WO2012121496A2 - Procédé de récupération de métaux du groupe du platine provenant de déchets industriels contenant des métaux du groupe du platine - Google Patents

Procédé de récupération de métaux du groupe du platine provenant de déchets industriels contenant des métaux du groupe du platine Download PDF

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Publication number
WO2012121496A2
WO2012121496A2 PCT/KR2012/001219 KR2012001219W WO2012121496A2 WO 2012121496 A2 WO2012121496 A2 WO 2012121496A2 KR 2012001219 W KR2012001219 W KR 2012001219W WO 2012121496 A2 WO2012121496 A2 WO 2012121496A2
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WO
WIPO (PCT)
Prior art keywords
platinum group
group metal
platinum
metal ions
recovering
Prior art date
Application number
PCT/KR2012/001219
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English (en)
Korean (ko)
Other versions
WO2012121496A3 (fr
Inventor
신장식
한상철
곽인섭
구정분
김영애
권현지
오경준
Original Assignee
(주)알티아이엔지니어링
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by (주)알티아이엔지니어링 filed Critical (주)알티아이엔지니어링
Priority to CN201280012351.3A priority Critical patent/CN103502484A/zh
Publication of WO2012121496A2 publication Critical patent/WO2012121496A2/fr
Publication of WO2012121496A3 publication Critical patent/WO2012121496A3/fr

