CN114058866A - Method for enriching platinum and rhenium from spent alumina carrier platinum-rhenium catalyst - Google Patents
Method for enriching platinum and rhenium from spent alumina carrier platinum-rhenium catalyst Download PDFInfo
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- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- 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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- C22B7/007—Wet processes by acid leaching
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Abstract
The invention discloses a method for enriching platinum and rhenium from a platinum-rhenium catalyst with a spent alumina carrier, belonging to the technical field of precious metal and rare dispersible metals recovery. The method comprises the steps of mixing an ineffective alumina carrier platinum-rhenium catalyst, a collector pyrite, a fluxing agent and a slagging constituent, carrying out sulfonium making and smelting at 1300-1500 ℃ to enrich platinum in the ineffective alumina carrier platinum-rhenium catalyst, and enriching rhenium from volatilized smoke dust to respectively obtain metal sulfonium, slag and rhenium-containing smoke dust. And (3) carrying out selective leaching on the FeS trapping substance by adopting sulfuric acid to realize further enrichment of platinum. The recovery rate of platinum is more than 99.25%, the recovery rate of rhenium is more than 98%, the enrichment multiple of platinum is more than 30, and the enrichment multiple of rhenium is more than 60. The method has the advantages of simplicity, high efficiency, economy, reliability, effective separation of platinum and rhenium, low technical difficulty and the like, and has potential industrialization prospect.
Description
Technical Field
The invention belongs to the technical field of precious metal and rare dispersible metal recovery, and relates to a method for further separating platinum and rhenium and further enriching platinum and rhenium from a platinum-rhenium catalyst with a spent alumina carrier.
Background
The platinum-rhenium catalyst taking the aluminum oxide as the carrier is widely applied to reactions such as hydrogenation, dehydrogenation, reforming, oxidation, isomerization, disproportionation, cracking, deamination and the like, and plays a very important role in the petrochemical industry. After the catalyst is used for a certain time, the catalytic activity of the platinum and the rhenium is weakened to cause failure, but the existing state of the platinum is unchanged, and the platinum is still a single body and has high value. Platinum metal resources in China are relatively poor, the content of platinum and rhenium in the spent alumina carrier catalyst is far higher than that of raw ores, and the energy consumption, the environmental pollution degree and the process complexity required in the recovery process are all lower than those of raw ore exploitation, so that the recovery of platinum and rhenium in the waste catalyst has important economic value and important social benefit from the viewpoints of resource recycling and environmental protection. At present, the method for recovering platinum and rhenium in the alumina carrier platinum-rhenium catalyst is as follows:
zhang Fang Yu, Wang Haixiang, et al disclose a method for recovering metals such as platinum, rhenium, aluminum, etc. from a waste reforming catalyst (application publication No. CN 00136509.6). The technology removes iron chemically from the waste reforming catalyst, dissolves it in the solution mixed by concentrated sulfuric acid, concentrated hydrochloric acid and water in proportion, ion-exchanges, acidifies and separates tin, ammonifies and separates platinum, deposits rhenium from sylvite, and recovers platinum, rhenium, aluminum and other metals. The method has short process flow and low recovery cost, and realizes the comprehensive utilization of the waste catalyst.
A method for recovering platinum group metals based on copper capture was invented by Ducheng, Chenjialin, etc. (application publication No. 201510235965.3). Mixing platinum group metal-containing waste with a copper trapping agent, an additive and a binder in proportion, finely grinding, adding water to prepare pellets, drying, placing the pellets in a crucible, adding a certain amount of reducing coal, and reducing at a certain temperature; and crushing and ball-milling the metallized pellets obtained by reduction, and then performing gravity separation to obtain concentrate which is metal copper powder containing platinum group metals, thereby realizing the recovery of the platinum group metals. The method has the advantages of simple process flow, low reduction temperature, and easy implementation of the used equipment which is conventional metallurgy and mineral processing equipment; the recovery rate of platinum group metals is more than 99%, and the content of platinum group metals in the reselected tailings is less than 10 g/t. The method can effectively recover platinum group metals from the spent automobile catalyst, the petrochemical catalyst and the fine chemical catalyst, has no harmful gas discharge, can use the tailings as building material raw materials, and has clean and pollution-free whole process.
Prunus mume et al discloses a process for recovering platinum and rhenium from spent alumina-based platinum-rhenium catalysts (application publication No. 201810116294.2). According to the invention, a potential-controlled electrodeposition method is adopted to respectively precipitate platinum and rhenium to obtain pure platinum powder and rhenium powder, so that the aim of efficiently separating platinum and rhenium is achieved, the precipitation and calcination processes of ammonium chloroplatinate and ammonium perrhenate are reduced, the process flow is short, the metal recovery rate is high, the reagent consumption is low, the environment is friendly, and compared with the traditional calcination method, the platinum powder and the rhenium powder prepared by electrodeposition have the advantages of large specific surface area, high powder purity, high chemical activity and great benefit for the subsequent preparation of compounds.
