CN108277350A - A method of recycling platinum and rhenium from failure alumina base platinum-rhenium catalyst - Google Patents
A method of recycling platinum and rhenium from failure alumina base platinum-rhenium catalyst Download PDFInfo
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- CN108277350A CN108277350A CN201810116294.2A CN201810116294A CN108277350A CN 108277350 A CN108277350 A CN 108277350A CN 201810116294 A CN201810116294 A CN 201810116294A CN 108277350 A CN108277350 A CN 108277350A
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- rhenium
- platinum
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- failure
- alumina base
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to a kind of methods that platinum and rhenium are recycled in alumina base platinum-rhenium catalyst from failure, specifically comprise the following steps,（1）Roasting（2）Acidleach（3）Resin adsorption（4）Stripping liquid complexing is handled（5）Stripping liquid controlling potential platinum electrodeposition（6）Controlling potential electro-deposition rhenium；The present invention sinks platinum, heavy rhenium respectively using the method for controlling potential electro-deposition, pure platinum powder and rhenium powder are obtained, achievees the purpose that platinum and rhenium efficiently separate, reduces ammonium chloroplatinate and ammonium perrhenate precipitation, calcination process, technological process is short, metal recovery rate is high, and reagent consumption is few, environmental-friendly, and compared with conventional calcination method, the platinum powder and rhenium powder large specific surface area, powder purity of electro-deposition preparation are high, and chemism is high, highly beneficial to follow-up prepare compound.
Description
Technical field
The present invention relates to precious and rare metals recovery fields, and in particular to a kind of to be recycled from the alumina base platinum-rhenium catalyst that fails
The method of platinum and rhenium.
Background technology
Platinum group metal and rare metal rhenium, due to the uniqueness of performance and the scarcity of resource, by many flourishing states of the world
Family is classified as " strategic reserves metal ", is widely used in each industrial circle, is referred to as " king of catalysis ", " modern industry vitamin ".
China is the poor state of resource of platinum group metal and dilute scattered rhenium, largely relies on import.For the Pt/Re catalyst of petroleum reforming, use
Catalytic activity can be lost after a certain period of time, it is necessary to be substituted, thus generate a large amount of failure platinum-rhenium catalyst, recovery value is huge
Greatly.Therefore implement platinum-rhenium catalyst secondary resource recycling utilization, resource can not only be made to be fully used, and be conducive to
Environmental security meets the requirement of " green economy ".
There are two main classes for the technique of recycling valuable metal platinum and rhenium from failure platinum-rhenium catalyst, and the first kind is active component
Dissolution method dissolves out metal platinum and rhenium with solvent selectivity, and alumina catalyst support is insoluble, and platinum and rhenium, the work are extracted after separation of solid and liquid
The shortcomings that skill is meeting residual metal platinum and rhenium in carrier, therefore the rate of recovery of platinum and rhenium is relatively low.Second class is complete molten method, is used
Different solvent substeps all dissolve active component platinum, rhenium and alumina support, after separation of solid and liquid, then using chemical method separation
It extracts platinum and rhenium, this method metal recovery rate is relatively high.
The main method that the Pt/Re alumina bases of China's recycling at present reform dead catalyst is to use complete molten method technique, this
Technique has been carried out industrial applications in China, but there are many problems for complete molten method technique, such as：The technological process of platinum rhenium separation
Very complicated, technological process is long, and platinum rhenium is difficult to be kept completely separate；Platinum rhenium eutectoid content so that the adsorption capacity of resin for platinum declines,
Reduce the organic efficiency of platinum；The anion species contained in the waste water generated after absorption platinum rhenium are excessive, it is difficult to recycle, ring
Border pollution etc..
Patent 2009119A discloses the recovery method of rhenium and platinum in a kind of failure petrochemical industry reforming catalyst, main to wrap
It includes alkali and leaches rhenium, separation platiniferous insoluble slag, resin adsorption rhenium, elution recycling rhenium, recycling platinum.Patent CN 103388077
A disclose it is a kind of failure petrochemical industry reforming catalyst in rhenium, platinum and aluminium comprehensive reutilization method, mainly include abrasive material,
Pressurization alkali soluble, refining carry rhenium, acid molten, platinum refining, sulfuric acid alum recovery.
Invention content
To solve technical problem present in background technology, that the purpose of the present invention is to provide a kind of metal recovery rates is high,
The environmentally protective method that platinum and rhenium are recycled from failure alumina base platinum-rhenium catalyst.
