CN101534948A - Method of extracting platinum group metals from waste catalists through electrochemical process - Google Patents

Method of extracting platinum group metals from waste catalists through electrochemical process Download PDF

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CN101534948A
CN101534948A CNA2007800419687A CN200780041968A CN101534948A CN 101534948 A CN101534948 A CN 101534948A CN A2007800419687 A CNA2007800419687 A CN A2007800419687A CN 200780041968 A CN200780041968 A CN 200780041968A CN 101534948 A CN101534948 A CN 101534948A
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platinum group
electrolyte
negative electrode
metal
electrode
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CN101534948B (en
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秦仁洙
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JIN In Soo
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/68—Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/90—Regeneration or reactivation
    • B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
    • 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
    • C22B11/06—Chloridising
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/045—Leaching using electrochemical processes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
    • 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

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Abstract

A method of extracting platinum group metals from waste catalysts through an electrochemical process is disclosed. The extracting method includes positioning the waste catalysts between both electrodes in an electrolytic cell, leaching the platinum group metals as regularly changing polarities of the electrodes to each other, and precipitating the platinum group metals on a cathode by circulating the electrolyte from an anode to a cathode. According to the method, the platinum group metals can be extracted with high efficiency and high yield. Also, the extracting process is simplified to remarkably reduce costs required to extract the platinum group metals.

