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WO2012029379A1 - Procédé de récupération de platine de haute pureté - Google Patents

Procédé de récupération de platine de haute pureté Download PDF

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Publication number
WO2012029379A1
WO2012029379A1 PCT/JP2011/064096 JP2011064096W WO2012029379A1 WO 2012029379 A1 WO2012029379 A1 WO 2012029379A1 JP 2011064096 W JP2011064096 W JP 2011064096W WO 2012029379 A1 WO2012029379 A1 WO 2012029379A1
Authority
WO
WIPO (PCT)
Prior art keywords
platinum
ruthenium
aqua regia
dissolved
purity
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2011/064096
Other languages
English (en)
Japanese (ja)
Inventor
関口　淳之輔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JX Nippon Mining and Metals Corp
Original Assignee
JX Nippon Mining and Metals Corp
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.)
Filing date
Publication date
Application filed by JX Nippon Mining and Metals Corp filed Critical JX Nippon Mining and Metals Corp
Priority to JP2011539574A priority Critical patent/JP5399510B2/ja
Priority to US13/813,354 priority patent/US20130139648A1/en
Priority to CN201180030294.7A priority patent/CN102959103B/zh
Priority to SG2012093555A priority patent/SG186401A1/en
Publication of WO2012029379A1 publication Critical patent/WO2012029379A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • 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
    • C22B11/02—Obtaining noble metals by dry processes
    • C22B11/021—Recovery of noble metals from waste materials
    • C22B11/025—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper, or baths
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • 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 high-purity platinum recovery method for recovering high-purity platinum in a high yield from scraps such as platinum alloys containing platinum and ruthenium as a component, particularly magnetic material targets.
  • the impurities as described above cause a decrease in the performance of the recording medium, the hard disk, and the semiconductor device element, and may cause splash, abnormal discharge, particles, and the like during the sputtering, thereby reducing the properties of the thin film.
  • acid such as aqua regia and removing the residue
  • the acid dissolved with platinum and ammonium chloride solution are reacted to precipitate and recover as ammonium chloroplatinate. Platinum is recovered by baking.
  • Magnetic thin films containing platinum as a main component of constituent elements or a part of constituent elements are often containing ruthenium as a part of the constituent elements. Since ruthenium is a platinum group element, its properties are similar and it is difficult to separate platinum and ruthenium. Ruthenium is an impurity unless platinum and ruthenium are separated, except in special cases where even if ruthenium is mixed in platinum, there is no particular problem with the properties of the material. Since platinum itself is a very expensive material, it must be recovered with good yield. Several techniques for recovering platinum have been proposed in the patent literature. The following are introduced below. What is an efficient recovery method for separating ruthenium from platinum and recovering high-purity platinum? I can not say.
  • Patent Document 1 when platinum is extracted as an ammonium chloride salt by extracting platinum, the pH of the gold-containing platinum group metal-containing chloride-containing aqueous solution is adjusted to perform two-stage neutralization and filtration. Techniques for separating are disclosed. Patent Document 2 below discloses a technique for removing impurities ruthenium by heating to high temperature in an oxygen gas stream against ammonium chloroplatinate or platinum.
  • Patent Document 3 when ruthenium is separated from a platinum group-containing solution by oxidative distillation, the pH of the solution is adjusted, and then sodium bromate is used to convert ruthenium to ruthenium tetroxide for oxidative distillation.
  • Patent Document 4 listed below discloses a method for producing platinum powder in which, when ammonium chloroplatinate is formed, fine ammonium chloroplatinate is obtained using a dispersion stabilizer in an ammonium chloride solution, and this is baked at a low temperature. Has been.
  • Patent Document 5 discloses a method for recovering high-purity platinum in which platinum-containing scraps are dissolved with an acid, reacted with an ammonium chloride solution, precipitated and recovered as ammonium chloroplatinate, and roasted to obtain a platinum sponge. It is disclosed.