To achieve the above object, the present invention provides the following technical solutions：
A method of recycling platinum and rhenium from failure alumina base platinum-rhenium catalyst include the following steps：
（1）Roasting
Failure alumina base platinum-rhenium catalyst is placed in Muffle furnace, constant temperature calcining 2-4h removes the surface in spent catalyst
Carbon deposit；
（2）Acidleach
Sulfuric acid reaction 1-2h is added, dissolves alumina support, adds hydrochloric acid and sodium chlorate or hydrochloric acid and hydrogen peroxide, oxidation leaching
Go out the platinum and rhenium in catalyst, 60-100 DEG C of extraction temperature, then extraction time 6-8h is filtered, filtrate is the molten of platiniferous and rhenium
Liquid；
（3）Resin adsorption
By step（2）The solution of obtained platiniferous and rhenium is adsorbed by resin anion (R.A.), and solution pH value is 3.5-6.0, when absorption
Between 30-60min, then desorb elution with the ammonium hydroxide or sodium hydroxide of 5%-15%, the concentration of platinum reaches 30-40g/L in eluent,
The concentration of rhenium reaches 15-20g/L；
（4）Stripping liquid complexing is handled
Complexing agent is added in stripping liquid, makes a concentration of 15-35mg/L of solution complexing agent, then 45-60 DEG C of reaction 60-
120min；
（5）Stripping liquid controlling potential platinum electrodeposition
Resin desorption liquid is transferred in electrolytic cell, electrode is made using inert anode, current density 350-600A/m2, interpolar away from
From 30-60mm, tune PH is 6.5-8.0, controlled at 35-65 DEG C, controls cathode potential 0.55V ~ 0.65V；
（6）Controlling potential electro-deposition rhenium
By step（5）Solution filtering after heavy platinum, filtrate are transferred in electrolytic cell, make electrode, current density using inert anode
300-500A/m2, interpolar distance 30-55mm, tune PH is 6.5-8.0, controlled at 35-65 DEG C, control cathode potential 0.4V ~
0.6V。
Further, the step（1）Middle calcination temperature is 200-350 DEG C, effectively avoids the volatilization of rhenium in catalyst
Loss.
Further, the step（2）Middle sulfuric acid, hydrochloric acid and sodium chlorate addition be respectively catalyst weight 55-75%,
25-30%, 10-15% or sulfuric acid, hydrochloric acid, hydrogen peroxide addition are respectively 55-75%, 25-30%, 10- of catalyst weight
15%。
Further, step（4）Complexing agent is ethylenediamine tetra-acetic acid either one kind of iminodiacetic acid or two kinds.
Beneficial effects of the present invention：
The present invention sinks platinum, heavy rhenium respectively using the method for controlling potential electro-deposition, obtains pure platinum powder and rhenium powder, reaches platinum and rhenium is high
The purpose for imitating separation reduces ammonium chloroplatinate and ammonium perrhenate precipitation, calcination process, and technological process is short, and metal recovery rate is high, examination
Agent consumption is few, environmental-friendly, and compared with conventional calcination method, platinum powder and rhenium powder large specific surface area, powder prepared by electro-deposition
Purity is high, and chemism is high, highly beneficial to follow-up prepare compound.
Description of the drawings
Fig. 1 is the flow chart of the present invention.
Specific implementation mode
Embodiment 1
A method of recycling platinum and rhenium from failure alumina base platinum-rhenium catalyst include the following steps：
（1）Roasting
Failure alumina base platinum-rhenium catalyst is placed in Muffle furnace, setting temperature is 200 DEG C, constant temperature calcining 4h, removes failure
Surface carbon deposit in catalyst improves metal recovery rate in favor of the leaching of follow-up platinum and rhenium；
（2）Acidleach
The sulfuric acid reaction 2h of catalyst weight 55% is added, dissolves alumina support；Add catalyst weight 25% hydrochloric acid and
The sodium chlorate of catalyst weight 10%, platinum and rhenium in Oxidation Leaching catalyst, 100 DEG C, extraction time 6h of extraction temperature, then
Filtering, filtrate are the solution of platiniferous and rhenium, the concentration point of wherein chloroplatinic acid radical ion PtCl62- and high rhenium acid group ion ReO4-
It Wei not 0.30g/L and 0.20g/L；
（3）Resin adsorption
By step（2）The solution of obtained platiniferous and rhenium is adsorbed by resin anion (R.A.), and solution pH value is 3.5, adsorption time
30min, then eluted with 15% ammonium hydroxide or sodium hydroxide desorption, the concentration of platinum reaches 30g/L in eluent, and the concentration of rhenium reaches
To 15g/L；
（4）Stripping liquid complexing is handled
Complexing agent ethylenediamine tetra-acetic acid is added in stripping liquid, makes a concentration of 15mg/L of ethylenediamine tetra-acetic acid in solution, 45 DEG C
React 120min；
（5）Stripping liquid controlling potential platinum electrodeposition
Resin desorption liquid is transferred in electrolytic cell, electrode, current density 350A/m2, interpolar distance are made using inert anode
30mm, it is 6.5 to adjust PH, controlled at 35 DEG C, controls cathode potential 0.55V；
（6）Controlling potential electro-deposition rhenium
By step（5）Solution filtering after heavy platinum, filtrate are transferred in electrolytic cell, make electrode, current density using inert anode
300A/m2, interpolar distance 30mm, it is 6.5 to adjust PH, controlled at 35 DEG C, controls cathode potential 0.4V.
