阅读说明：本技术 一种废氧化铝基半再生重整催化剂铂铼的回收方法 (Method for recovering platinum and rhenium from waste alumina-based semi-regenerated reforming catalyst ) 是由 张深根 丁云集 何学峰 于 2021-09-17 设计创作，主要内容包括：本发明涉及铂铼回收技术领域,公开了一种从Al-(2)O-(3)载体半再生重整催化剂中回收铂铼的方法。该方法公开了以铁粉为捕集剂、碳粉为还原剂,通过添加助熔剂形成Al-(2)O-(3)-CaO-B-(2)O-(3)-Na-(2)O渣型,经熔炼后将Pt、Re还原富集形成Fe-Pt-Re合金熔体后,雾化制粉、硫酸溶解除Fe、过滤后得到Pt和Re混合粉末,再用硝酸溶解Re粉后过滤分别得到Pt粉和HReO-(4)溶液,接着向HReO-(4)溶液加入KOH、经过滤后得到KReO-(4)沉淀物,最后用氢还原得到Re粉。本发明实现了协同回收废氧化铝基半再生重整催化剂中Pt和Re,具有流程短、回收率高、能耗低等优点,适合工业化生产。(The invention relates to the technical field of platinum-rhenium recovery, and discloses a secondary Al 2 O 3 A method for recovering platinum and rhenium from a reforming catalyst with semi-regenerated carrier. The method discloses that Al is formed by taking iron powder as a trapping agent and carbon powder as a reducing agent and adding a fluxing agent 2 O 3 ‑CaO‑B 2 O 3 ‑Na 2 Smelting, reducing and enriching Pt and Re to form Fe-Pt-Re alloy melt, atomizing to prepare powder, dissolving in sulfuric acid to remove Fe, filtering to obtain Pt and Re mixed powder, dissolving Re powder in nitric acid, filtering to obtain Pt powder and HReO powder 4 Solution, then to HReO 4 Adding KOH into the solution, and filtering to obtain KReO 4 Precipitating, and finally reducing by using hydrogen to obtain Re powder. The method realizes the synergistic recovery of Pt and Re in the waste alumina-based semi-regenerative reforming catalyst, has the advantages of short process, high recovery rate, low energy consumption and the like, and is suitable for industrial production.)

1. Waste oxygenThe method for recovering the platinum and rhenium from the aluminum-based semi-regenerated reforming catalyst is characterized by comprising the following steps: al is formed by using iron powder as a trapping agent and carbon powder as a reducing agent and adding a fluxing agent₂O₃-CaO-B₂O₃-Na₂Smelting, reducing and enriching Pt and Re to form Fe-Pt-Re alloy melt, atomizing to prepare powder, dissolving in sulfuric acid to remove Fe, filtering to obtain Pt and Re mixed powder, dissolving Re powder in nitric acid, filtering to obtain Pt powder and HReO powder₄Solution, then to HReO₄Adding KOH into the solution, and filtering to obtain KReO₄Precipitating, and finally reducing hydrogen to obtain Re powder.

2. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerative reforming catalyst as claimed in claim 1, wherein: the method comprises the following steps:

(1) material preparation and material mixing: uniformly mixing 100 parts of waste catalyst, 100 and 200 parts of fluxing agent, 5-20 parts of iron powder and 5-15 parts of carbon powder;

(2) smelting: smelting the uniformly mixed materials, and separating slag iron to obtain Fe-Pt-Re alloy melt and slag;

(3) atomizing to prepare powder: atomizing the Fe-Pt-Re alloy melt to obtain Fe-Pt-Re alloy powder;

(4) acid hydrolysis deferrization: dissolving Fe-Pt-Re alloy powder by using sulfuric acid to remove Fe, and filtering to obtain mixed powder of Pt powder and Re powder;

(5) separating platinum and rhenium: dissolving Re in the mixed powder of platinum and rhenium by using nitric acid, and filtering to obtain Pt powder and HReO₄Filtering the solution;

(6) and (3) precipitating rhenium: adding KOH to HReO₄Filtering the filtrate to obtain KReO₄A precipitate;

(7) reduction: hydrogen reduction of KReO₄Precipitating to obtain a mixture of KOH and Re powder;

(8) and (3) extracting rhenium: and washing and filtering the mixture of the KOH and the Re powder to obtain Re powder and a KOH solution, and recycling the KOH solution for precipitating rhenium.

3. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerative reforming catalyst as claimed in claim 2, wherein: the step (1) is assisted byFlux is CaO 50-80 weight portions and B₂O₃Is 30-60 portions of Na₂CO₃20 to 60 portions.

4. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerative reforming catalyst as claimed in claim 2, wherein: and (2) after the smelting is carried out at 1400-1600 ℃ for 1-3h, separating Fe-Pt-Re alloy melt from slag.

5. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerated reforming catalyst as claimed in claim 2, wherein: and (4) atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 50-200 mu m in the step (3).

6. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerated reforming catalyst as claimed in claim 2, wherein: and (4) the acidolysis iron removal is to dissolve Fe-Pt-Re alloy powder for 1-3h at room temperature of-90 ℃ by using 3-8mol/L sulfuric acid in a solid-to-liquid ratio of 1:3-1:10, and then filtering to obtain mixed powder of Pt powder and Re powder.

7. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerative reforming catalyst as claimed in claim 2, wherein: the platinum-rhenium separation in the step (5) is to perform acidolysis on Re for 1-3h at room temperature of-90 ℃ by using 2-6mol/L nitric acid and a solid-to-liquid ratio of 1:3-1:10, and then filtering to obtain Pt powder and HReO₄The recovery rate of Pt in the filtrate is more than 99%.

8. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerative reforming catalyst as claimed in claim 2, wherein: adding KOH into HReO in the step (6) of precipitating rhenium₄Filtering the filtrate until the pH value is more than or equal to 8 to obtain KReO₄And (4) precipitating.

9. The method for recovering platinum and rhenium from a waste alumina-based semi-regenerative reforming catalyst as claimed in claim 2, wherein: step (7) the rhenium extraction is KReO reduction by hydrogen at 800-₄The mixture of KOH and Re powder is obtained within 0.5-5h, and the recovery rate of Re is more than 98 percent.

Technical Field

The invention relates to the technical field of platinum-rhenium metal recovery, in particular to a method for recovering platinum-rhenium from a waste aluminum oxide-based semi-regenerative reforming catalyst.

Technical Field

The platinum-rhenium is an active component of the alumina-based semi-regenerated reforming catalyst and belongs to a strategic scarce resource. Therefore, the recovery of platinum and rhenium from the waste alumina-based semi-regenerated reforming catalyst is of great significance.

At present, Al₂O₃The recovery method of the Pt-Re catalyst of the carrier mainly adopts a wet method. For example, the Chinese patent (application No. 201810116294.2) uses sulfuric acid to dissolve carrier for failed alumina-based platinum-rhenium catalyst, then uses hydrochloric acid + sodium chlorate or hydrochloric acid + hydrogen peroxide to leach Pt and Re, and obtains Pt and Re through resin adsorption, desorption and electrodeposition. Although the method reduces the procedures of precipitation and reduction of ammonium chloroplatinate and ammonium perrhenate, the obtained platinum and rhenium have high purity, and the platinum and rhenium are leached with large acid consumption and long time. The Chinese patent of invention (application number: 201810979537.5) discloses a process for recovering platinum, rhenium and aluminum from waste platinum-rhenium catalyst with alumina carrier, which uses sulfuric acid to leach the carrier, and uses ammonium sulfide to precipitate platinum, but the method results in platinum and 60-70% rhenium being enriched in slag, the rest rhenium being in the leachate, the rhenium recovery steps are complicated, and the recovery rate is low. The Chinese patent application No. 201710383606.1 discloses a method for recovering platinum and rhenium from an aluminum-based platinum-rhenium reforming catalyst, which comprises the steps of leaching a carrier and rhenium by using alkali, then carrying out resin adsorption on a leaching solution containing rhenium to obtain a high-concentration rhenium solution, adding potassium salt to obtain potassium perrhenate, and refining platinum slag to obtain spongy platinum. The method has the advantages of environmental protection, complete recovery of carrier aluminum and no generation of waste slag. However, the liquid viscosity is high due to the formation of sodium metaaluminate colloid in the process, the recovery rate is low due to the adsorption of rhenium by the colloid, the working procedure is long, and the water consumption is high. The Chinese patent of invention (application number: 00136509.6) discloses a method for recovering metals such as platinum, rhenium, aluminum and the like from waste reforming catalyst, which comprises the steps of dissolving the metals completely by concentrated sulfuric acid and concentrated hydrochloric acid, then adding potassium chloride to leach the platinum and rhenium, and separating the platinum and the rhenium by ammonification and precipitating the platinum and the potassium salt to realize the separation of the platinum and the rhenium. The method realizes comprehensive recovery of platinum, rhenium and aluminum, but the acid dosage is large in the total dissolving process, ammonium perrhenate precipitate and chloroplatinum are easily generated during ammonification and platinum separationThe ammonium salts mix, resulting in reduced rhenium recovery. The Chinese patent of invention (application number: 201110236266.2) discloses a method for recovering platinum, aluminum and rhenium from waste reforming catalysts, wherein rhenium is recovered by carbonate dissolution and potassium salt precipitation; and (3) respectively recovering aluminum and platinum after alkali dissolution and acidolysis filtration. Although the method has mild reaction and low cost, the method needs four times of filtration, and has complex operation and low rhenium leaching rate.

