CN103502484A - Method for recovering platinum group metals from industrial waste containing platinum group metals - Google Patents

Method for recovering platinum group metals from industrial waste containing platinum group metals Download PDF

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CN103502484A
CN103502484A CN201280012351.3A CN201280012351A CN103502484A CN 103502484 A CN103502484 A CN 103502484A CN 201280012351 A CN201280012351 A CN 201280012351A CN 103502484 A CN103502484 A CN 103502484A
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platinum metals
platinum
ion
platinum group
metals
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申壮植
韩相彻
郭仁燮
具贞粉
金荣爱
权眩池
吴垧俊
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RTI ENGINEERING Co Ltd
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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
    • 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
    • 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
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • 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
    • 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
    • B01J38/02—Heat treatment
    • 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
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/04—Processes using organic exchangers
    • B01J41/05—Processes using organic exchangers in the strongly basic form
    • 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
    • C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • 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
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • 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
    • 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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  • Processing Of Solid Wastes (AREA)
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Abstract

The present invention leaches platinum groups from industrial waste containing platinum group metals (platinum (Pt), ruthenium (Ru), osmium (Os), rhodium (Rh), iridium (Ir), palladium (Pd)), adsorbs onto an absorbent platinum group metal ions inside a leachate, desorbs the platinum group metal ions attached to the adsorbent using a desorbent to recover high concentration platinum group metal ion mixed solution, and also, recover the platinum group metal ions in the metallic form by ashing the adsorbent having the platinum group metal ions attached thereto. In addition, the platinum dissolved through a dissolving process from the ash mixed with the platinum group metals after the ashing process can be recovered as high concentration platinum ion, and undissolved ruthenium can be isolated in a metallic form.