Embodiment 2
A method of recycling platinum and rhenium from failure alumina base platinum-rhenium catalyst include the following steps：
（1）Roasting
Failure alumina base platinum-rhenium catalyst is placed in Muffle furnace, setting temperature is 350 DEG C, constant temperature calcining 2h, removes failure
Surface carbon deposit in catalyst improves metal recovery rate in favor of the leaching of follow-up platinum and rhenium；
（2）Acidleach
The sulfuric acid reaction 1h of catalyst weight 75% is added, dissolves alumina support；Add catalyst weight 30% hydrochloric acid and
The hydrogen peroxide of catalyst weight 15%, platinum and rhenium in Oxidation Leaching catalyst, 60 DEG C, extraction time 8h of extraction temperature, then mistake
Filter, filtrate are the solution of platiniferous and rhenium, the concentration difference of wherein chloroplatinic acid radical ion PtCl62- and high rhenium acid group ion ReO4-
For 0.50g/L and 0.35g/L；
（3）Resin adsorption
By step（2）The solution of obtained platiniferous and rhenium is adsorbed by resin anion (R.A.), and solution pH value is 6.0, adsorption time
60min, then eluted with 5% ammonium hydroxide or sodium hydroxide desorption, the concentration of platinum reaches 40g/L in eluent, and the concentration of rhenium reaches
20g/L；
（4）Stripping liquid complexing is handled
Complexing agent iminodiacetic acid is added in stripping liquid, makes a concentration of 35mg/L of iminodiacetic acid in solution, 60 DEG C
React 60min；
（5）Stripping liquid controlling potential platinum electrodeposition
Resin desorption liquid is transferred in electrolytic cell, electrode, current density 600A/m2, interpolar distance are made using inert anode
60mm, it is 8.0 to adjust PH, controlled at 65 DEG C, controls cathode potential 0.65V；
（6）Controlling potential electro-deposition rhenium
By step（5）Solution filtering after heavy platinum, filtrate are transferred in electrolytic cell, make electrode, current density using inert anode
500A/m2, interpolar distance 55mm, it is 8.0 to adjust PH, controlled at 65 DEG C, controls cathode potential 0.6V.
Embodiment 3
A method of recycling platinum and rhenium from failure alumina base platinum-rhenium catalyst include the following steps：
（1）Roasting
Failure alumina base platinum-rhenium catalyst is placed in Muffle furnace, setting temperature is 300 DEG C, constant temperature calcining 1.5h, removes and loses
The surface carbon deposit in catalyst is imitated, in favor of the leaching of follow-up platinum and rhenium, improves metal recovery rate；
（2）Acidleach
The sulfuric acid reaction 1.5h of catalyst weight 65% is added, dissolves alumina support；Add the hydrochloric acid of catalyst weight 25%
With the sodium chlorate of catalyst weight 15%, platinum and rhenium in Oxidation Leaching catalyst, 80 DEG C, extraction time 7h of extraction temperature, then
Filtering, filtrate are the solution of platiniferous and rhenium, the concentration point of wherein chloroplatinic acid radical ion PtCl62- and high rhenium acid group ion ReO4-
It Wei not 0.40g/L and 0.3g/L；
（3）Resin adsorption
By step（2）The solution of obtained platiniferous and rhenium is adsorbed by resin anion (R.A.), and solution pH value is 5.0, adsorption time
45min, then eluted with 10% ammonium hydroxide or sodium hydroxide desorption, the concentration of platinum reaches 35g/L in eluent, and the concentration of rhenium reaches
To 18g/L；
（4）Stripping liquid complexing is handled
Complexing agent iminodiacetic acid is added in stripping liquid, makes a concentration of 25mg/L of iminodiacetic acid in solution, 50 DEG C
React 90min；
（5）Stripping liquid controlling potential platinum electrodeposition
Resin desorption liquid is transferred in electrolytic cell, electrode, current density 500A/m2, interpolar distance are made using inert anode
50mm, it is 7.0 to adjust PH, controlled at 50 DEG C, controls cathode potential 0.60V；
（6）Controlling potential electro-deposition rhenium
By step（5）Solution filtering after heavy platinum, filtrate are transferred in electrolytic cell, make electrode, current density using inert anode
400A/m2, interpolar distance 45mm, it is 7.0 to adjust PH, controlled at 50 DEG C, controls cathode potential 0.5V.
