CN113802015B - Trapping agent for recovering platinum group metals from waste catalyst and application thereof - Google Patents
Trapping agent for recovering platinum group metals from waste catalyst and application thereof Download PDFInfo
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- CN113802015B CN113802015B CN202110978895.6A CN202110978895A CN113802015B CN 113802015 B CN113802015 B CN 113802015B CN 202110978895 A CN202110978895 A CN 202110978895A CN 113802015 B CN113802015 B CN 113802015B
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- platinum group
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- tin
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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 discloses a trapping agent for recovering platinum group metals from waste catalysts and application thereof, belonging to the field of recycling of platinum group metals, wherein the trapping agent comprises copper, tin and nickel, and the content of Cu in the composition range of copper-tin-nickel alloy is as follows: sn: the molar ratio of Ni is (10-70): (30-80): (0-10), the invention utilizes copper, tin and nickel to form an alloy phase with the melting temperature of 600-900 ℃, and improves the recovery rate of platinum group metals; the trapping agent provided by the invention has the advantages of low smelting temperature (1000-1200 ℃), low equipment requirement, low energy consumption, low cost and the like, and is beneficial to industrial application. The copper of the invention is a commonly used trapping agent in industrial application, the tin and the nickel are also excellent trapping agents, the three alloy elements act synergistically, and the recovery rate of the obtained platinum group metal is more than 99.5%.
Description
Technical Field
The invention belongs to the field of recycling of platinum group metals, and relates to a trapping agent for recovering platinum group metals from waste catalysts and application thereof.
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.
At present, methods for recovering platinum group metals from 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 the carrier is achieved. 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 smelting process has great treating capacity, high recovering efficiency and other advantagesBecome the hotspot of research. Chinese invention patent (CN 201510797358.6) discloses that nickel matte is used as a collector, calcium oxide and silicon dioxide are used as slag formers, and platinum group metals in waste catalysts are melted and collected at 1400-1450 ℃, wherein nickel is toxic heavy metal and SO is generated in the melting process 2 A gas.
Chinese invention patent (CN 201710856842.0) discloses a method for collecting uranium group metals by microwave heating and melting, wherein Ni is used as a raw material 3 S 2 Adding 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 at 1050-1200 ℃ by microwave 2 Is a toxic gas and has certain environmental risks.
The Chinese invention patent (CN 201811156196.8) discloses a method for recycling waste circuit boards and automobile exhaust waste catalysts in a synergic mode, which is essentially characterized in that copper is adopted to collect platinum group metals in the waste catalysts, the recovery rate exceeds 98%, and the dangers of serious heavy metal pollution and dioxin emission exist.
Chinese invention patent (CN 201911145745.6) discloses a method for recovering platinum group metals from VOCs waste catalysts, and particularly FeS 2 As a collecting 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 collecting effect is good, but SO is generated 2 Large amount of gas and slag and the like.
Chinese invention patent (CN 103014352A) discloses a method for extracting platinum group metal from alumina carrier petrochemical catalyst by smelting, iron and copper are used as collectors, sodium salt is used as slag former, platinum group metal in alumina carrier petrochemical catalyst is collected at 1100-1450 ℃, the patent can avoid the generation of ferrosilicon alloy, but the sodium salt is seriously corroded to smelting furnace lining, and the collection effect is to be examined.
Disclosure of Invention
The invention aims to provide a trapping agent for recovering platinum group metals from waste catalysts and application thereof, aiming at the technical problems of high reagent consumption, difficulty in treating wastewater, heavy metal pollution caused by a nickel-lead trapping method in pyrogenic smelting and high temperature and energy consumption caused by a high-temperature iron trapping method in a wet method for recovering the platinum group metals from the alumina-based waste catalysts in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a trapping agent for recovering platinum group metals from waste catalysts by low-temperature smelting comprises copper, tin and nickel, wherein the trapping agent comprises the following components in the composition range of Cu: sn: the molar ratio of Ni is (10-70): (30-80): (0-10).
Further, the copper is one or more of copper powder, copper oxide and copper concentrate; the tin is one or more of tin powder, tin oxide and tin concentrate; the nickel is one or more of nickel powder, nickel oxide and nickel concentrate.
Further, the waste catalyst is a waste catalyst containing platinum group metal.
The invention also provides application of the trapping agent for recovering platinum group metals from the waste catalyst by low-temperature smelting, the waste catalyst, the trapping agent, the slagging flux and the reducing agent are uniformly mixed according to a set proportion, the uniformly mixed materials are subjected to low-temperature smelting, after reaction for preset time, a slag phase floats on the surface of an alloy liquid phase, and slag-gold separation is carried out to obtain the alloy containing the platinum group metals.
Further, the temperature of the low-temperature smelting is 1000-1200 ℃.
Further, the mass ratio of the waste catalyst to the trapping agent is 1: (0.2-0.5).
Further, the slagging flux comprises one or more of calcium oxide, magnesium oxide, calcium fluoride and borax.
Further, the reducing agent is one or more of coke, carbon powder, graphite and coal powder.
The invention has the advantages that:
according to the characteristics that a Cu-Sn and Cu-Sn-Ni phase diagram shows that tin, nickel and copper can form a eutectic point, the alloy composition is optimized, copper, tin and nickel can form an alloy phase with the melting temperature of 600-900 ℃, and copper, tin and nickel are all good trapping agents, so that the synergistic effect can be played, and the recovery rate of platinum group metals is improved.
The trapping agent provided by the invention has the advantages of low smelting temperature (1000-1200 ℃), low equipment requirement, low energy consumption, low cost and the like, and is beneficial to industrial application. The copper of the invention is a commonly used trapping agent in industrial application, the tin and the nickel are also excellent trapping agents, the three alloy elements act synergistically, and the recovery rate of the obtained platinum group metal is more than 99.5%.
