mixing, dividing, taking 200 g of slag, carrying out ball milling to 200 meshes, taking 10 g of slag sample, sending the slag sample to an analysis laboratory for analyzing the content of platinum, palladium and rhodium in the slag, and calculating the recovery rate of the noble metal according to the content of the noble metal in the slag.
2. The method for the synergistic recovery of noble metals from spent automotive catalysts according to claim 1, characterized in that the synergistic trapping agent is a mixture of tin dioxide and antimony trioxide in any ratio by mass.
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| CN109897971B (en) * | 2019-02-18 | 2021-02-02 | 西安交通大学 | Additive and method for extracting platinum group metal from radioactive glass solidified body |
| CN110184465B (en) * | 2019-05-31 | 2021-01-12 | 贵研资源（易门）有限公司 | Method for recovering rare and precious metals from spent automobile exhaust catalyst |
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| CN115418491B (en) * | 2022-09-21 | 2023-10-24 | 安徽工业大学 | Method for capturing platinum group metals by pyrometallurgy of bismuth base alloy |
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| GB295805A (en) * | 1927-07-07 | 1928-08-23 | Edgar Arthur Ashcroft | Improvements in the metallurgy of ores or materials containing tin and the extraction of metals or metal products therefrom |
| JP5077517B2 (en) * | 2006-06-20 | 2012-11-21 | 三菱マテリアル株式会社 | Precious metal recovery method and recovered precious metal |
| KR101226612B1 (en) * | 2012-04-24 | 2013-01-28 | 한국지질자원연구원 | A method for concentrating and recovering precious metals from spent mobile phone pcbs and spent auto-catalysts using waste nonferrous slag |
| CN106086416B (en) * | 2016-06-22 | 2018-07-13 | 江西自立环保科技有限公司 | A kind of technology that wiring board waste disposal utilizes |
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