In conclusion, the existing process for recovering platinum and rhenium from the alumina-based catalyst mainly adopts a full-wet method, and has the problems of large acid consumption, high water consumption, complicated process, long time, low rhenium recovery rate and the like.

The Chinese patent of invention (application number: 202010835163.7) discloses a method for enriching platinum group metals in aluminum-based waste catalyst by a pyrogenic process, which adopts CaO-Al₂O₃-Fe₂O₃-B₂O₃The slag system is subjected to iron capture of platinum group metals and platinum group metal enrichment by slag iron separation, but recovery of rhenium and its separation from the platinum group metals is not disclosed.

Disclosure of Invention

The invention discloses a method for recovering platinum and rhenium from a waste aluminum oxide-based semi-regenerated reforming catalyst, aiming at the problem of recycling the aluminum oxide-based waste catalyst. Platinum and rhenium in the waste catalyst are captured by iron, the platinum and rhenium are enriched firstly, then the platinum and rhenium are separated by dissolving in nitric acid, and finally rhenium is precipitated by KOH and recovered by hydrogen reduction. The method has the advantages of simple process, low material consumption, high recovery rate, near zero emission, good economic benefit and the like, and is suitable for industrial production.

The invention adopts the following technical scheme:

a method for recovering platinum and rhenium from a waste alumina-based semi-regenerated reforming catalyst is characterized by comprising the following steps: al is formed by using iron powder as a trapping agent and carbon powder as a reducing agent and adding a fluxing agent₂O₃-CaO-B₂O₃-Na₂Smelting, reducing and enriching Pt and Re to form Fe-Pt-Re alloy melt, atomizing to prepare powder, dissolving in sulfuric acid to remove Fe, filtering to obtain Pt and Re mixed powder, dissolving Re powder in nitric acid, filtering to obtain Pt powder and HReO powder₄Solution, then to HReO₄Solution additionKOH, filtering to obtain KReO₄Precipitating, and finally reducing hydrogen to obtain Re powder.

The method for recovering the platinum and rhenium from the waste alumina-based semi-regenerated reforming catalyst specifically comprises the following steps:

(1) material preparation and material mixing: uniformly mixing 100 parts of waste catalyst, 100 and 200 parts of fluxing agent, 5-20 parts of iron powder and 5-15 parts of carbon powder;

(2) smelting: smelting the uniformly mixed materials, and separating slag iron to obtain Fe-Pt-Re alloy melt and slag;

(3) atomizing to prepare powder: atomizing the Fe-Pt-Re alloy melt to obtain Fe-Pt-Re alloy powder;

(4) acid hydrolysis deferrization: dissolving Fe-Pt-Re alloy powder by using sulfuric acid to remove Fe, and filtering to obtain mixed powder of Pt powder and Re powder;

(5) separating platinum and rhenium: dissolving Re in the mixed powder of platinum and rhenium by using nitric acid, and filtering to obtain Pt powder and HReO₄Filtering the solution;

(6) and (3) precipitating rhenium: adding KOH to HReO₄Filtering the filtrate to obtain KReO₄A precipitate;

(7) reduction: hydrogen reduction of KReO₄Precipitating to obtain a mixture of KOH and Re powder;

(8) and (3) extracting rhenium: and washing and filtering the mixture of the KOH and the Re powder to obtain Re powder and a KOH solution, and recycling the KOH solution for precipitating rhenium.

Further, the fluxing agent in the step (1) is 50-80 parts of CaO, and B₂O₃Is 30-60 portions of Na₂CO₃20 to 60 portions.