Fanxingxiang, thunder et al invented a method to extract rhenium from a spent platinum-rhenium catalyst (application publication No. 201810701887.5). Crushing a failed platinum-rhenium catalyst, adding water and acid according to a certain liquid-solid ratio for size mixing, putting into a high-pressure kettle for reaction, taking out a reaction material, putting into a normal-pressure reaction kettle, adding an alkaline reagent for regulating the pH value, and filtering and washing to obtain a rhenium-containing solution; and (3) exchanging by using alkaline anion resin, eluting, heating, concentrating and crystallizing to obtain ammonium rhenate. By selecting low acid and oxygen pressure leaching, the carrier dissolution is less, the rhenium leaching rate is high, the obtained solution has low acidity and less other impurities, the subsequent ion exchange rhenium extraction is facilitated, the subsequent neutralization dosage is small, the reagent consumption is obviously reduced, the treatment cost is low, the acidity in the leaching process is low, the corrosion to equipment is small, and the rhenium recovery rate is high.
In summary, the existing method for recovering platinum group metals from the platinum-rhenium catalyst of the ineffective alumina carrier is the traditional reduction smelting and wet process, the method for enriching platinum and rhenium from the platinum-rhenium catalyst of the ineffective alumina carrier is provided, and the method has the advantages of simplicity, high efficiency, economy, reliability, realization of one-step effective separation of platinum and rhenium, low technical difficulty and the like, and has potential industrialization prospect. The adoption of pyrite for smelting FeS and trapping has not been reported in reference data.
Disclosure of Invention
The invention aims to provide a method for enriching platinum and rhenium from a platinum-rhenium catalyst on a failed alumina carrier.
The invention relates to a method for enriching platinum and rhenium from a platinum-rhenium catalyst with a spent alumina carrier, which comprises the following steps:
(1) the platinum-rhenium catalyst, the trapping agent, the fluxing agent and the slagging agent of the ineffective alumina carrier are mixed by ball milling;
(2) carrying out pyrite matte smelting at a high temperature to obtain FeS, and trapping platinum; collecting dust through a cloth bag to obtain volatile smoke dust enriched rhenium;
(3) and (3) carrying out selective leaching on the FeS trapping substance by adopting sulfuric acid to realize further enrichment of platinum.
In the step (1), the collector is pyrite, the fluxing agent is borax and calcium fluoride, and the slagging constituent is calcium oxide and quartz.
Furthermore, the adding amount of the pyrite is 10-60% of the weight of the failed platinum-rhenium catalyst, the adding amount of the quartz is 1-4 times of the weight of the failed platinum-rhenium catalyst, the adding amount of the calcium oxide is 10-50% of the weight of the failed platinum-rhenium catalyst, the adding amount of the calcium fluoride is 10-40% of the weight of the failed platinum-rhenium catalyst, and the adding amount of the borax is 10-40% of the weight of the failed platinum-rhenium catalyst.
Further, in the step (2), the smelting temperature is 1300-1500 ℃, the smelting time is 0.5-2 h, FeS is obtained by smelting pyrite for making matte, and platinum is collected; and collecting dust through a cloth bag to obtain volatile smoke dust enriched rhenium.
Further, in the step (3), sulfuric acid is adopted to selectively leach iron from the FeS trapping material, so that further enrichment of platinum is realized.
The invention provides a method for enriching platinum and rhenium from a platinum-rhenium catalyst of an ineffective alumina carrier. And (3) carrying out selective leaching on the FeS trapping substance by adopting sulfuric acid to realize further enrichment of platinum. The platinum content of the platinum-rhenium catalyst on the spent alumina carrier is 1780g/t, the rhenium content is 3600g/t, the recovery rate of the platinum is more than 99.25 percent, and the recovery rate of the rhenium is more than 98 percent. And (3) selectively leaching the iron from the FeS trap by using sulfuric acid, wherein the enrichment factor of platinum is more than 30, and the enrichment factor of rhenium is more than 60. The method is simple, efficient, economical and reliable, has low cost and technical difficulty, has higher recovery rate of platinum and rhenium, and has mature smelting process and potential industrialization prospect. The innovation points of the invention are mainly as follows:
(1) the cheap pyrite is used as a matte material, the pyrite is naturally cracked at high temperature to form a good platinum trap FeS, rhenium is volatilized into smoke dust, and the platinum and rhenium are naturally effectively separated and enriched in one step;
(2) the pyrite is adopted for smelting, the molten matte has the property of metalloid, the electronic conduction is realized under the high-temperature condition, platinum atoms enter a matte phase, rhenium enters smoke, and the total recovery rate of the platinum and the rhenium is more than 99%.
