CN110724829A - Method for efficiently enriching noble metals from difficultly-treated palladium-containing waste catalyst - Google Patents
Method for efficiently enriching noble metals from difficultly-treated palladium-containing waste catalyst Download PDFInfo
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- CN110724829A CN110724829A CN201911014235.5A CN201911014235A CN110724829A CN 110724829 A CN110724829 A CN 110724829A CN 201911014235 A CN201911014235 A CN 201911014235A CN 110724829 A CN110724829 A CN 110724829A
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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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- 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
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
-
- 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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- 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 efficiently enriching noble metals from a difficult-to-treat palladium-containing waste catalyst, which comprises the following steps: heating the palladium-containing waste catalyst, the copper mud pressurized slag, the reducing agent and the fluxing agent and preserving heat; cooling and separating slag and precious lead alloy, grinding, sampling and analyzing the content; and (3) carrying out vacuum melting, distillation and separation on the noble lead alloy to obtain the rare noble alloy and the lead bismuth alloy of the vacuum furnace, and separating the noble metal from the lead bismuth. The invention adopts a melting low-temperature alkaline enrichment smelting method to treat high-silicon and aluminum carrier type high-and low-grade palladium-containing waste catalyst and copper anode mud pressurized slag, realizes the cascade comprehensive utilization of gold, silver and platinum noble metals, lead, bismuth and rare and precious metal elements, and has the advantages of shortest flow, lowest cost and highest efficiency; the ratio of the palladium-containing waste catalyst can be large or small, the treatment capacity is flexible, the enrichment smelting treatment is realized, and the enrichment smelting of platinum group noble metals is not influenced; the smelting temperature is far lower than that of matte smelting by adopting a smelting low-temperature alkaline smelting technology, so that the energy consumption is greatly reduced, and the processing cost of the waste catalyst difficult to treat is reduced.
Description
Technical Field
The invention belongs to the technical field of rare and precious metal pyrometallurgy and vacuum metallurgy, and particularly relates to a method for efficiently enriching precious metals from a difficult-to-treat palladium-containing waste catalyst.
Background
Because the secondary resource grade of the platinum group metal is high, the carrier is usually cordierite or alumina carrier, when the all-wet process is directly adopted for treatment, the leaching slag still contains the platinum group metal, the leaching slag needs to be repeatedly subjected to wet treatment for many times, and the process is long, so that the one-time direct yield of the platinum group metal is not high, the reagent consumption is high, a large amount of high-hydrochloric acid wastewater is generated, and in addition, the problems of high processing cost and environmental pollution exist because a large amount of silicon and aluminum are dissolved, and the liquid-solid separation is difficult.
The palladium-containing waste catalyst is an aluminosilicate carrier catalyst, the contents of silicon dioxide, aluminum oxide and the like are high, the melting point is correspondingly high, palladium is an effective catalytic component, the contents of other metals are low, and the catalyst contains high sulfur. When the pyrometallurgical enrichment smelting is adopted, the melting point of the slag of a common slag type is very high, the melting is difficult, and the energy consumption is high.
Disclosure of Invention
The invention aims to provide a method for efficiently enriching noble metals from a difficult-to-treat palladium-containing waste catalyst so as to solve the problems.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for efficiently enriching noble metals from a difficult-to-treat palladium-containing waste catalyst comprises the following steps:
A. accurately weighing the ground waste catalyst containing palladium, copper mud pressurized slag, reducing agent and fluxing agent respectively, uniformly mixing, and filling into a clay crucible covered with a graphite crucible;
B. heating the crucible filled with the ingredients to 1250-;
C. after the smelting samples are taken out of the furnace, quenching or naturally cooling to normal temperature, pouring out the solidified slag and the precious lead alloy or smashing the crucible carefully and separating the slag and the precious lead alloy carefully, respectively and accurately weighing the mass of the slag and the precious lead alloy on an electronic scale, then respectively grinding the slag and the precious lead alloy on a vibration sample grinding machine, and sampling and analyzing the content of base metals or oxides and the content of precious metals;
D. and (3) conveying the noble lead alloy to a vacuum metallurgical furnace for vacuum melting, distilling and separating to obtain rare noble alloy and lead bismuth alloy of the vacuum furnace, and separating the noble metal from the lead bismuth.