Description

From dead catalyst, extract the method for platinum group metal by electrochemical process
Technical field
The present invention relates to from dead catalyst, extract the method for noble metal by electrochemical process.
Background technology
The platinum group metal (PGMs) that comprises Pt and Pd has the unique chemical characteristic, for example catalytic reduction and high-melting-point and excellent chemical resistance.World's average year output of platinum group metal is about 200 tons, wherein surpasses this metal of 90% and originates in the South Africa and the former Soviet Union, and about 6% originates in Canada, and remaining originates in the U.S., Australia, Japan etc.Except the catalyst as Electrical and Electronic industry such as platinum group metal circuit, the platinum group metal also is used as the catalyst of motor vehicle and petrochemical industry.
The performance of catalyst and its component as time passes and deterioration.When their end-of-life, they are finally discarded.Especially, because the platinum group metal is expensive and all amounts all are imports, so the recovery of dead catalyst and recirculation are useful economically, and utilization has important function to resources effective.
Though the noble metal that is contained in the catalyst carrier for recovery has proposed several method, they have himself technical advantage and inferior position.Especially, because the ionization potential of platinum group metal is very high, so described metal itself is difficult to dissolving.In addition, because catalyst carrier, other catalyst component and pollution, so be difficult to extract and separate the platinum group metal.
Usually, the bullion content of dead catalyst is about 0.02%～about 5.0%.Disclose by pulverizing dead catalyst and electrolysis and be contained in crushing catalyst in the electrolytic cell that is filled with electrolyte and has anion-exchange membrane to extract platinum (Pt), palladium (Pb), rhodium (Rh) and alloy thereof from dead catalyst method.Yet anion-exchange membrane is very expensive, and owing to the life-span of film shortens because of the chlorine precipitation that occurs in the extraction process, so this film should often be changed.In addition, because the concentration of noble metal is low in the liquid that extracts, thus the separate complex of noble metal, and the technology cost increases with the prolongation of extraction time.In addition, described technology should comprise many treatment steps.
Usually working concentration is that 5～35% hydrochloric acid (HCl) solution is as electrolyte.In the fixedly filter course of spent catalyst particles, leach, perhaps in fluid layer, leach when leaching material layer in circulate electrolyte.Then, noble metal is reduced by carbon granule by the solution encirclement in the cathode chamber of second electrolytic cell with cation-exchange membrane.At last, be deposited in the fluid layer once more by electrodissolution effect noble metal.
From being undertaken by leaching the platinum group metal simultaneously and the platinum group metal being deposited in the charged negative electrode such as the current method of extracting the platinum group metal the inorganic substances such as dead catalyst, sludge, concentrate.Some shortcomings of this method are that it only can obtain limited concentration in filtering solution; And because utilizing, it separates the technology modules that is provided with, so complex process.
Summary of the invention
Technical problem
Therefore, in view of the above problems, finished the present invention.
An object of the present invention is to provide the method for extracting the platinum group metal by electrochemical process from dead catalyst, this method has improved productivity ratio in simple and economic mode.
Technical scheme
In order to realize above-mentioned and other purpose, according to embodiments more of the present invention, the method of extracting the platinum group metal by electrochemical process from dead catalyst is provided, described method comprises: dead catalyst is placed between two electrodes of electrolyte, along with the polarity that changes electrode regularly mutually leaches the platinum group metal and by making electrolyte be circulated to negative electrode from anode the platinum group metal is deposited on the negative electrode.
In one embodiment of the invention, electrolyte comprises that concentration is 0.3～10.0% hydrochloric acid solution.
Electrochemistry leaches and activates by the multipole utmost point (multi-pole reverse electrodes), and the described multipole utmost point is in electrode is converted under the multipole electrode state that can cause all metal material anodic solutions.
Electrolyte is circulated to negative electrode with the speed that the chloride anionic complex of hydration (hydrated anionicchloride complex) that is enough to prevent noble metal flows on the negative electrode from anode.
Beneficial effect
The method of extracting the platinum group metal from dead catalyst of some embodiments according to the present invention can be extracted the platinum group metal with high efficiency and high yield.And, simplified extraction process, significantly reduce thus and extract the required cost in platinum group metal.In addition, extracting the platinum group metal from dead catalyst is very useful for the platinum group metal that all amounts of recirculation are import.
Description of drawings
In conjunction with the accompanying drawings, from following detailed description, aforementioned and other purposes, feature and advantage of the present invention will become more obvious.
Fig. 1 schematically shows the view that is used for extracting from dead catalyst the electrolytic cell of platinum group metal; With
Fig. 2 is the view that the circulation of HCL, chloride monohydrate and platinum group metal is shown.
Best mode
To describe the preferred embodiments of the invention in detail now.Should be appreciated that following examples only are illustrative, the invention is not restricted to this.
From such as inorganic substances such as dead catalyst, sludge, concentrates, extracting in the situation of platinum group metal, can utilize the method for from dead catalyst, extracting the platinum group metal by electrochemical process according to of the present invention.
Can with comprise 0.01～10.0%, the dead catalyst of the pulverizing of preferred 0.1～5.0% noble metal places between the negative electrode and anode of electrolytic cell.
In one embodiment of the invention, utilizing concentration is that 0.3～10.0% hydrochloric acid solution is as electrolyte.
Electrochemistry leaches and extremely activates by multipole, and the described multipole utmost point is in electrode is converted under the multipole electrode state of the metal anode dissolving that can cause in all material.
Leach in the step in electrochemistry, electrolyte does not circulate.The initial activation of metal appears at amorphous and interconnects on the surface of spent catalyst particles of the pulverizing under the state.Metallic particles externally changes into dipole in the dead catalyst under the electric field so that the metallic particles polarization.Activation process begins with the dissolving at the metal active center on each dipole anode.Along with change in polarity, the metal of dissolving is attached to particle surface, and is attended by the distribution of atomic hydrogen.The amount of the electric charge of each particle and the activated metal of encirclement increases pro rata.The corresponding increase in field of inducting between anode in electrolytic cell and the negative electrode.Feedback appears, so that particle is carried away in the process that increases passive metal.Externally under the electric field, all particles all are converted into dipole on the wire particles with electric charge separately.Therefore, the bulk material of whole weight begins to represent the volume multipolarity electrode (volumetric multi-polar electrode) of the metal anode dissolving that can cause in all material volume.