Further, after the smelting in the step (2) is 1400-1600 ℃ smelting for 1-3h, the Fe-Pt-Re alloy melt and the slag are separated.

Further, the atomization in the step (3) gives Fe-Pt-Re alloy powder having an average particle size of 50 to 200 μm.

Further, the iron removal by acid hydrolysis in the step (4) is to dissolve Fe-Pt-Re alloy powder for 1 to 3 hours at room temperature of 90 ℃ below zero by using 3 to 8mol/L sulfuric acid with a solid-to-liquid ratio of 1:3 to 1:10, and then filtering the solution to obtain mixed powder of Pt powder and Re powder.

Further, the platinum rhenium separation in the step (5) is performed by using 2-6mol/L nitric acid and solidCarrying out acidolysis on Re for 1-3h at room temperature of-90 ℃ in a liquid ratio of 1:3-1:10, and filtering to obtain Pt powder and HReO₄The recovery rate of Pt in the filtrate is more than 99%.

Further, the rhenium precipitation in the step (6) adds KOH into the HReO₄Filtering the filtrate until the pH value is more than or equal to 8 to obtain KReO₄And (4) precipitating.

Further, the step (7) of extracting rhenium is KReO reduction by 800-₄The mixture of KOH and Re powder is obtained within 0.5-5h, and the recovery rate of Re is more than 98 percent.

The technical principle of the invention is as follows:

(1) in terms of Pt, Re reduction: according to the phase diagrams of Fe-Pt and Fe-Re alloys, Pt, Re and Fe form a solid solution, and the solid solution is reduced to form the Fe-Pt-Re alloy. Re in the waste catalyst is mainly Re₂O₇Form exists, is volatile at high temperature, and reacts at the temperature of 570-670 ℃ to form Ca (ReO) by adding CaO₄)₂Solidified in the system and then reduced into metal Re in a high-temperature melting system (1000-1600 ℃) to form Fe-Pt-Re alloy with Fe and Pt, thereby improving the recovery rate of Re. The chemical reaction equation involved is as follows:

Re₂O₇+CaO→Ca(ReO₄)₂

Ca(ReO₄)₂+7C→CaO+7CO↑+2Re

(2) in the aspect of slag type blending: according to Al₂O₃-CaO-B₂O₃Phase diagram at Al₂O₃The region with a content of 40-50 wt.% is a low temperature region (about 1200 deg.C), and is prepared by adding Na₂The low temperature zone of O can be further expanded, the melting point of the slag phase is reduced, when the melting temperature is 1400-1600 ℃, the viscosity of the slag phase is reduced to be less than 0.2 Pa.s, the good fluidity is achieved, and meanwhile, Na is used for reducing the viscosity of the slag phase to be lower than 0.2 Pa.s₂O、B₂O₃The method is beneficial to reducing the density of the slag phase, further improves the separation of the alloy and the slag phase, and finally improves the recovery rate of Pt and Re.

(3) In terms of platinum-rhenium separation: the Pt and Re mixed powder has fine granularity and high activity, and the Re is selectively dissolved by the nitric acid, so that the Pt and the Re are efficiently separated. The chemical reaction equation involved is as follows:

3Re+7HNO₃→3HReO₄+7NO↑+2H₂O

(4) in the aspects of rhenium precipitation and rhenium reduction: HReO₄KReO is formed after KOH is added into the solution₄Precipitating, and introducing hydrogen at high temperature to reduce to obtain Re powder and KOH. The chemical reaction equation involved is as follows:

HReO₄+KOH→KReO₄↓+H₂O

2HReO₄+7H₂→2Re+2KOH+6H₂O

the beneficial technical effects of the invention comprise:

(1) the platinum-rhenium synergistic high-efficiency recovery is realized by iron capture, the problems of low platinum-rhenium recovery rate and large wastewater amount in a wet process are solved, the problem that the Re is not recovered in the traditional pyrometallurgical enrichment process is solved, and the recovery rates of Pt and Re respectively exceed 99% and 98%;

(2) re in the platinum-rhenium mixed powder has high activity, and can be selectively dissolved by nitric acid, so that a theoretical basis and a technical support are provided for platinum-rhenium separation;

(3) the byproduct KOH obtained by reducing Re by hydrogen can be reused for precipitating rhenium;

(4) the combined process of the fire method and the wet method has the advantages of short flow, high recovery rate, low material consumption and energy consumption and the like, and is suitable for industrial production.

