CN113802014A - Method for recovering platinum group metal in alumina-based waste catalyst by pyrogenic process - Google Patents
Method for recovering platinum group metal in alumina-based waste catalyst by pyrogenic process Download PDFInfo
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- CN113802014A CN113802014A CN202110978732.8A CN202110978732A CN113802014A CN 113802014 A CN113802014 A CN 113802014A CN 202110978732 A CN202110978732 A CN 202110978732A CN 113802014 A CN113802014 A CN 113802014A
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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
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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
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- 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 platinum group metals in an alumina-based waste catalyst by a pyrogenic process, which belongs to the field of platinum group metal recovery, wherein a metal trapping agent, the alumina-based waste catalyst, a magnesium-containing flux, a manganese-containing flux and a reducing agent are mixed and smelted according to a set proportion, the smelting temperature is 1200-1350 ℃, and molten metal and furnace slag containing the platinum group metals are obtained after solid-liquid separation; controlling a slag system (Al) during smelting2O3+ MgO + MnO) of Al2O3The content ranges from 45 to 65 wt%, the MgO content ranges from 5 to 30 wt%, and the MnO content ranges from 10 to 55 wt%; recovering the obtained metal liquid containing the platinum group metal to obtain the platinum group metal; the slag system provided by the invention can realize the high-efficiency recovery of platinum group metals, and has the advantages of low smelting temperature, low energy consumption and little environmental pollution.
Description
Technical Field
The invention belongs to the field of platinum group metal recycling, and particularly relates to a method for recovering platinum group metals in an alumina-based waste catalyst by a pyrogenic process.
Background
The platinum group metal has excellent physical and chemical properties such as high stability, high temperature resistance, good catalytic activity and the like, and is widely applied to the fields of automobiles, petroleum, chemical engineering, aerospace and the like. But the platinum group metal reserves are small, the use amount is large, the external dependence is high, and the contradiction between supply and demand is very prominent. How to realize the high-efficiency recovery of platinum group metals from waste catalysts is a critical technology which needs to be solved urgently. Al of aluminium-based waste catalyst with high melting point2O3The conventional slag mold is a carrier, has high melting point and large slag amount, and finally causes low recovery rate of platinum group metals by adopting iron to capture and generate indissolvable ferrosilicon alloy.
At present, methods for recovering platinum group metals in aluminum-based waste catalysts include wet methods and pyrogenic methods, wherein wet dissolution is mainly used, i.e., the platinum group metals are dissolved by various oxidants in an acidic environment, so that the effect of separating the platinum group metals from a carrier is realized. However, the wet process generates a large amount of wastewater, and toxic gas is easily generated in the process of dissolving platinum group metals, so that the environmental pollution is serious.
The pyrometallurgical process, i.e. high-temperature smelting metal trapping method, such as copper trapping method and iron trapping method, is characterized by that according to the composition of platinum group metal catalyst carrier, the trapping agent of copper oxide and iron oxide, slag-forming agent and reducing agent are added to make high-temperature smelting, and the metal platinum group metal is trapped by utilizing molten metal copper and iron, etc. to form alloy, and then the alloy and carrier are fed into slag phase so as to implement effective enrichment recovery of platinum group metal. The process has the advantages of high comprehensive recovery rate, simple method, short period, cleanness, environmental protection, easy large-scale production and the like. The companies such as noble metals in Japan, Youmei and the like have already been industrially applied to the recovery of platinum group metals by a high-temperature metal-melting capture method, are widely used for the recovery of various platinum group metal wastes, preempt the market in the aspect of efficient recovery of platinum group metal secondary resources, but have strict and confidential process parameters and realize technical monopoly. The pyrometallurgical smelting enrichment method has the advantages of large treatment capacity, high recovery efficiency and the like, and becomes a research hotspot.
Chinese invention patent (CN 201510797358.6) discloses that nickel matte is used as a trapping agent, calcium oxide and silicon dioxide are used as slag formers, and platinum group metals in waste catalysts are trapped by melting at the temperature of 1400 ℃ and 1450 ℃, wherein nickel is toxic heavy metal and SO is generated in the melting process2A gas.
Chinese invention patent (CN 201710856842.0) discloses a method for collecting platinum group metals by microwave heating and melting, and Ni is used3S2Adding at least one of borax, sodium carbonate, sodium bicarbonate, sodium hydroxide, sodium peroxide and methyl cellulose as a trapping agent for slagging, and trapping platinum group metals in the waste catalyst by microwaves at 1050-1200 ℃2Is a toxic gas and has certain environmental risks.