In order to further realize the method, the adding amount of the palladium-containing dead catalyst in the step A is 7-21% of the mass of the copper mud pressurizing slag.
In order to further realize the method, the reducing agent in the step A is coke powder, and the adding amount of the coke powder is 3-5% of the mass of the copper mud pressurized slag.
In order to further realize the method, the fluxing agent in the step A is sodium carbonate, and the adding amount of the sodium carbonate is 7-21% of the mass of the copper mud pressurized slag.
In order to further realize the invention, the vacuum degree of the vacuum melting distillation separation in the step D is 3-18Pa, the temperature is 1000-1050 ℃, and the time is 2.0-3.0 h.
Compared with the prior art, the invention has the beneficial effects that:
platinum and palladium have similar lattice structures and similar lattice radii with gold, silver, lead, bismuth, tellurium, selenium and the like, so that a continuous solid solution alloy or an intermetallic compound can be formed in a wide composition range, and a continuous solid solution, namely a noble lead alloy, can be formed between the platinum and the palladium in a wide composition range, so that the multi-element noble lead alloy in a molten state is a high-efficiency trapping agent for platinum and palladium.
The smelting process comprises the steps that oxides of lead, bismuth and the like and reducing agent coke are subjected to reduction reaction, oxides of silicon, aluminum, calcium, barium and magnesium and fluxing agent sodium carbonate and the like are subjected to slag formation to form molten low-temperature alkaline slag with strong liquidity, lead, bismuth and the like and rare noble metal simple substances form low-temperature noble lead alloy melt, and the noble metal simple substances all enter the noble lead alloy because the slag and the melt are not mutually soluble.
Because the alumina component content of the platinum and palladium carrier catalyst is high, when pyrometallurgical enrichment smelting is adopted, the melting point of general slag type furnace slag is very high, the smelting is difficult, the energy consumption is high, in order to reduce the melting temperature and the smelting cost, a melting low-temperature alkaline smelting method in an alkaline metallurgical process is adopted, a palladium-containing waste catalyst, copper anode mud pressurized slag, a fluxing agent and the like are mixed and proportioned, the melting low-temperature alkaline enrichment smelting is carried out, rare metals are efficiently enriched in the multi-metal noble lead alloy, then the noble lead alloy is separated by vacuum metallurgical distillation, and the noble metals such as silver, gold, platinum, palladium and the like are separated from lead and bismuth, so that the rare noble alloy and the lead bismuth alloy are obtained.
The palladium-containing waste catalyst component (unit: Pt, Pd, Au, g/t, the rest%): au38.8, Pd1060, Pt157, CaO0.15, MgO 0.055, Al2O370.81、SiO213.26。
(1) The invention adopts a melting low-temperature alkaline enrichment smelting method to treat the high-silicon and aluminum carrier type high-and low-grade palladium-containing waste catalyst and the copper anode mud pressurized slag, so that the gold, silver and platinum noble metals, lead, bismuth and rare and noble metal elements can be comprehensively utilized in a cascade manner, the process is shortest, the cost is lowest, and the efficiency is highest;
(2) the ratio of the palladium-containing waste catalyst can be large or small, the treatment capacity is flexible, the enrichment smelting treatment can be realized from 7 percent to 21 percent, and the enrichment smelting of platinum group noble metals is not influenced;
(3) by adopting a melting low-temperature alkaline smelting technology, the smelting temperature is lower and ranges from 1250-;
(4) compared with the traditional wet process or double wet process, the direct recovery rate of the metal processed in one step is higher, and the content of the valuable metal contained in the slag is low; the high-silicon aluminum carrier type low-grade palladium-containing waste catalyst is treated by adopting a melting low-temperature alkaline enrichment smelting method, and the direct yield of platinum and palladium can reach 98-99 percent through one-step enrichment smelting.
Detailed Description
The present invention will be further described with reference to the following embodiments.