Drawings

FIG. 1 is a schematic process flow diagram of the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

On the contrary, the invention is intended to cover alternatives, modifications, equivalents and alternatives which may be included within the spirit and scope of the invention as defined by the appended claims. Furthermore, in the following detailed description of the present invention, certain specific details are set forth in order to provide a better understanding of the present invention. It will be apparent to one skilled in the art that the present invention may be practiced without these specific details.

Example 1

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 100 parts of fluxing agent, 5 parts of iron powder and 5 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 100 parts of fluxing agent is prepared from 50 parts of CaO and 30 parts of B₂O₃20 portions of Na₂CO₃And (4) forming. Smelting the mixture at 1600 ℃ for 1h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 50 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1h at 90 ℃ by adopting 3mol/L sulfuric acid with a solid-to-liquid ratio of 1:10, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 1h at 90 ℃ by using 2mol/L nitric acid and a solid-liquid ratio of 1:10, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 8 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 800 deg.C₄And (5) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.7 percent and the recovery rate of Re is 99.6 percent.

Example 2

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 110 parts of fluxing agent, 8 parts of iron powder and 6 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 110 parts of fluxing agent are prepared from 50 parts of CaO and 35 parts of B₂O₃25 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1600 ℃ for 1h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 60 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1h at 90 ℃ by adopting 3.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:10, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 1h at 90 ℃ by using 2.5mol/L nitric acid with a solid-to-liquid ratio of 1:10, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 8 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 850 deg.C₄And (4.5 h) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.5 percent and the recovery rate of Re is 98.9 percent.

Example 3

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 125 parts of fluxing agent, 10 parts of iron powder and 9 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 125 parts of fluxing agent are prepared from 55 parts of CaO and 40 parts of B₂O₃30 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1580 ℃ for 1.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 80 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1h at 80 ℃ by adopting 4mol/L sulfuric acid with a solid-to-liquid ratio of 1:9, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 1h at 80 ℃ by using 3mol/L nitric acid and a solid-to-liquid ratio of 1:9, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 9 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 900 deg.C₄And (4) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.4 percent and the recovery rate of Re is 98.6 percent.

Example 4

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 135 parts of fluxing agent, 12 parts of iron powder and 10 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 135 parts of fluxing agent are composed of 55 parts of CaO and 45 parts of B₂O₃35 parts of Na₂CO₃And (4) forming. Smelting the mixture for 1.5h at 1560 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 100 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1.5h at 70 ℃ by adopting 4.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:8, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 1.5h at 70 ℃ by using 3.5mol/L nitric acid and a solid-to-liquid ratio of 1:8, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 10 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 950 deg.C₄And (3.5 h) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.3 percent and the recovery rate of Re is 98.5 percent.

Example 5

100 parts of waste alumina-based semi-regenerated reforming catalyst containing platinum and rhenium, 150 parts of fluxing agent,Mixing 14 parts of iron powder and 12 parts of carbon powder uniformly to obtain a mixture, wherein 150 parts of fluxing agent is composed of 60 parts of CaO and 50 parts of B₂O₃40 parts of Na₂CO₃And (4) forming. Smelting the mixture for 2h at 1520 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 120 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 2h at 60 ℃ by adopting 5mol/L sulfuric acid and a solid-liquid ratio of 1:7, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2 hours at 60 ℃ by using 4mol/L nitric acid and a solid-to-liquid ratio of 1:7, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 11 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1000 deg.C₄And 3h, obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.5 percent and the recovery rate of Re is 98.8 percent.

Example 6

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 160 parts of fluxing agent, 16 parts of iron powder and 15 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 160 parts of fluxing agent comprise 60 parts of CaO and 55 parts of B₂O₃45 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1500 ℃ for 2h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 140 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 2.5h at 40 ℃ by adopting 6mol/L sulfuric acid and a solid-liquid ratio of 1:5, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2.5h at 50 ℃ and with 4.5mol/L nitric acid and a solid-to-liquid ratio of 1:6, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 12 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1050 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 2.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.6 percent and the recovery rate of Re is 99.2 percent.