Drawings
FIG. 1 is a process flow diagram for the enrichment of platinum and rhenium from a spent alumina supported platinum rhenium catalyst.
Fig. 2 is an XRD pattern of the FeS trap obtained in process example 1 for platinum and rhenium enrichment from a spent alumina supported platinum rhenium catalyst.
Fig. 3 is an XRD pattern of the FeS trap obtained in process example 2 for platinum and rhenium enrichment from a spent alumina supported platinum rhenium catalyst.
Fig. 4 is an XRD pattern of the FeS trap obtained in process example 3 for platinum and rhenium enrichment from a spent alumina supported platinum rhenium catalyst.
Fig. 5 is an XRD pattern of the FeS trap obtained in process example 4 for platinum and rhenium enrichment from a spent alumina supported platinum rhenium catalyst.
Fig. 6 is an XRD pattern of the FeS trap obtained in process example 5 for platinum and rhenium enrichment from a spent alumina supported platinum rhenium catalyst.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the following detailed description of the present invention is given with reference to specific examples:
example 1
As shown in fig. 1, the present embodiment includes the following steps:
weighing 10kg of the platinum-rhenium catalyst with the failed alumina carrier, wherein the adding amount of pyrite is 30% of the weight of the failed platinum-rhenium catalyst, the adding amount of quartz is 2 times of the weight of the failed platinum-rhenium catalyst, the adding amount of calcium oxide is 30% of the weight of the failed platinum-rhenium catalyst, the adding amount of calcium fluoride is 10% of the weight of the failed platinum-rhenium catalyst, and the adding amount of borax is 10% of the weight of the failed platinum-rhenium catalyst. All materials are subjected to ball milling and mixing, and matte smelting is carried out for 2h at 1400 ℃, so as to respectively obtain matte, rhenium-containing smoke dust and slag. Alloy and slag are respectively obtained, and the recovery rates of platinum and rhenium respectively reach 99.33% and 98.21%. The sulfuric acid is adopted to selectively leach iron from the FeS trapping material, the enrichment factor of platinum reaches 35.23, and the enrichment factor of rhenium reaches 68.71. The resulting alloy was characterized by X-ray diffraction analysis and figure 2 is an XRD pattern of FeS trap obtained by a method of platinum and rhenium enrichment from spent alumina supported platinum-rhenium catalysts.
Example 2
As shown in fig. 1, the present embodiment includes the following steps:
weighing 15kg of a platinum-rhenium catalyst with a failure alumina carrier, wherein the addition amount of pyrite is 40% of the weight of the failure platinum-rhenium catalyst, the addition amount of quartz is 1.5 times of the weight of the failure platinum-rhenium catalyst, the addition amount of calcium oxide is 40% of the weight of the failure platinum-rhenium catalyst, the addition amount of calcium fluoride is 20% of the weight of the failure platinum-rhenium catalyst, the addition amount of borax is 20% of the weight of the failure platinum-rhenium catalyst, ball-milling and mixing all materials, and carrying out matte smelting at 1450 ℃ for 0.5h to respectively obtain matte, rhenium-containing smoke and slag. Alloy and slag are respectively obtained, and the recovery rates of platinum and rhenium respectively reach 99.42 percent and 98.37 percent. The sulfuric acid is adopted to selectively leach out iron from the FeS trapping material, the enrichment factor of platinum reaches 40.91, and the enrichment factor of rhenium reaches 71.08. The resulting alloy was characterized by X-ray diffraction analysis and figure 3 is an XRD pattern of FeS trap obtained by a method of platinum and rhenium enrichment from spent alumina supported platinum-rhenium catalysts.
Example 3
As shown in fig. 1, the present embodiment includes the following steps:
weighing 10kg of a platinum-rhenium catalyst with a failed alumina carrier, wherein the addition amount of pyrite is 50% of the weight of the failed platinum-rhenium catalyst, the addition amount of quartz is 2.5 times of the weight of the failed platinum-rhenium catalyst, the addition amount of calcium oxide is 30% of the weight of the failed platinum-rhenium catalyst, the addition amount of calcium fluoride is 30% of the weight of the failed platinum-rhenium catalyst, the addition amount of borax is 20% of the weight of the failed platinum-rhenium catalyst, ball-milling and mixing all materials, and carrying out matte smelting at 1400 ℃ for 1.5h to respectively obtain matte, rhenium-containing smoke and slag. Alloy and slag are respectively obtained, and the recovery rates of platinum and rhenium respectively reach 99.61 percent and 98.25 percent. The sulfuric acid is adopted to selectively leach out iron from the FeS trapping substance, the enrichment factor of platinum reaches 36.08, and the enrichment factor of rhenium reaches 65.02. The resulting alloy was characterized by X-ray diffraction analysis and figure 4 is an XRD pattern of a FeS trap obtained by a method of platinum and rhenium enrichment from a spent alumina supported platinum-rhenium catalyst.