A method for efficiently enriching noble metals from a difficult-to-treat palladium-containing waste catalyst comprises the following steps:
A. accurately weighing and uniformly mixing the ground palladium-containing waste catalyst, copper mud pressurized slag, a reducing agent and a fluxing agent, and filling the mixture into a clay crucible covered with a graphite crucible, wherein the addition amount of the palladium-containing waste catalyst is 7-21% of the mass of the copper mud pressurized slag, the addition amount of the reducing agent coke powder is 3-5% of the mass of the copper mud pressurized slag, and the addition amount of the fluxing agent sodium carbonate is 7-21% of the mass of the copper mud pressurized slag;
B. heating the crucible filled with the ingredients to 1250-;
C. after the smelting samples are taken out of the furnace, quenching or naturally cooling to normal temperature, pouring out the solidified slag and the precious lead alloy or smashing the crucible carefully and separating the slag and the precious lead alloy carefully, respectively and accurately weighing the mass of the slag and the precious lead alloy on an electronic scale, then respectively grinding the slag and the precious lead alloy on a vibration sample grinding machine, and sampling and analyzing the content of base metals or oxides and the content of precious metals;
D. the noble lead alloy is sent to a vacuum metallurgical furnace for vacuum melting distillation separation, the vacuum degree of the vacuum melting distillation separation is 3-18Pa, the temperature is 1000-1050 ℃, and the time is 2.0-3.0h, so that rare noble alloy and lead bismuth alloy of the vacuum furnace are obtained, and noble metal and lead bismuth and the like are separated.
Example 1:
the copper mud pressurized slag comprises the components (unit:percent, Au, Pd and Pt g/t) Ag13.79, Au2710, Pd236, Pt139, Ni3.60, Cu0.89, Pb21.84, Bi3.12, Se3.78 and Te1.93.
A. Accurately weighing and uniformly mixing the ground palladium-containing waste catalyst, copper mud pressurized slag, a reducing agent and a fluxing agent, and filling the mixture into a clay crucible covered with a graphite crucible, wherein the addition amount of the palladium-containing waste catalyst is 7-21% of the mass of the copper mud pressurized slag, the addition amount of the reducing agent coke powder is 3-5% of the mass of the copper mud pressurized slag, and the addition amount of the fluxing agent sodium carbonate is 7-21% of the mass of the copper mud pressurized slag;
B. heating the crucible filled with the ingredients to 1250-;
C. after the smelting samples are taken out of the furnace, quenching or naturally cooling to normal temperature, pouring out the solidified slag and the precious lead alloy or smashing the crucible carefully and separating the slag and the precious lead alloy carefully, respectively and accurately weighing the mass of the slag and the precious lead alloy on an electronic scale, then respectively grinding the slag and the precious lead alloy on a vibration sample grinding machine, and sampling and analyzing the content of base metals or oxides and the content of precious metals;
D. the noble lead alloy is sent to a vacuum metallurgical furnace for vacuum melting distillation separation, the vacuum degree of the vacuum melting distillation separation is 3-18Pa, the temperature is 1000-1050 ℃, and the time is 2.0-3.0h, so that rare noble alloy and lead bismuth alloy of the vacuum furnace are obtained, and noble metal and lead bismuth and the like are separated.
Example 2:
A. accurately weighing and uniformly mixing the ground palladium-containing waste catalyst, copper mud pressurized slag, a reducing agent and a fluxing agent, and filling the mixture into a clay crucible covered with a graphite crucible, wherein the addition amount of the palladium-containing waste catalyst is 7-21% of the mass of the copper mud pressurized slag, the addition amount of the reducing agent coke powder is 3-5% of the mass of the copper mud pressurized slag, and the addition amount of the fluxing agent sodium carbonate is 7-21% of the mass of the copper mud pressurized slag;
B. heating the crucible filled with the ingredients to 1250-;
C. after the smelting samples are taken out of the furnace, quenching or naturally cooling to normal temperature, pouring out the solidified slag and the precious lead alloy or smashing the crucible carefully and separating the slag and the precious lead alloy carefully, respectively and accurately weighing the mass of the slag and the precious lead alloy on an electronic scale, then respectively grinding the slag and the precious lead alloy on a vibration sample grinding machine, and sampling and analyzing the content of base metals or oxides and the content of precious metals;
D. the noble lead alloy is sent to a vacuum metallurgical furnace for vacuum melting distillation separation, the vacuum degree of the vacuum melting distillation separation is 3-18Pa, the temperature is 1000-1050 ℃, and the time is 2.0-3.0h, so that rare noble alloy and lead bismuth alloy of the vacuum furnace are obtained, and noble metal and lead bismuth and the like are separated.