Example 7

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 175 parts of fluxing agent, 18 parts of iron powder and 7 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 175 parts of fluxing agent are formed by 65 parts of CaO, CaO and the like,60 parts of B₂O₃50 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1480 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 160 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at 30 ℃ by adopting 7mol/L sulfuric acid and a solid-liquid ratio of 1:4, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2.5h at 40 ℃ by using 5mol/L nitric acid and a solid-to-liquid ratio of 1:5, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 13 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1100 deg.C₄And (3) obtaining a mixture of Re powder and KOH after 2h, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.7 percent and the recovery rate of Re is 99.4 percent.

Example 8

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 150 parts of fluxing agent, 20 parts of iron powder and 8 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 150 parts of fluxing agent are prepared from 65 parts of CaO and 30 parts of B₂O₃55 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1500 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 180 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at room temperature by adopting 7.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:3, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 3 hours at 30 ℃ by using 5.5mol/L nitric acid and a solid-to-liquid ratio of 1:4, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1150 deg.C₄Obtaining a mixture of Re powder and KOH after 1 hour, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.9 percent and the recovery rate of Re is 99.8 percent.

Example 9

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 165 parts of fluxing agent, 6 parts of iron powder and 11 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 165 parts of fluxing agent are prepared from 70 parts of CaO and 35 parts of B₂O₃60 parts of Na₂CO₃And (4) forming. Subjecting the mixture toSmelting at 1540 ℃ for 2h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 200 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3 hours at room temperature by using 8mol/L sulfuric acid with a solid-to-liquid ratio of 1:3, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 3 hours at room temperature by using 6mol/L nitric acid with the solid-to-liquid ratio of 1:3, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1200 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 0.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.2 percent and the recovery rate of Re is 98.2 percent.

Example 10

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 130 parts of fluxing agent, 7 parts of iron powder and 13 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 130 parts of fluxing agent are prepared from 70 parts of CaO and 40 parts of B₂O₃20 portions of Na₂CO₃And (4) forming. Smelting the mixture for 1.5h at 1560 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 70 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1h at 80 ℃ by adopting 4mol/L sulfuric acid with a solid-to-liquid ratio of 1:9, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 1h at 90 ℃ by using 2.5mol/L nitric acid with a solid-to-liquid ratio of 1:10, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 8 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 850 deg.C₄And (4.5 h) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.3 percent and the recovery rate of Re is 98.3 percent.

Example 11

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 145 parts of fluxing agent, 9 parts of iron powder and 14 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 145 parts of fluxing agent is prepared from 75 parts of CaO and 45 parts of B₂O₃25 parts of Na₂CO₃And (4) forming. The mixture is smelted for 1.5h at 1580 ℃, slag is separated to obtain Fe-Pt-Re alloy melt, and the average granularity is obtained by atomization90 μm Fe-Pt-Re alloy powder. Carrying out acidolysis on Fe-Pt-Re alloy powder for 2h at 60 ℃ by adopting 5mol/L sulfuric acid and a solid-liquid ratio of 1:8, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 1.5h at 70 ℃ by using 3.5mol/L nitric acid and a solid-to-liquid ratio of 1:8, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 10 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 900 deg.C₄And (4) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.4 percent and the recovery rate of Re is 98.4 percent.

Example 12

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 155 parts of fluxing agent, 11 parts of iron powder and 5 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 155 parts of fluxing agent is prepared from 75 parts of CaO and 50 parts of B₂O₃30 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1540 ℃ for 2h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 110 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 2h at 50 ℃ by adopting 5.5mol/L sulfuric acid and a solid-liquid ratio of 1:8, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2 hours at 60 ℃ by using 4mol/L nitric acid and a solid-to-liquid ratio of 1:7, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 11 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 950 deg.C₄And (3.5 h) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.5 percent and the recovery rate of Re is 98.6 percent.

Example 13

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 170 parts of fluxing agent, 13 parts of iron powder and 6 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 170 parts of fluxing agent is composed of 80 parts of CaO and 55 parts of B₂O₃35 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1480 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 130 mu m. 6mol/L sulfuric acid is adopted to carry out acidolysis on Fe-Pt-Re alloy at 40 ℃ with the solid-liquid ratio of 1:5And (5) filtering the powder for 2.5h to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2.5h at 50 ℃ and with 4.5mol/L nitric acid and a solid-to-liquid ratio of 1:6, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 12 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1000 deg.C₄And 3h, obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.6 percent and the recovery rate of Re is 98.8 percent.