The electrochemistry that this preliminary treatment of described material has activated following noble metal based on anodic solution leaches.If do not carry out this activating process, then electrochemistry appears at the center of each particle, and dissolving stops rapidly thus.As a result, most of noble metal is retained on the carrier with passive state, and small amount of precious metals is positioned on the negative electrode.
On anode: Cl-+2H 2O-5e -→ ClO 2-5H +
ClO 2Output depend on storage of chlorine ion (Cl -) the degree of parallel reaction process.
ClO 2+5H +→Cl-+2H 2O-5e -
In order to keep maximum ClO 2Output is necessary to prevent ClO 2Contact with negative electrode, until noble metal is extracted from dead catalyst fully.
On negative electrode: 5H ++ 5e -→ 5H
If the formation hydrogen atom, then this atom discharges from material surface, destroys and activate this surface thus.Because the polarity inversion of electrode is so all particles all are exposed to anodic solution.
Pt 0+e -→Pt +
That is to say that metallic particles flow to the catholyte pond, and in electrolyte, shift.Otherwise metallic particles directly shifts in electrolyte by advance (go-ahead) method or other ionic conduction method.
Electrolyte is circulated to negative electrode with the speed that the chloride anionic complex of the hydration that can prevent noble metal flows on the negative electrode from anode.
If circulation has the electrolyte of 0.3～10.0% HCl, then noble metal with the direction of the flowing opposite of the anionic complex of noble metal on (promptly from the anode to the negative electrode) be deposited on the negative electrode.
The pump that cycles through of this electrolyte is implemented.Circular electrolyte is in order to activate the precipitation of all metals in the electrolyte.Should notice that the chloride anionic complex of hydration that prevents the noble metal of formation in electrochemistry leaches flows on the negative electrode, this observes by form brown smoke on anode in initial procedure.
The metal (platinum or palladium-hydrochloric acid (the chloride anionic complex of the hydration of noble metal)) of dissolving flows to anode.Concentration increase along with anionic complex on the anode little by little forms brown smoke, and distributes to negative electrode subsequently.Then, anionic complex decomposes, and the anionic current of aforementioned metal precipitates at this negative electrode place to negative electrode.
Under the situation of replacing, on the negative electrode of metal, do not produce the metal of enrichment with external anolyte.When electrolyte when negative electrode flows to anode, the process that metal is assigned on the negative electrode stops.And, the dissolving metal of original allocation to the negative electrode.The chlorine that this means the high-load in the anolyte has dissolved the metal that surrounds.
In the circulation of electrolyte from the anode to the negative electrode, metal is concentrated and is assigned on the negative electrode, and the dispensing rate of metal is 2～5 times of static schema.This means that the oxidation anolyte that is used for metal along with anolyte consumption increases relatively, and the enrichment active chlorine.When the rapid circulation time of electrolyte, the formation of the brown smoke on anode stops, and the distribution of metal on negative electrode also stops.The chloride anionic complex of hydration of the noble metal that forms when preventing to leach flows to negative electrode, and the speed that should form with the brown smoke of not interrupting on the anode make electrolyte be circulated to negative electrode from anode.When the concentration of carrier is peak, can visually observe initial procedure.
Current density when preferably, electrochemistry precipitates is 0.006A/cm 2～0.025A/cm 2If current density is at most 0.006A/cm 2, then the sedimentation time prolongs, and if current density is higher than 0.025A/cm 2, then produce hydrogen.
Embodiment 1
40 liters of dead catalyst (palladium on the granite) are filled between the electrode in the electrolytic cell that is of a size of 20 * 20 * 100cm.The content of palladium is 0.3wt%, and is the particle use of 5mm with the diameter without preliminary preparation.2% HCl solution is as electrolyte, and by using pump to be circulated to negative electrode with 0.5 liter/minute speed continuously from anode.Temperature remains on 70 ℃.
Changed the polarity of electrode every 1 minute, carried out 1 hour.
When electrochemistry precipitates, apply the voltage of 21V and the electric current of 6A (current density: 0.015A/cm to electrode 2).Determine that the circulation rate of electrolyte do not interrupt precipitating the formation of the brown smoke on negative electrode when carrying out.
As a result, produce metal forming on negative electrode, this metal forming comprises the metal of 85～90% noble metals.These metal formings are easy to remove from negative electrode.
The result that analysis operation obtained after 10 hours, the palladium concentration in the electrolyte is up to 1ppm.Analyze electrochemistry and extract dead catalyst afterwards, the content of palladium is up to 0.0015%, has therefore extracted 99.5% palladium.The geometry of dead catalyst is kept perfectly, and color becomes white.Except palladium, do not extract the composition of dead catalyst.Electrolysis 1.25kWh, the heating and circular electrolyte consumed 7.5kWh.
Embodiment 2
The method of more palladiums is extracted in enforcement from the aluminium oxide-palladium catalyst that experiences leaching process.The content of palladium is 0.02～0.03%, and this is similar to United States Patent (USP) 4,775, the disclosed palladium content that is retained on the carrier in 452.The volume that is filled in the catalyst in the electrolytic cell is 40 liters, and electrolytic cell is the cylinder of diameter 10mm and high 15mm.The HCl solution of use 0.03% is as electrolyte, and the ratio of solid phase and liquid phase is set at 1:1.For the activating catalyst surface, changed the polarity of electrode, carried out 1 hour in per 1 minute.Circular electrolyte was extracted metal 15 hours with electrochemistry.Current density is 0.06A/cm 2As a result, the palladium concentration in the carrier is 0.005%, and the concentration of palladium is up to 1ppm in the electrolyte.
Embodiment 3
With crystallite dimension is that 40 liters of aluminium oxide-palladium catalysts of 3～5mm are filled in the electrolytic cell.HCl solution with 4% is used as electrolyte, and the ratio of solid phase and liquid phase is set at 1: 1.
Changed the polarity of electrode in per 1 minute, carried out 1 hour, to activate precipitation.Current density is 0.025A/cm 2(electric current of electrolytic cell is 10A), temperature remains on 70 ℃, and circular electrolyte extracted metal 20 hours with electrochemistry, and is the same with embodiment 1.As a result, extracted 98% platinum, and be 60～70% attached to the content of the platinum on the negative electrode as granular conglomerate.
Industrial applicibility
By preamble as seen, extracting method of the present invention can be extracted the platinum group metal with high efficiency and high yield.And, simplified extraction process, reduced significantly thus and extracted the required cost in platinum group metal.In addition, extracting the platinum group metal from dead catalyst is very useful based on the platinum group metal of import all for the whole amounts of recirculation.The present invention also is applicable to other catalyst that extracts load on the carrier, for example Ni, Co and Mo etc.
Though about thinking that at present the most practical and embodiment preferred described the present invention, however, it should be understood that to the invention is not restricted to described disclosed embodiment and accompanying drawing.On the contrary, the interior various change schemes and the variation scheme of spirit and scope of claims contained in the present invention.

