CN113737013B - Method for low-temperature trapping and recovering platinum group metal in waste catalyst - Google Patents
Method for low-temperature trapping and recovering platinum group metal in waste catalyst Download PDFInfo
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- CN113737013B CN113737013B CN202110978883.3A CN202110978883A CN113737013B CN 113737013 B CN113737013 B CN 113737013B CN 202110978883 A CN202110978883 A CN 202110978883A CN 113737013 B CN113737013 B CN 113737013B
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- C—CHEMISTRY; METALLURGY
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- 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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- 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
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
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Abstract
The invention discloses a method for low-temperature trapping and recovering platinum group metals in waste catalysts, which comprises the steps of firstly preparing copper and antimony into a platinum group metal trapping agent according to the element molar ratio of 1 (0.2-1), and uniformly mixing the waste catalysts, a slagging flux, the trapping agent and a reducing agent according to a preset proportion; smelting the mixed material at 1000-1200 deg.c, setting the reaction time, floating the slag on the surface of the alloy phase, and separating the slag phase from the alloy phase to obtain Cu-Sb alloy phase containing Pt group metal; and recovering the obtained platinum group metal-containing copper-antimony alloy phase to obtain the platinum group metal. The method utilizes the multi-metal synergistic trapping, the recovery rate of the platinum group metal is high, and the copper and the antimony can form low-melting-point alloy with the melting temperature lower than 700 ℃, so that the melting temperature is reduced. The invention has the advantages of low energy consumption, low cost, high recovery rate and the like, and is beneficial to industrial application.
Description
Technical Field
The invention belongs to the field of platinum group metal recovery, and relates to a method for low-temperature trapping and recovering platinum group metals in a waste catalyst.
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 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 a method for collecting platinum group metals in waste catalysts by melting at 1400-1450 ℃ by taking nickel matte as a collecting agent and calcium oxide and silicon dioxide as a slagging agent, wherein nickel is a toxic heavy metal and SO is generated in the melting process 2 A gas.
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 constituent to collect the platinum group metal in the alumina carrier petrochemical catalyst at 1100-1450 ℃.
Chinese invention patent (CN 112011696A) discloses a method for pyrogenically enriching platinum group metal in aluminum-based waste catalyst, which adopts CaO-Al 2 O 3 -Fe 2 O 3 -B 2 O 3 The slag system is smelted, the smelting temperature is 1500-1800 ℃, the smelting temperature is high, and the energy consumption is high.
Disclosure of Invention
Aiming at the technical problems of high reagent consumption, difficult wastewater treatment, heavy metal pollution caused by a nickel-lead trapping method in pyrometallurgical smelting and high temperature and energy consumption caused by a high-temperature iron trapping method in the wet method for recovering platinum group metals from waste catalysts in the prior art, the invention aims to provide a method for low-temperature trapping and recovering platinum group metals from waste catalysts.
In order to achieve the purpose, the invention provides the following technical scheme: a method for low-temperature trapping and recovering platinum group metals in waste catalysts comprises the following steps:
(1) Copper and antimony are prepared into a platinum group metal trapping agent according to the element molar ratio of 1 (0.2-1), and the waste catalyst, the slagging flux, the trapping agent and the reducing agent are uniformly mixed according to a preset proportion;
(2) Smelting the mixed material at 1000-1200 deg.c, setting the reaction time and floating slag on the surface of the alloy phase, and separating slag phase from alloy phase to obtain Cu-Sb alloy phase containing Pt group metal;
(3) And recovering the obtained copper-antimony alloy phase containing the platinum group metal, and carrying out acidolysis, separation and purification treatment to obtain the platinum group metal.
Further, the copper is one or more of copper powder, copper oxide and copper concentrate; the antimony is one or more of antimony metal powder, antimony oxide and antimony concentrate.
Further, the waste catalyst is a waste catalyst containing platinum group metal.
Furthermore, the mass ratio of the waste catalyst to the trapping agent is 1 (0.1-0.4).
Further, the reducing agent is any one or more of coke, carbon powder, graphite and coal powder.