Drawings
FIG. 1 is a process of using the collector for recovering platinum group metals from a spent catalyst 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.
In the examples of the present invention, the used catalyst had the following main components: (C content 2.6wt%, al) 2 O 3 The content was 96.8w%, the Pt content was 4430 g/t)
Example 1
Copper powder and tin powder were prepared as a collector according to 70 parts by weight of 30, and 100 parts of a platinum group metal-containing spent catalyst was added with a slag-forming flux to control the composition of slag (Al) 2 O 3 ＝38％、CaO＝43％、B 2 O 3 And = 19%), 30 parts of trapping agent and 10 parts of graphite powder are mixed uniformly according to a proportion and then smelted in a smelting furnace, the smelting temperature is 1000 ℃, after 5 hours of reaction, slag is observed to float on the surface of an alloy phase, the copper-based multi-metal alloy containing platinum group metal is obtained by separating the slag phase from the alloy, and the recovery rate of the platinum group metal is detected to be more than 99.5%.
Example 2
Copper powder, tin oxide and nickel oxide are prepared into a trapping agent according to the ratio of 60 2 O 3 ＝45％、CaO＝33％、B 2 O 3 = 22%), 25 parts of trapping agent and 15 parts of graphite powder are mixed uniformly according to the proportion and then smelted in a smelting furnace at the smelting temperatureAnd (3) reacting at the temperature of 1100 ℃ for 5 hours, observing that slag floats on the surface of an alloy phase, separating the slag phase from the alloy to obtain the copper-based multi-metal alloy containing the platinum group metal, and detecting that the recovery rate of the platinum group metal is more than 99.5%.
Example 3
Copper powder, tin powder and nickel powder are prepared into a trapping agent according to the ratio of 50 2 O 3 ＝45％、CaO＝35％、B 2 O 3 And the recovery rate of the platinum group metal is detected to be more than 99.5 percent.
Example 4
Copper powder, tin powder and nickel powder are prepared into a trapping agent according to the proportion of 40 2 O 3 ＝31％、CaO＝39％、B 2 O 3 And = 30%), 25% of trapping agent and 10% of graphite powder are mixed uniformly in proportion and then smelted in a smelting furnace, the smelting temperature is 1150 ℃, after 5 hours of reaction, slag floating on the surface of an alloy phase is observed, a copper-based multi-metal alloy containing platinum group metal is obtained through separation of the slag phase and the alloy, and the recovery rate of the platinum group metal is higher than 99.5% through detection.
Example 5
Copper powder, tin powder and nickel oxide were prepared as a collector according to a 30 2 O 3 ＝46％、CaO＝35％、B 2 O 3 ＝10％、 9％CaF 2 ) 20 parts of trapping agent and 12 parts of graphite powder are mixed uniformly according to a certain proportion and then smelted in a smelting furnace, the smelting temperature is 1100 ℃, after 5 hours of reaction, slag is observed to float on the surface of an alloy phase, the copper-based multi-metal alloy containing platinum group metal is obtained by separating the slag phase from the alloy, and the recovery rate of the platinum group metal is detected to be more than 99.5%.
Comparative example
(1) Copper oxide is used as a trapping agent;
(2) 100 parts of platinum group metal-containing waste catalyst is added with a slagging flux to control the composition of molten slag (the alkalinity is 1.0, al) 2 O 3 Mixing 40 parts of trapping agent and 10 parts of graphite powder in proportion, smelting in a smelting furnace at 1450 ℃, observing that slag floats on the surface of an alloy phase after reacting for 5 hours, and separating the slag phase from the alloy to obtain the copper-based alloy containing platinum group metal;
(3) And recovering the obtained alloy containing the platinum group metal, and performing acidolysis, separation and purification treatment to obtain the platinum group metal, wherein the recovery rate of the platinum group metal is 96.2% by detection.
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 (5)
1. The application of the trapping agent for recovering platinum group metals from the waste catalyst is characterized in that the waste catalyst, the trapping agent, a slagging flux and a reducing agent are uniformly mixed according to a set proportion, the uniformly mixed materials are smelted at a low temperature, after reaction for a preset time, a slag phase floats on the surface of an alloy liquid phase, and the slag-gold is separated to obtain an alloy containing the platinum group metals;
the collector comprises copper, tin and nickel, and the copper-tin-nickel alloy comprises the following components in percentage by weight: sn: the molar ratio of Ni is (10-70): (30-80): (0-10) preparation;
the low-temperature smelting temperature is 1000-1100 ℃;
the mass ratio of the waste catalyst to the trapping agent is 1: (0.2-0.5).
2. The use of the collector according to claim 1, wherein the copper is one or more of copper powder, copper oxide, and copper concentrate.
3. The use of the collector according to claim 1, wherein the tin is one or more of tin powder, tin oxide, and tin concentrate.
4. The use of the collector according to claim 1, wherein the nickel is one or more of nickel powder, nickel oxide, and nickel concentrate.
5. Use of a collector according to claim 1, wherein the spent catalyst is a spent catalyst comprising a platinum group metal.
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| CN1311090C (en) * | 2005-08-23 | 2007-04-18 | 云锡元江镍业有限责任公司 | Bessemer matte production method using nickel sulfide materials |
| GB2465603B (en) * | 2008-11-24 | 2010-10-13 | Tetronics Ltd | Method for recovery of metals |
| CN101629241B (en) * | 2009-08-04 | 2011-02-16 | 齐大全 | Method for extracting noble metals from circuit boards by using lead, tin and alloys of lead and tin as capturing agents |
| CN105861851A (en) * | 2015-01-21 | 2016-08-17 | 昆明冶金高等专科学校 | Method for enriching platinum group metal secondary resource with high efficiency |
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