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Classifications

    • 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

Definitions

  • the present invention relates to a method for separating and recovering a platinum group metal from various industrial wastes containing platinum group metals.
  • Platinum group matals are platinum (Pt) and ruthenium transition metals.
  • Platinum group metals have a very high melting temperature, excellent corrosion resistance to chemical erosion, and have unique chemical properties such as reduction catalysis.
  • platinum group metals are used as catalysts for automobiles and petrochemical industries in addition to the electric electronics industry such as platinum group metal circuits. These catalysts and components are degraded over time, and eventually discarded at the end of their useful life.
  • platinum group metals are expensive and imported in their entirety, it is economically beneficial to recover and reuse them. Rather, it can play a large role in the effective use of resources.
  • a conventional method for recovering a platinum group metal is to remove the platinum group metal ion selectively extracted using a stripping agent after extracting a solvent of a mixed platinum group ion solution using a selective extracting agent after leaching.
  • a method of reducing metal ions to a platinum group metal form using a reducing agent has been used.
  • the extraction agent, stripping agent, and reducing agent used for each platinum group metal are different, and there is a problem that the recovery efficiency is very low due to a very complicated and long process.
  • the extraction agent having selectivity for the platinum group is very expensive and has good selectivity. There is also a problem that the extraction efficiency is very low.
  • the present invention is much simpler and more by-product than the conventional method for recovering the platinum group metal.
  • the purpose of the present invention is to provide a method for recovering a new platinum group metal, which does not occur and has a very high recovery efficiency.
  • a method for recovering the platinum group metal from the waste of the present invention for achieving the above object includes (a) dissolving and leaching the platinum group metal-containing waste; and (b) using a platinum group using an adsorbent in the leached waste. Adsorbing metal ions; and (c) recovering the platinum group metal ions in the form of metal by sintering the adhesive agent.
  • the platinum dissolved in the ash can be recovered in the form of ions in the solution, and ruthenium that is not dissolved in the metal form can be further separated and recovered. have. Through this step, platinum can be recovered separately from ions and ruthenium into metals.
  • the step of recovering the platinum group metal ions attached to the adsorbent with a desorption agent to a high concentration platinum group metal ion mixed solution may be performed.
  • the present invention provides a new method for recovering a platinum group metal, which is much simpler than the conventional method for recovering a platinum group metal, almost no by-products are generated, and a recovery efficiency is also very high.
  • 1 is a flow chart for separating, concentrating and recovering a platinum group metal according to the present invention.
  • FIG. 2 is a graph showing the adsorption performance of platinum group metal ions using ion exchange resin in leachate.
  • 3 to 6 are SEM photographs and EDX analysis graphs at each step according to the present invention.
  • 1 is a flow chart for separating, concentrating and recovering a platinum group metal according to the present invention.
  • the present invention relates to an industrial waste (fuel cell stack) containing platinum group metals (platinum (Pt), ruthenium (Ru), osmium (Os), rhodium (Rh), iridium (Ir), palladium (Pd)).
  • Platinum group is leached from an automobile catalyst, a chemical catalyst, an electron scrap, etc. (leaching step), and the platinum group metal ion in the leaching liquid is adsorbed to the adsorbent (adsorption step).
  • the platinum group metal ions attached to the adsorbent can be desorbed and recovered with a high concentration of platinum group metal ion mixed solution (desorption step), and the adsorbents with platinum group metal ions are incinerated ( ⁇ ⁇ , ashing) may be used to recover the platinum group metal ions in the metallic form (ashing process).
  • platinum dissolved in the ash process which is dissolved as a platinum group metal after the incineration process, is recovered as a high concentration of platinum ions, and insoluble ruthenium can be separated into a metal form (dissolution process).
  • the present invention is largely classified into three types. First, a technique for recovering high concentration platinum group metal ions using an adsorbent from a low concentration platinum group metal ion leachate. Second, the technology to recover the platinum group metal ions in the form of platinum group metal. Third, the present invention relates to a technique for separating each platinum group metal from the platinum group mixed metal recovered in the form of platinum group metal.
  • the recovery techniques of the existing platinum group metals mentioned in the prior art are different extractants, stripping agents, and reducing agents used for each platinum group metal, and are very complicated and long processes, and the recovery efficiency is very low. Extraction efficiency is very low due to very expensive and poor selectivity, while the present invention is a very simple process compared to the existing platinum group recovery process, almost no by-products are generated and the recovery efficiency is also very high.
  • wastewater containing platinum group metals is crushed and screened, followed by aqua regia.
  • Platinum group metals that are poorly soluble in acids are dissolved by hydrochloric acid in the presence of an oxidizing agent.
  • Oxidizing agents include nitric acid, hydrogen peroxide, chlorine gas, hypochlorous acid (H0C1), and sodium hypochlorite (NaOCl).
  • concentrations of the platinum group metals (platinum (Pt) and ruthenium (Ru)) in the leachate in which the fuel cell stack is leached with the leachate (7M hydrochloric acid (HC1 5M sodium hypochlorite (NaOCl)) are shown in Table 1.
  • the platinum group metal complex is preferably negatively charged. It shows ionicity.
  • platinum group metal ions in the leachate are adsorbed by using a cohesive agent, and an adsorbent is preferably used such as an ion exchange resin, activated carbon, and a biosorbent material.
  • Figure 2 shows the adsorption performance of platinum group metal ions using the ion exchange resin in the leachate as an example, the ion exchange resin used to adsorb the platinum group metal ion of the leachate is a strong base anion exchange resin Amberjet-4400 (C1). ) was used.
  • the reaction vessel of the ion exchange resin is quaternary amine, which has a positive charge in aqueous solution. It is possible to adsorb and recover the ion exchange resin by the platinum group metal ions and the electrostatic attraction in the platinum group metal leaching aqueous solution.
  • the platinum group metal ions attached to the adsorbent are desorbed with the desorbent and recovered as a highly concentrated platinum group metal ion mixed solution.
  • the desorption process can be used alone or in strong acid (hydrochloric acid, nitric acid and sulfuric acid) or in a mixed solution of thiourea and strong acid.
  • the platinum group metal is present in the metal form (metal lie form) on the surface of the ash, so that the metal form can be recovered.
  • Platinum group metals such as platinum (Pt) and ruthenium (RU) are mixed on the surface of the ashed ash, and when dissolved using a solvent that selectively dissolves platinum, platinum is not dissolved in the form of ions in the solution. Ruthenium can be recovered separately in the form of a metal.
  • the solution may include one or more of hydrochloric acid, nitric acid, sulfuric acid, and cyanide (CN) depending on the type of the platinum group metal.
  • Table 2 shows the removal efficiency of the platinum group metal in the leachate using the ion exchange resin and the recovery efficiency of the platinum group metal after incineration.
  • Araberjet-4400 (C1) was used as the strong basic anion exchange resin.
  • the adsorption amount in Table 2 indicates the amount of platinum group metal adsorbed by the adsorption material.
  • the removal efficiency is the efficiency of removing the platinum group metal from the platinum group metal leach solution.
  • the recovery efficiency is the efficiency in which the platinum group metal is adsorbed after adsorption on the adsorbent to recover the platinum group metal. Such adsorption amount, removal efficiency, and recovery efficiency can be calculated through Equation 1 below.
  • Recovery efficiency (%) Weight of metal attached to the cohesive agent () -X100 Looking at Table 2, if more ion exchange resins are used, 100% of the platinum group metal ions in the leachate can be removed, but they are adsorbed on the ion exchange resin. The platinum group metal ions present are reduced, resulting in poor recovery efficiency.
  • Tables 3 and 6 show the results of SEM and EDX analysis at each step according to the present invention.
  • EDX analysis of a fuel cell waste stack containing platinum group metals showed 95: 5 ⁇ .% Of platinum and ruthenium, indicating that the platinum and ruthenium contents decreased significantly after leaching the stack. It can be seen that the intensity of EDX is rarely analyzed, and chloride ion used as a leaching agent after stack leaching is analyzed.
  • EDX which has been analyzed after incineration of ion exchange resins containing platinum group metal ions, has a much higher platinum and ruthenium content compared to the adsorption of ion exchange resins in leachate.
  • 7 and 8 are graphs showing the results of XPS analysis according to an embodiment of the present invention.
  • platinum group metal ions in the leachate is present in the form of ions, and platinum group metals (metallic Pt and Ru 3 ⁇ 4) are reliably present on the ash surface of the ash exchanged after adsorption. This analysis indicates that platinum in the ionic form does not exist.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