Further, the slagging flux comprises one or more of calcium oxide, magnesium oxide, calcium fluoride and borax.
Further, the smelting temperature is 1000-1100 ℃.
The invention has the advantages that:
according to a Cu-Sb phase diagram, the fact that copper and antimony can form an alloy with a low melting point can be found, the alloy with the melting temperature lower than 700 ℃ can be obtained after the composition is optimized, the copper-antimony alloy with the low melting temperature is used as a trapping agent, slag with low melting temperature and good fluidity is selected, the smelting temperature is favorably reduced, the energy consumption and the production cost are reduced, platinum group metals are more easily dissolved, the trapping capacity is stronger, the requirements on equipment and refractory materials are reduced, the industrial application is favorably realized, the recovery rate of the obtained platinum group metals is more than 99.5%, and the recovery rate of the platinum group metals is high.
Drawings
FIG. 1 is a process flow diagram of 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 96.8wt% Pt content 4430 g/t)
Example 1
A method for low-temperature trapping and recovering platinum group metals in waste catalysts comprises the following steps:
(1) Copper powder and antimony oxide are prepared into a trapping agent according to the ratio of 1;
(2) 100 parts of platinum group metal-containing waste catalyst, 15 parts of trapping agent and 10 parts of graphite powder are mixed uniformly according to a certain proportion and then smelted in a smelting furnace, and a slagging flux is added to control the composition of molten slag (Al) 2 O 3 ＝45％、CaO＝33％、B 2 O 3 = 22%), the smelting temperature is 1200 ℃, after the full reaction, the slag is observed to float on the surface of the alloy phase, and the copper-antimony alloy containing platinum group metal is obtained by separating the slag phase from the alloy;
(3) And recovering the obtained copper-antimony alloy phase containing the platinum group metal, carrying out acidolysis, separation and purification treatment to obtain the platinum group metal, wherein the recovery rate of the platinum group metal is more than 99.5% by detection.
Example 2
A method for low-temperature trapping and recovering platinum group metals in waste catalysts comprises the following steps:
(1) Copper powder and antimony powder are prepared into a trapping agent according to 1:1;
(2) 100 parts of platinum group metal-containing waste catalyst, 30 parts of trapping agent and 10 parts of graphite powder are mixed uniformly according to a certain proportion and then smelted in a smelting furnace, and a slagging flux is added to control the composition of molten slag (Al) 2 O 3 ＝38％、CaO＝43％、B 2 O 3 = 19%), the smelting temperature is 1000 ℃, after the full reaction, the slag is observed to float on the surface of the alloy phase, and the copper-antimony alloy containing platinum group metal is obtained by separating the slag phase from the alloy;
(3) And recovering the obtained copper-antimony alloy phase containing the platinum group metal, carrying out acidolysis, separation and purification treatment to obtain the platinum group metal, wherein the recovery rate of the platinum group metal is more than 99.5% by detection.
Example 3
A method for low-temperature trapping and recovering platinum group metals in waste catalysts comprises the following steps:
(1) Copper powder and antimony powder are prepared into a trapping agent according to the ratio of 1.5;
(2) 100 parts of platinum group metal-containing waste catalyst, 15 parts of trapping agent and 10 parts of graphite powder are mixed uniformly according to a certain proportion and then smelted in a smelting furnace, and a slagging flux is added to control the composition of molten slag (Al) 2 O 3 ＝46％、CaO＝36％、B 2 O 3 = 18%), the smelting temperature is 1100 ℃, after full reaction, the slag is observed to float on the surface of the alloy phase, and the copper-antimony alloy containing platinum group metal is obtained by separating the slag phase from the alloy;
(3) And recovering the obtained copper-antimony alloy phase containing the platinum group metal, carrying out acidolysis, separation and purification treatment to obtain the platinum group metal, wherein the recovery rate of the platinum group metal is more than 99.5% by detection.