  • Patent Document 6 after a platinum-containing scrap is dissolved with an acid, it is reacted with an ammonium chloride solution, and precipitated and recovered as ammonium chloroplatinate, and the remaining platinum is recovered using an ion exchange resin and activated carbon. The technology is described.
  • the present invention is a platinum alloy for sputtering, in particular, target scrap containing platinum used for forming a magnetic thin film (used target) or scraps generated in the manufacturing process of the target, cutting scrap, flat grinding scrap. It is possible to efficiently remove cobalt, chromium, copper, iron, nickel, silicon and the like mixed in scrap such as ruthenium contained in platinum alloy scrap for sputtering, and thereby platinum and
  • the present invention provides a method for recovering high-purity platinum that can be reused for a platinum-containing target at a low cost and in a high yield.
  • the present invention 1) Dissolve a platinum alloy containing ruthenium in aqua regia and remove the residue, then react the platinum-dissolved acid with an ammonium chloride solution to precipitate an ammonium chloroplatinate salt.
  • This ammonium chloroplatinate salt Of high purity platinum to obtain platinum sponge by reducing platinum, wherein the acid in which platinum is dissolved and ammonium chloride solution are reacted at a temperature of 40 ° C or higher 2
  • the platinum alloy containing ruthenium is A method for recovering high-purity platinum according to 1) or 2), wherein the ruthenium concentration of a solution dissolved in water is 6 g / L or less.
  • the present invention also provides: 4) The ruthenium content as an impurity in the platinum sponge obtained by roasting ammonium chloroplatinate is 2% or less, 1) to 3) 5) The high purity platinum recovery method according to 4), wherein the ruthenium content is 1% or less. 6) The ruthenium-containing platinum alloy is a scrap of a magnetic material target. A method for recovering high-purity platinum according to any one of 1) to 5), wherein the platinum recovery rate from the scrap is 99% or more.
  • Cobalt, chromium, copper, iron, nickel, silicon, etc. mixed into scraps such as scrap containing platinum-containing target scrap (used target) for sputtering or scraps generated in the target manufacturing process, cutting scraps, flat scraps, etc. are relatively easy.
  • it has an excellent effect of efficiently separating ruthenium, which is a platinum group element contained in the magnetic material target, from platinum.
  • a scrap containing platinum and ruthenium and further containing cobalt, chromium, copper, iron, nickel, silicon and the like as impurity elements is first dissolved with an acid.
  • Aqua regia is used as the acid for dissolution.
  • aqua regia is used, dissolution is sufficiently achieved, and since nitrogen oxides and hydrogen are generated at the same time, there is an advantage that hydrogen is diluted and there is no danger of explosion.
  • platinum does not readily dissolve in the initial stage, but platinum gradually dissolves well.
  • an acid in which platinum is dissolved is reacted with an ammonium chloride solution to precipitate ammonium chloroplatinate ((NH 4 ) 2 PtCl 6 ) crystals.
  • an ammonium chloride solution to precipitate ammonium chloroplatinate ((NH 4 ) 2 PtCl 6 ) crystals.
  • aqua regia in which platinum is dissolved to the ammonium chloride solution.
  • it is common knowledge to try to add an ammonium chloride solution to aqua regia in which platinum is dissolved.
  • ammonium chloroplatinate is redissolved and hardly precipitated, and platinum remains in the solution.
  • a phenomenon in which the yield of platinum falls is observed.
  • the problem is that ruthenium separation has not been studied in the scrap. This is because the formation of a magnetic film or the addition of ruthenium as a constituent element of the target has not been widely performed, so that the separation of ruthenium has not been a major problem. However, it is urgent at present. On the other hand, since ruthenium is a platinum group element as described above, separation from platinum is not easy. The present invention provides a technique for easily and efficiently separating this.
  • the high purity platinum recovery method of the present invention involves dissolving a ruthenium-containing platinum alloy with aqua regia, removing the residue, and then reacting an acid in which platinum is dissolved with an ammonium chloride solution to obtain an ammonium chloroplatinate salt.
  • the acid in which the platinum is dissolved and the ammonium chloride solution are reacted at a temperature of 40 ° C. or higher.