Description

Reclaim the method for platinum metals for the trade waste from containing platinum metals
Technical field
The present invention relates to separate and reclaim the method for platinum metals for the various trade wastes from containing platinum metals.
Background technology
Platinum metals refers to platinum (Pt), ruthenium (Ru), osmium (Os), rhodium (Rh), the iridium (Ir) in the middle of transition metal, and palladium (Pd).Platinum metals has unique chemical property, for example high solvent temperature, fabulous chemical resistance of concrete, reduction catalysts, etc.
Every annual production platinum metals is approximately 200 tons in the world, and 90% or more platinum metals Shi Antarctica and USSR (Union of Soviet Socialist Republics) production, approximately 6% platinum metals is to produce in Canada, and remaining a small amount of platinum metals be in South America, state's productions such as the U.S., Australia, Japan.These platinum metals are for electricity and electronics industry, such as the platinum metals circuit etc., and also with the catalyzer that acts on automobile and petrochemical industry.These catalyzer and composition suffer performance degradation in time, once and final performance become unacceptable and be dropped.Yet exactly, because the high and complete import of platinum metals price, so the recovery of platinum metals and effective use of being used in again economic feasibility and resource are obviously favourable.
For reclaiming the typical method of platinum metals, use selective extractant to carry out the solvent extraction of platinum metals ion from the platinum family solion, and use steam stripping agent (stripping agent) to collect the platinum metals ion of selective extraction, then use reductive agent that it is reduced into to platinum metals.Yet, this technique has problem: each extraction agent, steam stripping agent and the reductive agent for platinum metals is different compounds, organic efficiency is extremely low owing to extremely complicated and long process, and extraction efficiency is because extraction agent is extremely expensive and have bad selectivity and extremely low.
Summary of the invention
[technical problem]
Aspect of the present invention is to provide a kind of for reclaiming the novel method of platinum metals, and it is compared extremely simply with the typical method in technique, prevents in fact byproduct, and represents high organic efficiency.
[technical solution]
According to an aspect of the present invention, a kind ofly for the method that reclaims platinum metals from waste, comprise: the waste that (a) by dissolving, contains platinum metals leaches the waste that contains platinum metals; (b) use sorbent material from described leaching waste absorption platinum metals ion; And (c) by the described sorbent material of ashing, with metallic forms, reclaim described platinum metals ion.
Therefore, can reclaim platinum metals with metallic forms by extremely simple technique.
In operation (c) afterwards, described method can further comprise to separate respectively and be recovered in to dissolve after ash content immediately with ionic species and is dissolved in platinum in solution and the undissolved ruthenium that becomes metallic forms after dissolving ash content.By this operation, can separate respectively and reclaim platinum and ruthenium with metallic forms with ionic species.
In operation (b) afterwards, the platinum metals ion that described method can further comprise by be attached to sorbent material by the strippant desorption reclaims the platinum metals ion as high density platinum metals Ar ion mixing solution.
[favourable effect]
It is a kind of for reclaiming the novel method of platinum metals that embodiments of the invention provide, and it is compared extremely simply with the typical method in technique, prevents in fact byproduct, and represents high organic efficiency.
The accompanying drawing explanation
Above and other aspects, features and advantages of the present invention will be from by reference to the accompanying drawings to the detailed description of following examples and become apparent, in the accompanying drawings:
Fig. 1 be illustrated according to an embodiment of the invention for the method that reclaims platinum metals the schema for separating of the process of, enrichment and recovery platinum metals;
Fig. 2 is the curve of absorption property of describing to use the platinum metals ion of the ion exchange resin in leach liquor;
Fig. 3 to 6 is SEM image and the EDX analytic curves in each operation in method according to an embodiment of the invention; And
Fig. 7 and 8 is according to an embodiment of the invention for the XPS analysis curve in each operation of the method that reclaims platinum metals.
Embodiment
Hereinafter with reference to accompanying drawing, describe example embodiment of the present invention in detail.
Fig. 1 be illustrated according to an embodiment of the invention for the method that reclaims platinum metals the schema for separating of the process of, enrichment and recovery platinum metals.
According to an embodiment of the invention for reclaiming the method for platinum metals, from waste (fuel cell stack, automobile catalyst, chemical catalyst, the electronic waste that contains platinum metals (platinum (Pt), ruthenium (Ru), osmium (Os), rhodium (Rh), iridium (Ir), palladium (Pd)), and analogue) leach platinum metals (leaching process), and by the platinum metals ionic adsorption in leach liquor (adsorption process) to sorbent material.
After adsorption process, can be attached to the platinum metals ion of sorbent material and the platinum metals ion is recovered as to high density platinum metals Ar ion mixing solution (desorption process) by using the strippant desorption, or by ashing platinum metals ion accompanying to sorbent material and reclaim described platinum metals ion (podzolic process) with metallic forms.In addition, after podzolic process, the platinum that the dissolution process of the ash content by being mixed with platinum metals can be dissolved is recovered as the high density platinum ion, and can metallic forms reclaim undissolved ruthenium (dissolution process).
The present invention relates generally to following three technology: the first, and use sorbent material to reclaim the technology of high density platinum family ion from lower concentration platinum family ion leach liquor; The second, reclaim the platinum family ion with metallic forms; And the 3rd, separate each platinum metals from the platinum family hybrid metal reclaimed with metallic forms.