Example 3:
A. accurately weighing and uniformly mixing the ground palladium-containing waste catalyst, copper mud pressurized slag, a reducing agent and a fluxing agent, and filling the mixture into a clay crucible covered with a graphite crucible, wherein the addition amount of the palladium-containing waste catalyst is 7-21% of the mass of the copper mud pressurized slag, the addition amount of the reducing agent coke powder is 3-5% of the mass of the copper mud pressurized slag, and the addition amount of the fluxing agent sodium carbonate is 7-21% of the mass of the copper mud pressurized slag;
B. heating the crucible filled with the ingredients to 1250-;
C. after the smelting samples are taken out of the furnace, quenching or naturally cooling to normal temperature, pouring out the solidified slag and the precious lead alloy or smashing the crucible carefully and separating the slag and the precious lead alloy carefully, respectively and accurately weighing the mass of the slag and the precious lead alloy on an electronic scale, then respectively grinding the slag and the precious lead alloy on a vibration sample grinding machine, and sampling and analyzing the content of base metals or oxides and the content of precious metals;
D. the noble lead alloy is sent to a vacuum metallurgical furnace for vacuum melting distillation separation, the vacuum degree of the vacuum melting distillation separation is 3-18Pa, the temperature is 1000-1050 ℃, and the time is 2.0-3.0h, so that rare noble alloy and lead bismuth alloy of the vacuum furnace are obtained, and noble metal and lead bismuth and the like are separated.
Claims (5)
1. A method for efficiently enriching noble metals from a difficult-to-treat palladium-containing waste catalyst is characterized by comprising the following steps:
A. accurately weighing the ground waste catalyst containing palladium, copper mud pressurized slag, reducing agent and fluxing agent respectively, uniformly mixing, and filling into a clay crucible covered with a graphite crucible;
B. heating the crucible filled with the ingredients to 1250-;
C. after the smelting samples are taken out of the furnace, quenching or naturally cooling to normal temperature, pouring out the solidified slag and the precious lead alloy or smashing the crucible carefully and separating the slag and the precious lead alloy carefully, respectively and accurately weighing the mass of the slag and the precious lead alloy on an electronic scale, then respectively grinding the slag and the precious lead alloy on a vibration sample grinding machine, and sampling and analyzing the content of base metals or oxides and the content of precious metals;
D. and (3) conveying the noble lead alloy to a vacuum metallurgical furnace for vacuum melting, distilling and separating to obtain rare noble alloy and lead bismuth alloy of the vacuum furnace, and separating the noble metal from the lead bismuth.
2. The method for efficiently enriching noble metals from difficult-to-treat palladium-containing spent catalysts according to claim 1, wherein: the adding amount of the palladium-containing dead catalyst in the step A is 7-21% of the mass of the copper mud pressurizing slag.
3. The method for efficiently enriching noble metals from a difficult-to-treat palladium-containing spent catalyst according to claim 1 or 2, wherein: in the step A, the reducing agent is coke powder, and the adding amount of the coke powder is 3-5% of the mass of the copper mud pressurized slag.
4. The method for efficiently enriching noble metals from difficult-to-treat palladium-containing spent catalysts according to claim 3, wherein: in the step A, the fluxing agent is sodium carbonate, and the adding amount of the sodium carbonate is 7-21% of the weight of the copper mud pressurized slag.
5. The method for efficiently enriching noble metals from difficult-to-treat palladium-containing spent catalysts according to claim 4, wherein: in the step D, the vacuum degree of the vacuum melting distillation separation is 3-18Pa, the temperature is 1000-1050 ℃, and the time is 2.0-3.0 h.
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Cited By (4)
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| CN113528828A (en) * | 2021-07-01 | 2021-10-22 | 昆明贵研新材料科技有限公司 | Enrichment method of waste alumina carrier platinum group metal catalyst |
| CN114774709A (en) * | 2022-05-25 | 2022-07-22 | 有研资源环境技术研究院(北京)有限公司 | Method for recovering platinum group metals by combination of bismuth pyrogenic process trapping and vacuum distillation |
| 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 |
| CN116622999A (en) * | 2023-05-31 | 2023-08-22 | 昆明理工大学 | Method for enriching platinum group metals |
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Application publication date: 20200124 |