The Chinese invention patent (CN 201811156196.8) discloses a method for synergistically recycling a waste circuit board and an automobile exhaust waste catalyst, which is essentially to adopt copper to trap platinum group metals in the waste catalyst, the recovery rate exceeds 98 percent, and the dangers of serious heavy metal pollution and dioxin emission exist.
Chinese patent (CN 201911145745.6) discloses a method for recovering platinum group metals from VOCs waste catalysts, in particular to FeS2As a trapping agent, calcium oxide, sodium carbonate, calcium fluoride, borax and the like are added as slag formers, the smelting temperature is 1000-1700 ℃, the platinum group metal trapping effect is good, but SO is generated2Large amount of gas and slag and the like.
The Chinese invention patent (CN 103014352A) discloses a method for smelting and extracting platinum group metal from an alumina carrier petrochemical catalyst, which takes iron and copper as collectors and sodium salt as a slagging agent to collect the platinum group metal in the alumina carrier petrochemical catalyst at 1100-1450 ℃.
Chinese patent (CN112011696A) discloses a method for enriching platinum group metals in aluminum-based waste catalyst by pyrogenic process, which adopts CaO-Al2O3-Fe2O3-B2O3The slag system is smelted, the smelting temperature is 1500-1800 ℃, the smelting temperature is high, and the energy consumption is high.
Disclosure of Invention
The invention aims to provide a method for recovering platinum group metals from alumina-based waste catalysts by a pyrogenic process, aiming at the technical problems of high reagent consumption, difficulty in treating wastewater, heavy metal pollution caused by a nickel-lead capture method in pyrogenic process smelting and high temperature and energy consumption caused by a high-temperature iron capture method in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for recovering platinum group metals in alumina-based waste catalysts by a pyrogenic process comprises the following steps:
(1) mixing and smelting a metal trapping agent, an alumina-based waste catalyst, a magnesium-containing flux, a manganese-containing flux and a reducing agent according to a set proportion, wherein the smelting temperature is 1200-1350 ℃, and obtaining molten metal containing platinum group metals and furnace slag after slag-gold separation;
controlling a slag system (Al) during smelting2O3+ MgO + MnO) of Al2O3The content ranges from 45 to 65 wt%, the MgO content ranges from 5 to 30 wt%, and the MnO content ranges from 10 to 55 wt%;
(2) and recovering the platinum group metal from the obtained metal liquid containing the platinum group metal.
Further, Al in the slag2O3The sum of the contents of MgO and MnO is more than or equal to 90 wt%.
Further, the viscosity of the slag at 1200-1350 ℃ is not more than 1.0 Pa.s.
Further, the magnesium-containing flux comprises one or more of magnesium oxide, magnesium carbonate and magnesite.
Further, the manganese-containing flux comprises one or more of manganese oxide, manganese carbonate and pyrolusite.
Further, the metal collector comprises one or more of iron, copper, nickel, antimony, lead and alloys thereof.
Further, the alumina-based waste catalyst is a waste catalyst containing platinum group metal and taking alumina as a carrier.
Further, the reducing agent is one or more of coke, carbon powder, graphite and coal powder.
The principle of the invention is as follows:
the technical and economic indicators of the pyrometallurgical high-temperature smelting process are closely related to the properties of the smelting slag, such as melting temperature, pH value, viscosity, surface (interface) tension and density and platinum group metal distribution coefficient. The slag with proper viscosity at lower melting temperature can promote platinum group metals to enter the alloy for trapping, so that the platinum group metals can be efficiently recovered. According to the invention, MgO-Al2O3The ternary-MnO phase diagram has the characteristic that ternary eutectic reaction occurs at about 1172 ℃, a large melting temperature area lower than 1350 ℃ is arranged in the phase diagram, a slag phase with a low melting temperature can be formed, the viscosity is proper at 1200-1350 ℃, the fluidity is good, and the platinum group metal can migrate into the trapping alloy.
Compared with the prior art, the invention has the advantages that:
(1) the MgO-Al provided by the invention2O3A slag system of MnO based, SiO-free2Can solve the problem of the conventional SiO-containing2The difficult problem of forming ferrosilicon alloy by capturing slag system high-temperature iron is favorable for recovering platinum group metals, and the recovery rate of the platinum group metals is more than 99.5 percent.
(2) CaO-Al provided by the invention2O3the-MnO slag system has the advantages of lower melting temperature, low energy consumption, less magnesium-manganese fluxing agent added in the slagging process, less slag amount and environmental protection.
(3) The fluxing agent containing magnesium and manganese used for slagging is cheaper than borax and sodium salt, has low cost and good economic benefit, keeps a proper viscosity range, reduces the erosion effect on a furnace lining, and prolongs the service life of the smelting furnace.