Example 4
A method for low-temperature trapping and recovering platinum group metals in a waste catalyst comprises the following steps:
(1) Copper powder and antimony powder are prepared into a trapping agent according to the ratio of 1.8;
(2) Mixing 100 parts of platinum group metal-containing waste catalyst, 10 parts of trapping agent and 10 parts of graphite powder in proportion, smelting in a smelting furnace, and adding a slagging flux to control the composition of molten slag (Al) 2 O 3 ＝45％、CaO＝35％、B 2 O 3 ＝10％、10CaF 2 ) The smelting temperature is 1100 ℃, after full reaction, slag is observed to float on the surface of an alloy phase, and the copper-antimony alloy containing platinum group metal is obtained by separating the slag phase from the alloy;
(3) And recovering the obtained copper-antimony alloy phase 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 more than 99.5% through detection.
Comparative example
(1) Copper oxide is used as a trapping agent;
(2) 100 parts of platinum group metal-containing waste catalyst, 40 parts of trapping agent and 10 parts of graphite powder are mixed uniformly according to a certain proportion and then smelted in a smelting furnace, and a slagging flux is added to control the composition of molten slag (Al) 2 O 3 CaO/SiO in alkalinity of 25 =25% 2 1.0), smelting temperature 1450 ℃, reacting for 5 hours, observing that slag floats on the surface of an alloy phase, and separating the slag phase from the alloy to obtain a 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. It will be apparent to those skilled in the art that various modifications and variations can be made without departing from the spirit of the invention.
Claims (5)
1. A method for low-temperature trapping and recovering platinum group metals in waste catalysts is characterized by comprising the following steps:
(1) Copper and antimony are prepared into a platinum group metal trapping agent according to the element molar ratio of 1 (0.2-1), and the waste catalyst, the slagging flux, the trapping agent and the reducing agent are uniformly mixed according to a preset proportion;
(2) Smelting the mixed material at 1000-1100 deg.c, setting the reaction time and making slag float on the surface of the alloy phase, and separating the slag phase from the alloy phase to obtain Cu-Sb alloy phase containing Pt group metal;
(3) Recovering the obtained copper-antimony alloy phase containing the platinum group metal, and carrying out acidolysis, separation and purification treatment to obtain the platinum group metal;
the copper is one or more of copper powder, copper oxide and copper concentrate;
the antimony is one or more of antimony metal powder, antimony oxide, antimony concentrate and the like.
2. The method for low-temperature trapping and recovering platinum group metals in waste catalysts according to claim 1, wherein in the step (1), the waste catalysts are waste catalysts containing platinum group metals.
3. The method for low-temperature trapping and recovering platinum group metals in waste catalysts according to claim 1, wherein in the step (1), the mass ratio of the waste catalyst to the trapping agent is 1 (0.1-0.4).
4. The method for low-temperature trapping and recovering the platinum group metal in the waste catalyst according to claim 1, wherein in the step (1), the reducing agent is any one or more of coke, carbon powder, graphite and coal powder.
5. The method for low temperature capture and recovery of platinum group metals in spent catalysts according to claim 1, step (1), wherein the slagging flux comprises one or more of calcium oxide, magnesium oxide, calcium fluoride, borax.
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| CN114990347B (en) * | 2022-06-24 | 2024-04-02 | 江苏北矿金属循环利用科技有限公司 | Method for recycling platinum group metals in waste catalysts through pyrometallurgy |
| CN115418492B (en) * | 2022-09-21 | 2023-10-24 | 安徽工业大学 | Method for capturing platinum group metals in waste automobile exhaust catalyst by low-temperature smelting copper |
| CN116144929A (en) * | 2022-12-20 | 2023-05-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for capturing and recycling platinum group metals in waste catalysts by semi-molten reinforced reduced iron |
| CN116904758A (en) * | 2023-07-19 | 2023-10-20 | 昆明理工大学 | Method for recovering noble metal by silver-containing copper slag in cooperation with automobile failure catalyst |
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| CN103014352A (en) * | 2013-01-08 | 2013-04-03 | 昆明贵金属研究所 | Method for smelting and extracting platinum metal from alumina-supported petrochemical catalyst |
| CN104178634A (en) * | 2014-08-19 | 2014-12-03 | 昆明贵金属研究所 | Method for efficiently and cleanly recovering platinum group metals from spent automobile catalyst |
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