Claims (4)
1. a kind of method for recycling platinum and rhenium in alumina base platinum-rhenium catalyst from failure, which is characterized in that include the following steps：
（1）Roasting
Failure alumina base platinum-rhenium catalyst is placed in Muffle furnace, constant temperature calcining 2-4h removes the surface in spent catalyst
Carbon deposit；
（2）Acidleach
Sulfuric acid reaction 1-2h is added, dissolves alumina support, adds hydrochloric acid and sodium chlorate or hydrochloric acid and hydrogen peroxide, oxidation leaching
Go out the platinum and rhenium in catalyst, 60-100 DEG C of extraction temperature, then extraction time 6-8h is filtered, filtrate is the molten of platiniferous and rhenium
Liquid；
（3）Resin adsorption
By step（2）The solution of obtained platiniferous and rhenium is adsorbed by resin anion (R.A.), and solution pH value is 3.5-6.0, when absorption
Between 30-60min, then desorb elution with the ammonium hydroxide or sodium hydroxide of 5%-15%, the concentration of platinum reaches 30-40g/L in eluent,
The concentration of rhenium reaches 15-20g/L；
（4）Stripping liquid complexing is handled
Complexing agent is added in stripping liquid, makes a concentration of 15-35mg/L of solution complexing agent, then solution is anti-at 45-60 DEG C
Answer 60-120min；
（5）Stripping liquid controlling potential platinum electrodeposition/
Resin desorption liquid is transferred in electrolytic cell, electrode is made using inert anode, current density 350-600A/m2, interpolar away from
From 30-60mm, tune PH is 6.5-8.0, controlled at 35-65 DEG C, controls cathode potential 0.55V ~ 0.65V；
（6）Controlling potential electro-deposition rhenium
By step（5）Solution filtering after heavy platinum, filtrate are transferred in electrolytic cell, make electrode, current density using inert anode
300-500A/m2, interpolar distance 30-55mm, tune PH is 6.5-8.0, controlled at 35-65 DEG C, control cathode potential 0.4V ~
0.6V。
2. the method for recycling platinum and rhenium in a kind of alumina base platinum-rhenium catalyst from failure according to claim 1, special
Sign is：Step（1）Middle calcination temperature is 200-350 DEG C.
3. the method for recycling platinum and rhenium in a kind of alumina base platinum-rhenium catalyst from failure according to claim 1, special
Sign is：Step（2）Middle sulfuric acid, hydrochloric acid, sodium chlorate addition are respectively 55-75%, 25-30%, 10-15% of catalyst weight,
Or sulfuric acid, hydrochloric acid, hydrogen peroxide addition are respectively 55-75%, 25-30%, 10-15% of catalyst weight.
4. the method for recycling platinum and rhenium in a kind of alumina base platinum-rhenium catalyst from failure according to claim 1, special
Sign is：Step（4）Complexing agent is ethylenediamine tetra-acetic acid either one kind of iminodiacetic acid or two kinds.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113215590A (en) * | 2021-04-25 | 2021-08-06 | 郴州百一环保高新材料有限公司 | Platinum element extraction process for waste ternary catalyst based on electrolytic reaction |
| CN113564367A (en) * | 2021-08-09 | 2021-10-29 | 北京化工大学 | Method for recovering silver and rhenium from waste ethylene oxide catalyst |
| 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 |
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| CN107034360A (en) * | 2017-06-14 | 2017-08-11 | 贵研资源（易门）有限公司 | The method that silver and rhenium are reclaimed from failure epoxyethane catalyst |
| CN107267772A (en) * | 2017-05-26 | 2017-10-20 | 核工业北京化工冶金研究院 | A kind of method that platinum and rhenium are reclaimed in the platinum-rhenium reforming catalyst from aluminium base |
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| CN1769504A (en) * | 2004-11-04 | 2006-05-10 | 日矿金属株式会社 | Method of recovering platinum and rhenium from waste catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113215590A (en) * | 2021-04-25 | 2021-08-06 | 郴州百一环保高新材料有限公司 | Platinum element extraction process for waste ternary catalyst based on electrolytic reaction |
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| CN113564367B (en) * | 2021-08-09 | 2022-03-11 | 北京化工大学 | Method for recovering silver and rhenium from waste ethylene oxide catalyst |
| 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 |
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