Example 14

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 180 parts of fluxing agent, 15 parts of iron powder and 9 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 180 parts of fluxing agent is composed of 80 parts of CaO and 60 parts of B₂O₃40 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1460 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 150 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at 30 ℃ by adopting 6.5mol/L sulfuric acid and a solid-liquid ratio of 1:4, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2.5h at 40 ℃ by using 5mol/L nitric acid and a solid-to-liquid ratio of 1:5, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 13 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1050 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 2.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.7 percent and the recovery rate of Re is 99.2 percent.

Example 15

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 100 parts of fluxing agent, 17 parts of iron powder and 10 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 100 parts of fluxing agent is prepared from 50 parts of CaO and 30 parts of B₂O₃20 portions of Na₂CO₃And (4) forming. Smelting the mixture at 1600 ℃ for 1h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 170 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at 30 ℃ by adopting 7mol/L sulfuric acid and a solid-liquid ratio of 1:4, and filtering to obtain mixed powder of Pt powder and Re powder. Then 5.5mol/L nitric acid and solid liquid are usedCarrying out acidolysis on Re powder for 3h at 30 ℃ in a ratio of 1:4, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1100 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 1.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.8 percent and the recovery rate of Re is 99.4 percent.

Example 16

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 115 parts of fluxing agent, 19 parts of iron powder and 12 parts of carbon powder are uniformly mixed to obtain a mixed material, wherein the 115 parts of fluxing agent comprise 55 parts of CaO and 35 parts of B₂O₃25 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1580 ℃ for 1.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 190 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at room temperature by adopting 7.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:3, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 3 hours at room temperature by using 6mol/L nitric acid with the solid-to-liquid ratio of 1:3, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1150 deg.C₄Obtaining a mixture of Re powder and KOH after 1 hour, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.8 percent and the recovery rate of Re is 99.6 percent.

Example 17

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 130 parts of fluxing agent, 6 parts of iron powder and 15 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 130 parts of fluxing agent comprise 60 parts of CaO and 40 parts of B₂O₃30 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1500 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 200 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3 hours at room temperature by using 8mol/L sulfuric acid with a solid-to-liquid ratio of 1:3, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 3 hours at room temperature by using 6mol/L nitric acid with the solid-to-liquid ratio of 1:3, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HR with KOHeO₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1200 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 0.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.0 percent and the recovery rate of Re is 98.1 percent.

Example 18

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 145 parts of fluxing agent, 7 parts of iron powder and 7 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 145 parts of fluxing agent is prepared from 65 parts of CaO and 45 parts of B₂O₃35 parts of Na₂CO₃And (4) forming. Smelting the mixture for 2.5h at 1520 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 60 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1h at 90 ℃ by adopting 3.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:10, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 1h at 90 ℃ by using 2.5mol/L nitric acid with a solid-to-liquid ratio of 1:10, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 8 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 850 deg.C₄And (4.5 h) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.1 percent and the recovery rate of Re is 98.3 percent.

Example 19

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 170 parts of fluxing agent, 9 parts of iron powder and 8 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 170 parts of fluxing agent is prepared from 70 parts of CaO and 50 parts of B₂O₃50 parts of Na₂CO₃And (4) forming. The mixture is smelted for 3 hours at 1420 ℃, slag is separated to obtain Fe-Pt-Re alloy melt, and Fe-Pt-Re alloy powder with the average particle size of 80 mu m is obtained through atomization. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1h at 80 ℃ by adopting 4mol/L sulfuric acid with a solid-to-liquid ratio of 1:9, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 1h at 80 ℃ by using 3mol/L nitric acid and a solid-to-liquid ratio of 1:9, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 9 to obtain KReO₄And (4) precipitating. Hydrogen reduction KRe at 900 deg.CO₄And (4) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.2 percent and the recovery rate of Re is 98.4 percent.

Example 20

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 185 parts of fluxing agent, 11 parts of iron powder and 11 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 185 parts of fluxing agent are composed of 75 parts of CaO and 55 parts of B₂O₃55 parts of Na₂CO₃And (4) forming. Smelting the mixture for 3h at 1400 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 100 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 1.5h at 70 ℃ by adopting 4.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:8, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 1.5h at 70 ℃ by using 3.5mol/L nitric acid and a solid-to-liquid ratio of 1:8, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 10 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 950 deg.C₄And (3.5 h) obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.3 percent and the recovery rate of Re is 98.5 percent.