La présente invention concerne un procédé suivant lequel on soumet à une lixiviation des métaux du groupe du platine provenant de déchets industriels contenant des métaux du groupe du platine (platine (Pt), ruthénium (Ru), osmium (Os), rhodium (Rh), iridium (Ir), palladium (Pd)), on fait adsorber sur un absorbant des ions des métaux du groupe du platine à l'intérieur d'un lixiviat, on fait désorber les ions des métaux du groupe du platine attachés à l'adsorbant à l'aide d'un désorbant pour récupérer une solution mixte d'ions de métaux du groupe du platine, de concentration élevée, et également, on récupère les ions des métaux du groupe du platine sous la forme métallique par incinération de l'adsorbant ayant les ions de métaux du groupe du platine attachés à celui-ci. De plus, le platine dissous par un procédé de dissolution à partir des cendres mélangées avec les métaux du groupe du platine après le procédé d'incinération peut être récupéré comme ion platine de concentration élevée, et du ruthénium non dissous peut être isolé sous une forme métallique.
PCT/KR2012/001219 2011-03-09 2012-02-17 Procédé de récupération de métaux du groupe du platine provenant de déchets industriels contenant des métaux du groupe du platine WO2012121496A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201280012351.3A CN103502484A (zh) 2011-03-09 2012-02-17 用于从含有铂族金属的工业废弃物回收铂族金属的方法

Applications Claiming Priority (2)

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KR20110021116A KR101224503B1 (ko) 2011-03-09 2011-03-09 백금족 금속 함유 산업폐기물로부터 백금족 금속을 회수하는 방법
KR10-2011-0021116 2011-03-09

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WO2012121496A2 true WO2012121496A2 (fr) 2012-09-13
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KR101392179B1 (ko) 2013-02-08 2014-05-08 강희남 백금족 금속의 회수방법 및 이에 사용되는 백금족 금속의 회수장치
KR101454645B1 (ko) 2013-02-20 2014-10-27 한국생산기술연구원 배기 가스 정화 장치의 폐촉매에 포함된 금속 정량 방법
KR101452809B1 (ko) * 2013-04-22 2014-10-22 (주)알티아이엔지니어링 폐촉매에서 회수한 백금을 이용한 연료전지용 백금 담지 촉매 제조방법
KR101579498B1 (ko) * 2015-02-24 2015-12-22 (주) 유천테크 팔라듐함유 폐 페이스트로부터 팔라듐의 회수방법
CN108579695A (zh) * 2018-01-22 2018-09-28 江苏欣诺科催化剂有限公司 一种吸附铱的吸附剂及脱附方法
CN112029998B (zh) * 2020-08-27 2022-03-18 湖南高鑫铂业有限公司 一种从颗粒状废催化剂中溶-吸-脱联合回收铂族金属的方法
CN113957244A (zh) * 2021-10-26 2022-01-21 中钢集团南京新材料研究院有限公司 一种含铂料液中铂族金属的富集方法

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KR20030041841A (ko) * 2001-11-21 2003-05-27 쉬플리 캄파니, 엘.엘.씨. 촉매 금속의 회수방법
JP2005002414A (ja) * 2003-06-12 2005-01-06 Maezawa Ind Inc 溶液中の貴金属の回収方法
KR20100113678A (ko) * 2009-04-14 2010-10-22 전북대학교산학협력단 유가금속의 회수방법

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WO2012121496A3 (fr) 2012-11-15
KR20120103082A (ko) 2012-09-19
KR101224503B1 (ko) 2013-02-04
CN103502484A (zh) 2014-01-08

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