CN113528843A - Method for smelting and trapping platinum and rhenium from spent aluminum-based catalyst - Google Patents
Method for smelting and trapping platinum and rhenium from spent aluminum-based catalyst Download PDFInfo
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- CN113528843A CN113528843A CN202110881695.9A CN202110881695A CN113528843A CN 113528843 A CN113528843 A CN 113528843A CN 202110881695 A CN202110881695 A CN 202110881695A CN 113528843 A CN113528843 A CN 113528843A
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- 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
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- C22B11/00—Obtaining noble metals
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- 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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- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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- C22B5/00—General methods of reducing to metals
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Abstract
The invention discloses a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps: roasting and ball-milling the platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; uniformly mixing the ineffective aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material; and reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and an iron matte alloy containing platinum and rhenium. The method for smelting and capturing the platinum and the rhenium from the spent aluminum-based catalyst has the advantages that the yield of the platinum and the rhenium in the iron matte is respectively more than 99.5 percent and 85.0 percent from the raw materials to the iron matte. The method has the advantages of simple process, high platinum and rhenium yield, low cost, subsequent platinum extraction of the concentrate, less acid consumption, less environmental pollution and the like.
Description
Technical Field
The invention belongs to the field of rare and precious metal metallurgy, and relates to a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst.
Background
The platinum-rhenium-containing catalyst is mainly applied to the petrochemical industry, can lose efficacy due to pollution of high temperature, combustible gas and the like in the using process, but the value of platinum is not changed, and the platinum-rhenium content of the platinum-rhenium-containing waste catalyst is higher than that of platinum-containing minerals and is rare and expensive, so that the recovery of platinum from the platinum-rhenium-containing waste catalyst has very important economic and social meanings.
The existing method for recovering platinum group metals from the spent aluminum-based catalyst is a wet process, and has the disadvantages of short process flow, low yield and serious environmental pollution caused by waste water and waste residues. The development of a platinum-rhenium method capable of realizing low-cost and environment-friendly efficient trapping is urgently needed.
Disclosure of Invention
To this end, the present invention provides a process for the smelt capture of platinum and rhenium from spent aluminum-based catalysts.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting and ball-milling the platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles;
uniformly mixing the ineffective aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material;
and reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and an iron matte alloy containing platinum and rhenium.
In one embodiment of the invention, the roasting temperature is 450-550 ℃, and the roasting time is 2-4 h.
In one embodiment of the present invention, the reducing agent is one or more of coke powder, anthracite, iron powder, bituminous coal and charcoal.
In an embodiment of the present invention, the fluxing agent is one or more of fluorite, borax, calcium fluoride and sodium carbonate.
In one embodiment of the invention, the addition amount of fluorite is 20-60% of the weight ratio of the spent aluminum-based catalyst, and the addition amount of borax is 30-60% of the weight ratio of the spent aluminum-based catalyst.
In one embodiment of the invention, the collector is ferrous sulfate.
In one embodiment of the present invention, the slagging agent is limestone and/or quartz sand.
In one embodiment of the invention, the addition amount of the trapping agent is 1.8-2.4 times of the weight ratio of the spent aluminum-based catalyst;
the addition amount of the reducing agent is 20% of the weight ratio of the spent aluminum-based catalyst.
In one embodiment of the invention, in the smelting and trapping process of the reduced iron making matte, the smelting temperature is 1350-1400 ℃, and the smelting time is 20-40 min.
The invention has the following advantages:
the method for smelting and capturing the platinum and the rhenium from the spent aluminum-based catalyst has the advantages that the yield of the platinum and the rhenium in the iron matte is respectively more than 99.5 percent and 85.0 percent from the raw materials to the iron matte. The method has the advantages of simple process, high platinum and rhenium yield, low cost, subsequent platinum extraction of the concentrate, reduction of acid consumption, small environmental pollution and the like, realizes low-cost clean platinum and rhenium capture from the ineffective aluminum-based catalyst, has simple pyrogenic process smelting process, short process, mature main equipment, easy industrialization and wide industrialization application prospect, and the product obtained by the method is convenient for selective platinum leaching by adding sulfuric acid subsequently to obtain platinum concentrate, and the ferrous sulfate solution can be returned to be used as an ingredient after being concentrated and crystallized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a flow chart of a process for smelting and trapping platinum from a spent aluminum-based catalyst according to an embodiment of the present invention;
fig. 2 is an iron matte XRD pattern of an embodiment of the present invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting and ball-milling the platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 450-550 ℃, and the roasting time is 2-4 h.
Uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material; the reducing agent is one or more of coke powder, iron powder, anthracite, bituminous coal and charcoal. The fluxing agent is one or more of fluorite, borax, calcium fluoride and sodium carbonate. The adding amount of fluorite is 20-60% of the weight ratio of the ineffective aluminum-based catalyst, and the adding amount of borax is 30-60% of the weight ratio of the ineffective aluminum-based catalyst. The trapping agent is ferrous sulfate. The addition amount of the trapping agent is 1.8-2.4 times of the weight ratio of the spent aluminum-based catalyst; the addition amount of the reducing agent is 20% of the weight ratio of the spent aluminum-based catalyst. The slagging agent is limestone and/or quartz sand.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of the reduction iron making matte, the smelting temperature is 1350-1400 ℃, and the smelting time is 20-40 min.
Example 1
As shown in fig. 1, an embodiment of the present invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, comprising the steps of:
roasting and ball-milling 5kg of a platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 450 ℃, and the roasting time is 2 h.
And uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material. Wherein, the fluxing agent calcium fluoride is 0.3 times of the weight of the failure aluminum-based catalyst, the fluxing agents sodium carbonate and borax are respectively 20 percent of the weight of the failure aluminum-based catalyst, and the reducing agent charcoal is 20 percent of the weight of the failure aluminum-based catalyst. The adding amount of the trapping agent ferrous sulfate is 2.0 times of the weight ratio of the spent aluminum-based catalyst; the addition amount of the reducing agent iron powder is 0.2 times of the weight ratio of the spent aluminum-based catalyst. The slagging agent quartz sand is 2 times of the ineffective aluminum-based catalyst, and the slagging agent limestone is 1 time of the ineffective aluminum-based catalyst.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of reducing and manufacturing the iron matte, the smelting temperature is 1350 ℃, and the smelting time is 20 min.
According to the detection, in the iron-matte alloy containing platinum and rhenium, the recovery rates of platinum and rhenium respectively reach 99.56% and 86.71%.
Example 2
The embodiment of the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting and ball-milling 10kg of platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 500 ℃, and the roasting time is 3 h.
And uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material. Wherein, the fluxing agent calcium fluoride is 0.3 times of the weight of the ineffective aluminum-based catalyst, the fluxing agents sodium carbonate and borax are respectively 20 percent of the weight of the ineffective aluminum-based catalyst, and the reducing agent charcoal is 20 percent of the weight of the ineffective aluminum-based catalyst; the addition amount of the reducing agent iron powder is 0.2 times of the weight ratio of the spent aluminum-based catalyst. The adding amount of the trapping agent ferrous sulfate is 2.1 times of the weight ratio of the spent aluminum-based catalyst. The slagging agent quartz sand is 2 times of the ineffective aluminum-based catalyst, and the slagging agent limestone is 1.2 times of the ineffective aluminum-based catalyst.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of reducing and manufacturing the iron matte, the smelting temperature is 1400 ℃, and the smelting time is 30 min.
According to the detection, in the iron-matte alloy containing platinum and rhenium, the recovery rates of platinum and rhenium respectively reach 99.66% and 86.80%.
Example 3
The embodiment of the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting 8kg of a platinum-containing spent aluminum-based catalyst, and carrying out ball milling to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 550 ℃, and the roasting time is 3 h.
And uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material. Wherein, the fluxing agent calcium fluoride is 0.3 times of the weight of the ineffective aluminum-based catalyst, the fluxing agents sodium carbonate and borax are respectively 20 percent of the weight of the ineffective aluminum-based catalyst, and the reducing agent charcoal is 20 percent of the weight of the ineffective aluminum-based catalyst; the addition amount of the reducing agent iron powder is 0.4 times of the weight ratio of the spent aluminum-based catalyst. The adding amount of the trapping agent ferrous sulfate is 2.3 times of the weight ratio of the spent aluminum-based catalyst. The slagging agent quartz sand is 2 times of the ineffective aluminum-based catalyst, and the slagging agent limestone is 1 time of the ineffective aluminum-based catalyst.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of reducing and manufacturing the iron matte, the smelting temperature is 1450 ℃, and the smelting time is 35 min.
According to the detection, in the iron-matte alloy containing platinum and rhenium, the recovery rates of platinum and rhenium respectively reach 99.65% and 88.92%.
Example 3
The embodiment of the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting and ball-milling 10kg of platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 550 ℃, and the roasting time is 3 h.
And uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material. Wherein, the fluxing agent calcium fluoride is 0.3 times of the weight of the failure aluminum-based catalyst, the fluxing agent sodium carbonate is 60 percent of the weight of the failure aluminum-based catalyst, the fluxing agent borax is 20 percent of the weight of the failure aluminum-based catalyst, and the reducing agent charcoal is 20 percent of the weight of the failure aluminum-based catalyst; the addition amount of the reducing agent iron powder is 0.2 times of the weight ratio of the spent aluminum-based catalyst. The adding amount of the trapping agent ferrous sulfate is 1.9 times of the weight ratio of the spent aluminum-based catalyst. The slagging agent quartz sand is 2 times of the ineffective aluminum-based catalyst, and the slagging agent limestone is 1 time of the ineffective aluminum-based catalyst.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of reducing and manufacturing the iron matte, the smelting temperature is 1450 ℃, and the smelting time is 35 min.
According to the detection, in the iron-matte alloy containing platinum and rhenium, the recovery rates of platinum and rhenium respectively reach 99.71% and 89.33%.
Example 4
The embodiment of the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting and ball-milling 20kg of platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 550 ℃, and the roasting time is 3 h.
And uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material. Wherein, the fluxing agent calcium fluoride is 0.3 times of the weight of the failure aluminum-based catalyst, the fluxing agent sodium carbonate is 20 percent of the weight of the failure aluminum-based catalyst, the fluxing agent borax is 60 percent of the weight of the failure aluminum-based catalyst, and the reducing agent charcoal is 20 percent of the weight of the failure aluminum-based catalyst; the addition amount of the reducing agent iron powder is 0.2 times of the weight ratio of the spent aluminum-based catalyst. The adding amount of the trapping agent ferrous sulfate is 2.4 times of the weight ratio of the spent aluminum-based catalyst. The slagging agent quartz sand is 2 times of the ineffective aluminum-based catalyst, and the slagging agent limestone is 1 time of the ineffective aluminum-based catalyst.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of reducing and manufacturing the iron matte, the smelting temperature is 1450 ℃, and the smelting time is 35 min.
According to the detection, in the iron-matte alloy containing platinum and rhenium, the recovery rates of platinum and rhenium respectively reach 99.52% and 86.21%.
Example 5
The embodiment of the invention provides a method for smelting and trapping platinum and rhenium from a spent aluminum-based catalyst, which comprises the following steps:
roasting and ball-milling 20kg of platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles; the roasting temperature is 550 ℃, and the roasting time is 3 h.
And uniformly mixing the invalid aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material. Wherein, the fluxing agent calcium fluoride is 0.6 times of the weight of the ineffective aluminum-based catalyst, the fluxing agents sodium carbonate and borax are respectively 20 percent of the weight of the ineffective aluminum-based catalyst, and the reducing agent charcoal is 20 percent of the weight of the ineffective aluminum-based catalyst; the addition amount of the reducing agent iron powder is 0.2 times of the weight ratio of the spent aluminum-based catalyst. The adding amount of the trapping agent ferrous sulfate is 2.2 times of the weight ratio of the spent aluminum-based catalyst. The slagging agent quartz sand is 2 times of the ineffective aluminum-based catalyst, and the slagging agent limestone is 1 time of the ineffective aluminum-based catalyst.
And reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and iron matte alloy containing platinum and rhenium. In the smelting and trapping process of reducing and manufacturing the iron matte, the smelting temperature is 1450 ℃, and the smelting time is 35 min.
According to the detection, in the iron-matte alloy containing platinum and rhenium, the recovery rates of platinum and rhenium respectively reach 99.72% and 85.96%.
In the embodiment of the invention, the iron matte is analyzed by adopting X-diffraction, and the result is shown in figure 2, wherein the main phases of the iron matte are FeS and Fe, and other substances are not shown. The iron matte is an excellent platinum group metal trapping stage, and the platinum trapping effect is good in the embodiment, so that the recovery rates of the platinum and the rhenium are respectively more than 99.5 percent and 85.0 percent.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A process for the smelt capture of platinum and rhenium from spent aluminum-based catalysts, characterized in that said process comprises the steps of:
roasting and ball-milling the platinum-containing spent aluminum-based catalyst to obtain crushed spent aluminum-based catalyst particles;
uniformly mixing the ineffective aluminum-based catalyst particles with a trapping agent, a slagging agent and a fluxing agent to obtain a mixed material;
and reducing the mixed material to produce iron matte, smelting and trapping to respectively obtain smelting slag and an iron matte alloy containing platinum and rhenium.
2. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
the roasting temperature is 450-550 ℃, and the roasting time is 2-4 h.
3. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
the reducing agent is one or more of coke powder, anthracite, iron powder, bituminous coal and charcoal.
4. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
the fluxing agent is one or more of fluorite, borax, calcium fluoride and sodium carbonate.
5. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 4,
the addition amount of the fluorite is 20-60% of the weight ratio of the ineffective aluminum-based catalyst, and the addition amount of the borax is 30-60% of the weight ratio of the ineffective aluminum-based catalyst.
6. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
the trapping agent is ferrous sulfate.
7. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
the slagging agent is limestone and/or quartz sand.
8. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
the addition amount of the trapping agent is 1.8-2.4 times of the weight ratio of the spent aluminum-based catalyst;
the addition amount of the reducing agent is 20% of the weight ratio of the spent aluminum-based catalyst.
9. The process for the smelt capture of platinum and rhenium from spent aluminum based catalysts according to claim 1,
in the smelting and trapping process of the reduction iron making matte, the smelting temperature is 1350-1400 ℃, and the smelting time is 20-40 min.
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| CN114107692A (en) * | 2021-11-30 | 2022-03-01 | 红河学院 | Method for adding nickel sulfate to smelt and capture platinum group metal in spent automobile exhaust catalyst |
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| CN109097584A (en) * | 2018-08-27 | 2018-12-28 | 浙江特力再生资源有限公司 | The technique of platinum rhenium aluminium is recycled in a kind of platinum rhenium dead catalyst from alumina supporter |
| CN109280774A (en) * | 2018-10-29 | 2019-01-29 | 昆明理工大学 | A method of rare precious metal is extracted and is enriched with from spent catalyst |
| CN109402403A (en) * | 2018-12-12 | 2019-03-01 | 北京科技大学 | A kind of method that pickling sludge traps platinum group metal in spent catalyst |
| US20190256949A1 (en) * | 2019-04-29 | 2019-08-22 | Techemet, LP | Low-Flux Converting Process for PGM Collector Alloy |
| CN110863104A (en) * | 2019-11-28 | 2020-03-06 | 北京科技大学 | Method for trapping agglomerate by using platinum group metal-containing waste catalyst iron |
| CN112011696A (en) * | 2020-08-19 | 2020-12-01 | 北京科技大学 | Method for enriching platinum group metal in aluminum-based waste catalyst by pyrogenic process |
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| CN114058866A (en) * | 2021-11-30 | 2022-02-18 | 红河学院 | Method for enriching platinum and rhenium from spent alumina carrier platinum-rhenium catalyst |
| CN114107692A (en) * | 2021-11-30 | 2022-03-01 | 红河学院 | Method for adding nickel sulfate to smelt and capture platinum group metal in spent automobile exhaust catalyst |
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Application publication date: 20211022 |