Example 21

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 200 parts of fluxing agent, 13 parts of iron powder and 13 parts of carbon powder are uniformly mixed to obtain a mixture, wherein 200 parts of fluxing agent is composed of 80 parts of CaO and 60 parts of B₂O₃60 parts of Na₂CO₃And (4) forming. Smelting the mixture for 3h at 1400 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 120 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 2h at 60 ℃ by adopting 5mol/L sulfuric acid and a solid-liquid ratio of 1:7, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2 hours at 60 ℃ by using 4mol/L nitric acid and a solid-to-liquid ratio of 1:7, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 11 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1000 deg.C₄And 3h, obtaining a mixture of Re powder and KOH, washing with water, and filtering to obtain Re powder and a KOH solution. KOH solutionAnd the liquid is reused for the rhenium precipitation process. The recovery rate of Pt is 99.4 percent and the recovery rate of Re is 98.8 percent.

Example 22

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 150 parts of fluxing agent, 15 parts of iron powder and 14 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 150 parts of fluxing agent are composed of 50 parts of CaO and 45 parts of B₂O₃55 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1500 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 140 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 2.5h at 40 ℃ by adopting 6mol/L sulfuric acid and a solid-liquid ratio of 1:5, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2.5h at 50 ℃ and with 4.5mol/L nitric acid and a solid-to-liquid ratio of 1:6, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 12 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1050 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 2.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.4 percent and the recovery rate of Re is 99.2 percent.

Example 23

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 165 parts of fluxing agent, 17 parts of iron powder and 11 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 165 parts of fluxing agent are prepared from 55 parts of CaO and 50 parts of B₂O₃60 parts of Na₂CO₃And (4) forming. Smelting the mixture at 1480 ℃ for 2.5h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 160 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at 30 ℃ by adopting 7mol/L sulfuric acid and a solid-liquid ratio of 1:4, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 2.5h at 40 ℃ by using 5mol/L nitric acid and a solid-to-liquid ratio of 1:5, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 13 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1100 deg.C₄And (3) obtaining a mixture of Re powder and KOH after 2h, washing with water, and filtering to obtain Re powder and a KOH solution. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.5 percent and the recovery rate of Re is 99.5 percent.

Example 24

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 170 parts of fluxing agent, 19 parts of iron powder and 13 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 170 parts of fluxing agent are prepared from 60 parts of CaO and 55 parts of B₂O₃55 parts of Na₂CO₃And (4) forming. And smelting the mixture at 1440 ℃ for 3h, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 180 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3h at room temperature by adopting 7.5mol/L sulfuric acid with a solid-to-liquid ratio of 1:3, and filtering to obtain mixed powder of Pt powder and Re powder. Carrying out acidolysis on Re powder for 3 hours at 30 ℃ by using 5.5mol/L nitric acid and a solid-to-liquid ratio of 1:4, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1150 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 1.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.7 percent and the recovery rate of Re is 99.8 percent.

Example 25

100 parts of waste alumina-based semi-regenerative reforming catalyst containing platinum and rhenium, 185 parts of fluxing agent, 20 parts of iron powder and 14 parts of carbon powder are uniformly mixed to obtain a mixture, wherein the 185 parts of fluxing agent are prepared from 65 parts of CaO and 60 parts of B₂O₃60 parts of Na₂CO₃And (4) forming. Smelting the mixture for 3h at 1400 ℃, separating slag to obtain Fe-Pt-Re alloy melt, and atomizing to obtain Fe-Pt-Re alloy powder with the average particle size of 200 mu m. Carrying out acidolysis on Fe-Pt-Re alloy powder for 3 hours at room temperature by using 8mol/L sulfuric acid with a solid-to-liquid ratio of 1:3, and filtering to obtain mixed powder of Pt powder and Re powder. Then carrying out acidolysis on Re powder for 3 hours at room temperature by using 6mol/L nitric acid with the solid-to-liquid ratio of 1:3, and filtering to obtain Pt powder and HReO₄And (6) filtering the solution. Regulation of HReO with KOH₄Filtering the filtrate until the pH value is 14 to obtain KReO₄And (4) precipitating. Hydrogen reduction of KReO at 1200 deg.C₄And (5) obtaining a mixture of Re powder and KOH after 0.5h, and obtaining Re powder and KOH solution after washing and filtering. The KOH solution is reused for the rhenium precipitation process. The recovery rate of Pt is 99.8 percent and the recovery rate of Re is 99.7 percent.