Drawings
FIG. 1 is a flow chart of a method for pyrogenically recovering platinum group metals from alumina-based spent catalysts according to the present invention.
Detailed Description
The following examples further illustrate embodiments of the present invention, but the embodiments of the present invention are not limited to the following examples.
Example 1
The invention relates to a method for recovering platinum group metals in alumina-based waste catalysts by a pyrogenic process, which comprises the following steps:
(1) mixing and smelting an iron trapping agent, an alumina-based platinum-containing catalyst, a magnesium-containing flux (magnesium oxide), a manganese-containing flux (manganese oxide) and a reducing agent (graphite) according to a set proportion, adding the mixture into an electric furnace according to the formula (Al)2O353 percent, 17 percent of MgO and 30 percent of MnO) are respectively added with magnesia and manganese oxide for slagging, the smelting temperature is 1200 ℃, the smelting time is 120min, and molten iron and slag containing platinum group metals are obtained by separation;
(2) the obtained molten iron containing platinum group metals is dissolved in acid such as hydrochloric acid (sulfuric acid or nitric acid), and then the platinum group metals can be recovered by separation and purification, and the final recovery rate of Pt is 99.6%.
Example 2
The invention relates to a method for recovering platinum group metals in alumina-based waste catalysts by a pyrogenic process, which comprises the following steps:
(1) mixing and smelting an iron trapping agent, an alumina-based platinum-rhenium catalyst, a magnesium-containing flux (magnesium carbonate), a manganese-containing flux (pyrolusite) and a reducing agent (graphite) according to a set proportion, adding the mixture into an electric furnace, and smelting according to the formula (Al)2O345 percent, 5 percent of MgO and 55 percent of MnO) are respectively added with manganese oxide for slagging, the smelting temperature is 1300 ℃, the smelting time is 120min, and molten iron and slag containing platinum group metals are obtained by separation;
(2) after the obtained molten iron containing the platinum group metals is dissolved by acid such as hydrochloric acid (sulfuric acid or nitric acid), the platinum group metals can be recovered by separation and purification, and finally the recovery rates of Pt and Re are 99.7 percent and 99.9 percent.
Example 3
The invention relates to a method for recovering platinum group metals in alumina-based waste catalysts by a pyrogenic process, which comprises the following steps:
(1) copper trapping agent, alumina-based platinum-iridium-containing catalyst, magnesium-containing flux (magnesite), copper-containing catalyst, magnesium-containing flux (magnesite), copper-containing catalyst, and magnesium-containing catalystManganese fusing agent (manganese carbonate) and reducing agent (graphite) are mixed and smelted according to a set proportion, added into an electric furnace according to the proportion of (Al)2O365 percent, 25 percent of MgO and 10 percent of MnO) are respectively added with magnesium oxide and manganese carbonate for slagging, the smelting temperature is 1350 ℃, the smelting time is 120min, and the metal phase containing platinum group metal and the slag are obtained by separation;
(2) the obtained metal phase containing the platinum group metal is dissolved by acid such as hydrochloric acid (sulfuric acid or nitric acid), and the platinum group metal can be recovered by separation and purification, and finally the recovery rates of Pt and Ir are 99.6% and 99.8%.
Example 4
The invention relates to a method for recovering platinum group metals in alumina-based waste catalysts by a pyrogenic process, which comprises the following steps:
(1) mixing and smelting a copper trapping agent, an alumina-based palladium-containing catalyst, a magnesium-containing flux (magnesium oxide), a manganese-containing flux (manganese carbonate) and a reducing agent (graphite) according to a set proportion, adding the mixture into an electric furnace, and smelting according to the formula (Al)2O358 percent, 22 percent of MgO and 20 percent of MnO) are respectively added with magnesium carbonate and manganese oxide for slagging, the smelting temperature is 1250 ℃, the smelting time is 120min, and the metal phase containing platinum group metal and the slag are obtained by separation;
(2) the obtained metal phase containing the platinum group metal is dissolved by acid such as hydrochloric acid (sulfuric acid or nitric acid), and then the platinum group metal can be recovered by separation and purification, and the final recovery rate of Pd is 99.7%.