According to above in the background technology part, describe for reclaiming the typical technology of platinum metals, each extraction agent, steam stripping agent and reductive agent for platinum metals is different compounds, and organic efficiency is extremely low owing to extremely complicated and long process, and extraction efficiency is because extraction agent is extremely expensive and have bad selectivity and extremely low.On the contrary, with the canonical process for reclaiming platinum metals, compare, the method according to this invention is extremely simple technique, does not produce byproduct in fact, and has high organic efficiency.
Next, will describe according to an embodiment of the invention for reclaiming the method for platinum metals in more detail.
In leaching process, after the waste that crushing and classification contain platinum metals, by being dissolved in chloroazotic acid, spirit of salt, halogen compounds, form soluble salt and the fellow leaches Powdered waste.The example of oxygenant comprises nitric acid, hydrogen peroxide, chlorine, hypochlorous acid (HOCl), clorox (NaOCl), and the fellow.In an example, during platinum metals (platinum (Pt), ruthenium (Ru)) concentration in the leach liquor by using leach liquor (7M spirit of salt (HCl)+5M clorox (NaOCl)) leaching fuel cell stack to produce is showed in table 1.Platinum metals misfit thing has electric charge, is preferably anionic charge.
Table 1
Stacking leach liquor Pt Ru
Concentration (mg/L) 181.25 37.14
In adsorption process, use the platinum metals ion in sorbent material absorption leach liquor, and ion exchange resin, activated carbon, biological adsorption material etc. can be used as sorbent material.
Fig. 2 is the curve of absorption property of describing to use in an example the platinum metals ion of the ion exchange resin in leach liquor, and wherein strongly basic anion exchange resin Amberjet-4400 (Cl) is as ion exchange resin.The reactive group of ion exchange resin is quaternary amine, and it has positive charge in the aqueous solution.The platinum metals ion that represents negative charge in the aqueous solution is leached in platinum metals by and ion exchange resin between electrostatic attraction be adsorbed on ion exchange resin, and can be reclaimed.
In desorption process, the platinum metals ion that is attached to sorbent material by desorption reclaims the platinum metals Ar ion mixing solution of platinum metals ion as the height enrichment.Strong acid (spirit of salt, nitric acid or sulfuric acid) or carry out desorption process with the mixing solutions of thiocarbamide and strong acid can be used alone.
When by the accompanying sorbent material burn to ash arrived of platinum family ion, platinum metals is present on the surface of ash content with metallic forms, and therefore can metallic forms be reclaimed.
Mix on the surface of ash content platinum metals such as platinum (Pt), ruthenium (Ru) and fellow thereof.Therefore, in the time of in ash content being dissolved in to the solvent that can optionally dissolve platinum, can reclaim individually platinum and ruthenium with the ionic species in solution and metallic forms respectively.Solution can be depending on the type of platinum metals and comprises at least one in spirit of salt, nitric acid, sulfuric acid and cyanogen (CN).
Table 2 is showed makes spent ion exchange resin remove the efficiency of the platinum metals in leach liquor and its organic efficiency after ashing.Strongly basic anion exchange resin Amberjet-4400 (Cl) is as described ion exchange resin.
Table 2
Figure BDA0000379193670000041
In table 2, adsorptive capacity refers to the amount of the platinum metals of adsorbing by sorbing material.In addition, remove efficiency and refer to the efficiency while from the platinum metals leach liquor, removing platinum metals.In addition, organic efficiency refers to the efficiency when carrying out ashing reclaim platinum metals after being adsorbed onto on sorbent material by platinum metals.Can calculate adsorptive capacity, remove efficiency and organic efficiency by equation 1.
[equation 1]
Figure BDA0000379193670000042
As shown in table 2, although use the more ion exchange resin of volume can allow to remove 100% platinum metals ion, organic efficiency may reduce, because be adsorbed onto the amount of the platinum metals ion on ion exchange resin, will reduce.
Fig. 3 to 6 is SEM image and the EDX analytic curves in each operation in method according to an embodiment of the invention.
Table 3
Figure BDA0000379193670000052
From the discarded stacking EDX analytical results of the fuel cell that contains platinum metals (platinum, ruthenium), can find out, it is 95 % by weight that there are ratio in platinum and ruthenium: 5 % by weight, and the amount of platinum and ruthenium reduces (seldom analyzing when observing EDX intensity) after stacking leaching, and can find out, the chlorion as leaching agent detected after stacking leaching.
EDX analytical results after on ion exchange resin from the platinum metals ionic adsorption to stacking leach liquor, can find out, with fuel cell stack, without undergoing leaching, compares, and platinum and ruthenium present high concentration.
Be adsorbed onto leach liquor in ion exchange resin on after result compare, the EDX analytical results after the ion exchange resin of ashing absorption platinum metals ion shows high platinum and ruthenium amount.
Fig. 7 and 8 is curves of describing XPS analysis result according to an embodiment of the invention.
Can find out, in leach liquor, the lip-deep platinum of the ion exchange resin of absorption platinum family ion exists with ionic species, and platinum metals clearly detected on the surface of ion exchange resin ash content (Pt metal and RuO x), and the platinum of ionic species does not exist thereon after absorption and ashing.
In addition, can see, in the situation that the ash content obtained by the platinum after the dissolving ashing, the platinum of metallic forms dissolves fully and disappears, and ruthenium changes into RuO xbut not dissolve.Therefore, can find out, from platinum metals mixing ash content, reclaim out individually platinum and ruthenium.That is, can reclaim individually platinum and ruthenium with ionic species and metallic forms respectively.
Hereinbefore, with reference to accompanying drawing, disclose example embodiment.Although this paper has been used particular term, described term is only for the illustrative purpose, and should not be interpreted as by any way limiting the present invention.Therefore, should be understood that the those skilled in the art can carry out various modifications, variation, change and equivalent embodiment, and do not break away from the spirit and scope of the present invention.Therefore scope of the present invention should only be limited by appended claims and equivalent thereof.