Claims (6)

1. one kind is extracted the method for platinum group metal by electrochemical process from dead catalyst, and described method comprises:
Described dead catalyst is placed between two electrodes of electrolytic cell;
Along with the polarity that changes described electrode regularly mutually leaches described platinum group metal; With
By making electrolyte be circulated to negative electrode described platinum group metal is deposited on the negative electrode from anode.
2. method according to claim 1, wherein said electrolyte produces cl anion.
3. method according to claim 1 and 2, wherein said electrolyte are 0.3～10.0% hydrochloric acid solutions.
4. method according to claim 1, wherein the current density when electrochemistry precipitates is 0.006A/cm 2～0.025A/cm 2
5. method according to claim 1, wherein said electrochemistry leaches and extremely activates by multipole, and the described multipole utmost point is in described electrode is converted under the multipole electrode state that can cause all metal material anodic solutions.
6. method according to claim 1 wherein makes described electrolyte be circulated to described negative electrode with the speed that the chloride anionic complex of hydration that is enough to prevent described noble metal flows on the described negative electrode from described anode.
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KR20060111811A KR100858551B1 (en) 2006-11-13 2006-11-13 A method of extraction of platinum group metals from the spent catalysts by electrochemical processes
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PCT/KR2007/004828 WO2008060038A1 (en) 2006-11-13 2007-10-02 Method of extracting platinum group metals from waste catalists through electrochemical process

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CN102234812A (en) * 2010-04-29 2011-11-09 光洋应用材料科技股份有限公司 Electrochemical dissolving method of ruthenium-cobalt-based alloy
CN105229203A (en) * 2013-04-11 2016-01-06 赛丹思科大学 For reclaiming the method for platinum metals from catalytic structure
CN112088223A (en) * 2018-05-16 2020-12-15 罗伯特·博世有限公司 Method for obtaining gold and/or silver and/or at least one platinum group metal from a component of a fuel cell stack or a component of an electrolysis cell
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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JP5180409B2 (en) 2010-05-20 2013-04-10 インスー ジン Method and apparatus for extracting precious metal from waste inorganic granule catalyst
KR101323754B1 (en) * 2013-04-29 2013-10-31 한국지질자원연구원 Recovery of acid and platinum group metals from leaching solution of waste catalyst
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CN102234812A (en) * 2010-04-29 2011-11-09 光洋应用材料科技股份有限公司 Electrochemical dissolving method of ruthenium-cobalt-based alloy
CN102234812B (en) * 2010-04-29 2013-12-25 光洋应用材料科技股份有限公司 Electrochemical dissolving method of ruthenium-cobalt-based alloy
CN105229203A (en) * 2013-04-11 2016-01-06 赛丹思科大学 For reclaiming the method for platinum metals from catalytic structure
CN112088223A (en) * 2018-05-16 2020-12-15 罗伯特·博世有限公司 Method for obtaining gold and/or silver and/or at least one platinum group metal from a component of a fuel cell stack or a component of an electrolysis cell
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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