Comparative example
(1) Copper trapping agent, alumina-based platinum-containing catalyst, MgO and SiO2CaO and a reducing agent (graphite) are mixed and smelted according to a set proportion and added into an electric furnace according to the formula (Al)2O3＝25％，MgO＝10％，CaO/SiO21.0) slagging, wherein the smelting temperature is 1450 ℃, the smelting time is 5h, and the metal phase containing platinum group metal and the furnace slag are obtained through separation;
(2) the obtained metal phase containing the platinum group metal is dissolved by acid such as hydrochloric acid (sulfuric acid or nitric acid), and then the platinum group metal can be recovered by separation and purification, and the final recovery rate of Pt is 97.1%.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Claims (8)
1. A method for recovering platinum group metals in alumina-based waste catalysts by a pyrogenic process is characterized by comprising the following steps:
(1) mixing and smelting a metal trapping agent, an alumina-based waste catalyst, a magnesium-containing flux, a manganese-containing flux and a reducing agent according to a set proportion, wherein the smelting temperature is 1200-1350 ℃, and obtaining molten metal containing platinum group metals and furnace slag after slag-gold separation;
controlling a slag system (Al) during smelting2O3+ MgO + MnO) of Al2O3The content ranges from 45 to 65 wt%, the MgO content ranges from 5 to 30 wt%, and the MnO content ranges from 10 to 55 wt%;
(2) and recovering the platinum group metal from the obtained metal liquid containing the platinum group metal.
2. The method for the pyrometallurgical recovery of platinum group metals from alumina-based spent catalysts according to claim 1, wherein Al in the slag is2O3The sum of the contents of MgO and MnO is more than or equal to 90 wt%.
3. The method for pyrometallurgical recovery of platinum group metals from alumina-based spent catalysts according to claim 1, wherein the viscosity of the slag at 1200 to 1350 ℃ is not more than 1.0 pa.s.
4. The method for recovering platinum group metals in the alumina-based waste catalyst by the pyrogenic process according to any one of claims 1 to 3, wherein the magnesium-containing flux comprises one or more of magnesium oxide, magnesium carbonate and magnesite.
5. The method for pyrogenically recovering a platinum group metal from an alumina-based spent catalyst according to any one of claims 1 to 3, wherein the manganese-containing flux comprises one or more of manganese oxide, manganese carbonate, pyrolusite.
6. The method for recovering the platinum group metal in the alumina-based waste catalyst by the pyrogenic process according to any one of claims 1 to 3, wherein the metal trapping agent comprises one or more of iron, copper, nickel, antimony, lead and alloys thereof.
7. The method for recovering the platinum group metal in the alumina-based waste catalyst according to any one of claims 1 to 3, wherein the alumina-based waste catalyst is a waste catalyst containing the platinum group metal and taking alumina as a carrier.
8. The method for recovering the platinum group metal in the alumina-based waste catalyst by the pyrogenic process according to any one of claims 1 to 3, wherein the reducing agent is one or more of coke, carbon powder, graphite and coal powder.
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Cited By (8)
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| CN113684372A (en) * | 2021-07-29 | 2021-11-23 | 昆明贵研新材料科技有限公司 | Method for recovering platinum group metal from spent automobile catalyst |
| CN114892018A (en) * | 2022-05-19 | 2022-08-12 | 广东先导稀材股份有限公司 | Method for separating and recovering platinum and manganese in platinum-manganese alloy |
| CN115161479A (en) * | 2022-04-29 | 2022-10-11 | 重庆大学 | Method for preparing Ti-Al-Si alloy by using waste denitration catalyst |
| CN115323188A (en) * | 2022-07-27 | 2022-11-11 | 中南大学 | Method for trapping platinum group metal in spent catalyst by copper |
| CN115433835A (en) * | 2022-09-02 | 2022-12-06 | 昆明理工大学 | Method for simultaneously recovering precious metals in automobile waste catalyst and preparing high-purity antimony |
| CN115612858A (en) * | 2022-08-22 | 2023-01-17 | 中南大学 | Method for trapping platinum group metals in PGM secondary resources by repeatedly discharging residues |
| CN115612859A (en) * | 2022-10-28 | 2023-01-17 | 安徽工业大学 | Method for trapping platinum group metal in waste catalyst by bismuth |
| CN117070760A (en) * | 2023-08-08 | 2023-11-17 | 横峰县凯怡实业有限公司 | Composition for preparing platinum group metal, application of composition and method for preparing platinum group metal |
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| CN115612859A (en) * | 2022-10-28 | 2023-01-17 | 安徽工业大学 | Method for trapping platinum group metal in waste catalyst by bismuth |
| CN115612859B (en) * | 2022-10-28 | 2024-02-09 | 安徽工业大学 | Method for trapping platinum group metals in waste catalyst by bismuth |
| CN117070760A (en) * | 2023-08-08 | 2023-11-17 | 横峰县凯怡实业有限公司 | Composition for preparing platinum group metal, application of composition and method for preparing platinum group metal |
| CN117070760B (en) * | 2023-08-08 | 2024-05-03 | 横峰县凯怡实业有限公司 | Composition for preparing platinum group metal, application of composition and method for preparing platinum group metal |
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