Claims (3)

1. a method that reclaims described platinum metals for the trade waste from containing platinum metals, it comprises:
(a) waste that contains platinum metals by dissolving leaches the described waste that contains platinum metals;
(b) use sorbent material from described leaching waste absorption platinum metals ion; And
(c) adsorb the described sorbent material of described platinum metals ion and reclaim described platinum metals ion with metallic forms by ashing.
2. method according to claim 1, it further comprises: after (c) reclaims described platinum metals ion, separate respectively and be recovered in to dissolve after ash content immediately with ionic species being dissolved in platinum in solution and the undissolved ruthenium that becomes metallic forms after dissolving ash content.
3. method according to claim 1, it further comprises: after the ion of (b) absorption platinum metals, by the described platinum metals ion that is attached to described sorbent material by the strippant desorption, reclaim described platinum metals ion as high density platinum metals Ar ion mixing solution.
CN201280012351.3A 2011-03-09 2012-02-17 Method for recovering platinum group metals from industrial waste containing platinum group metals Pending CN103502484A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108579695A (en) * 2018-01-22 2018-09-28 江苏欣诺科催化剂有限公司 A kind of adsorbent and desorption method of absorption iridium
CN113957244A (en) * 2021-10-26 2022-01-21 中钢集团南京新材料研究院有限公司 Method for enriching platinum group metal in platinum-containing feed liquid

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KR101392179B1 (en) 2013-02-08 2014-05-08 강희남 Recovery method of platinum group metal and apparatus for recovering platinum group metal
KR101454645B1 (en) 2013-02-20 2014-10-27 한국생산기술연구원 Method for quantitative analysis of metals from spent catalyst of exhaust gas consecration system
KR101452809B1 (en) * 2013-04-22 2014-10-22 (주)알티아이엔지니어링 Method of preparing platinum catalyst supported on carbon black for fuel cell using a recycled platinum from spent catalyst
KR101579498B1 (en) * 2015-02-24 2015-12-22 (주) 유천테크 Method for recovering palladium of waste pastes containing palladium
CN112029998B (en) * 2020-08-27 2022-03-18 湖南高鑫铂业有限公司 Method for recovering platinum group metal from granular waste catalyst by combination of dissolution, absorption and desorption

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CN1445380A (en) * 2001-11-21 2003-10-01 希普雷公司 Method for recovering catalytic metal
CN1452605A (en) * 2000-09-05 2003-10-29 约翰森·马瑟公开有限公司 Method for recovery of metals by incineration of metal contg. basic ion exchange resin
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CN1123843A (en) * 1994-11-30 1996-06-05 核工业北京化工冶金研究院 Recovery of platinum family elements from waste catalysts
CN1452605A (en) * 2000-09-05 2003-10-29 约翰森·马瑟公开有限公司 Method for recovery of metals by incineration of metal contg. basic ion exchange resin
CN1445380A (en) * 2001-11-21 2003-10-01 希普雷公司 Method for recovering catalytic metal
JP2005002414A (en) * 2003-06-12 2005-01-06 Maezawa Ind Inc Method of recovering noble metal in solution
KR20100113678A (en) * 2009-04-14 2010-10-22 전북대학교산학협력단 Recovery method of valuableness metals

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108579695A (en) * 2018-01-22 2018-09-28 江苏欣诺科催化剂有限公司 A kind of adsorbent and desorption method of absorption iridium
CN113957244A (en) * 2021-10-26 2022-01-21 中钢集团南京新材料研究院有限公司 Method for enriching platinum group metal in platinum-containing feed liquid

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Application publication date: 20140108