Example 4
As shown in fig. 1, the present embodiment includes the following steps:
weighing 15kg of a platinum-rhenium catalyst with a failure alumina carrier, wherein the adding amount of pyrite is 50% of the weight of the failure platinum-rhenium catalyst, the adding amount of quartz is 3 times of the weight of the failure platinum-rhenium catalyst, the adding amount of calcium oxide is 30% of the weight of the failure platinum-rhenium catalyst, the adding amount of calcium fluoride is 30% of the weight of the failure platinum-rhenium catalyst, the adding amount of borax is 20% of the weight of the failure platinum-rhenium catalyst, performing ball milling and mixing on all materials, and performing matte smelting at 1400 ℃ for 1h to respectively obtain matte, rhenium-containing smoke dust and slag. Alloy and slag are respectively obtained, and the recovery rates of platinum and rhenium respectively reach 99.27 percent and 98.42 percent. The sulfuric acid is adopted to selectively leach iron from the FeS trapping material, the enrichment factor of platinum reaches 38.61, and the enrichment factor of rhenium reaches 70.11. The resulting alloy was characterized by X-ray diffraction analysis and figure 5 is an XRD pattern of a FeS trap obtained by a method of platinum and rhenium enrichment from a spent alumina supported platinum-rhenium catalyst.
Example 5
Weighing 20kg of a platinum-rhenium catalyst with a failure alumina carrier, wherein the addition amount of pyrite is 60% of the weight of the failure platinum-rhenium catalyst, the addition amount of quartz is 2 times of the weight of the failure platinum-rhenium catalyst, the addition amount of calcium oxide is 40% of the weight of the failure platinum-rhenium catalyst, the addition amount of calcium fluoride is 30% of the weight of the failure platinum-rhenium catalyst, the addition amount of borax is 30% of the weight of the failure platinum-rhenium catalyst, ball-milling and mixing all materials, and carrying out matte smelting at 1450 ℃ for 1h to respectively obtain matte, rhenium-containing smoke dust and slag. Alloy and slag are respectively obtained, and the recovery rates of platinum and rhenium respectively reach 99.51% and 98.22%. The sulfuric acid is adopted to selectively leach out iron from the FeS trapping material, the enrichment factor of platinum reaches 34.99, and the enrichment factor of rhenium reaches 61.90. The resulting alloy was characterized by X-ray diffraction analysis and figure 6 is an XRD pattern of a FeS trap obtained by a method of platinum and rhenium enrichment from a spent alumina supported platinum-rhenium catalyst.
Claims (4)
1. A process for the enrichment of platinum and rhenium from a platinum-rhenium catalyst on a spent alumina support, characterized by the steps of:
(1) the platinum-rhenium catalyst, the trapping agent, the fluxing agent and the slagging agent of the ineffective alumina carrier are mixed by ball milling;
(2) carrying out pyrite matte smelting at a high temperature to obtain FeS, and trapping platinum; collecting dust through a cloth bag to obtain volatile smoke dust enriched rhenium;
(3) and (3) carrying out selective leaching on the FeS trapping substance by adopting sulfuric acid to realize further enrichment of platinum.
Wherein: in the step (1), the collector is pyrite, the fluxing agent is borax and calcium fluoride, and the slagging constituent is calcium oxide and quartz.
2. A process as claimed in claim 1, for enriching platinum and rhenium from a platinum-rhenium catalyst on a spent alumina support, wherein: the adding amount of pyrite is 10-60% of the weight of the failed platinum-rhenium catalyst, the adding amount of quartz is 1-4 times of the weight of the failed platinum-rhenium catalyst, the adding amount of calcium oxide is 10-50% of the weight of the failed platinum-rhenium catalyst, the adding amount of calcium fluoride is 10-40% of the weight of the failed platinum-rhenium catalyst, and the adding amount of borax is 10-40% of the weight of the failed platinum-rhenium catalyst.
3. A process as claimed in claim 1, for enriching platinum and rhenium from a platinum-rhenium catalyst on a spent alumina support, wherein: smelting at 1300-1500 ℃ for 0.5-2 h, and carrying out pyrite matte smelting to obtain FeS, and trapping platinum; and collecting dust through a cloth bag to obtain volatile smoke dust enriched rhenium.
4. A process as claimed in claim 1, for enriching platinum and rhenium from a platinum-rhenium catalyst on a spent alumina support, wherein: and (4) selectively leaching iron from the FeS trapping substance by using sulfuric acid in the step (3) to realize further enrichment of platinum.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116751981A (en) * | 2023-06-16 | 2023-09-15 | 昆明理工大学 | Method for recovering rare noble metals in automobile failure tail gas purifier |
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2021
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