  • the upper limit of the temperature is not particularly limited, but it can be said that the upper limit of the temperature is preferably 100 ° C. or less at which the liquid does not evaporate.
  • the process until obtaining the sponge can be said to be a conventional technique.
  • it was difficult to separate ruthenium and the intended separation was not realized.
  • the platinum recovery rate was improved, and the ruthenium content in the platinum salt could be reduced. This was a very unexpected result.
  • the technique of reducing the chloroplatinic acid ammonium salt to obtain a platinum sponge is a relatively simple and efficient manufacturing process, and this technique on the extension line enables the separation of ruthenium. Although this looks simple at first glance, as described above, it was difficult to predict and a dramatic effect was obtained.
  • the platinum concentration of a solution obtained by dissolving a platinum alloy containing ruthenium with aqua regia is preferably 15 g / L or more. This is because, when the platinum concentration is reduced to less than 15 g / L, the solubility of the platinum salt increases, so that the platinum recovery rate from scrap decreases (less than 99%).
  • the platinum content in scrap is usually 30% by weight or more.
  • the platinum concentration in the solution is much higher than 15 g / L, diluted with a large amount of water. As long as it is not, the concentration never falls below 15 g / L.
  • the concentration of ruthenium is high and the platinum content is relatively low, if the concentration is lower than 15 g / L as it is, the aqua regia can be dissolved by mixing with scrap having a high platinum content.
  • the ruthenium concentration of a solution obtained by dissolving a platinum alloy containing ruthenium with aqua regia is 6 g / L or less.
  • the reaction temperature is also affected, but if the ruthenium concentration exceeds 6 g / L, ruthenium tends to enter precipitates. To reduce this ruthenium concentration, it is only necessary to dilute with water. However, since the platinum concentration of the liquid is decreased, mutual adjustment is necessary.
  • the ruthenium content as an impurity in the platinum sponge obtained by baking the chloroplatinic acid ammonium salt is 2% or less, further 1% or less. Can do. Furthermore, it is possible to achieve a platinum recovery rate of 99% or more from scrap of a magnetic material target containing a platinum alloy containing ruthenium.
  • the present invention provides a method for recovering such high-purity platinum.
  • Example 1 In Example 1, a scrap of a magnetic material target containing platinum, cobalt, chromium and ruthenium was dissolved in aqua regia to remove the residue, and then diluted with water to have a platinum concentration of 30 g / L and a ruthenium concentration of 5 g / L. The aqua regia solution. This aqua regia solution and ammonium chloride were reacted at 45 ° C. to obtain ammonium chloroplatinate ((NH 4 ) 2 PtCl 6 ) crystals. Next, it was baked at 800 ° C. to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as impurities were measured. The results are shown in Table 1.
  • the platinum recovery rate reached 99.5%, and the ruthenium content in the platinum salt decreased to 0.5% by weight. This ruthenium content was sufficiently reduced in the case of using recycled platinum as a target. Further, if the reaction temperature between the aqua regia solution and ammonium chloride is 40 ° C. or higher, the same platinum purity and ruthenium reduction can be achieved.
  • the roasting temperature is not particularly limited and can be adjusted as appropriate, and the temperature at which a platinum sponge is usually obtained can be arbitrarily selected. The same applies hereinafter.
  • Example 2 the scrap of the magnetic material target containing platinum, cobalt, chromium, and ruthenium was dissolved in aqua regia to remove the residue, and then diluted with water to obtain a platinum concentration of 18 g / L and a ruthenium concentration of 3 g / L.
  • the aqua regia solution This aqua regia solution and ammonium chloride are reacted at 90 ° C. to precipitate ammonium chloroplatinate salt, which is roasted at 800 ° C. to form a platinum sponge.
  • Platinum recovery rate and impurities from the aqua regia solution The ruthenium content as was measured. The results are shown in Table 1.
  • the platinum recovery rate reached 99.3%, and the ruthenium content in the platinum salt decreased to 0.3% by weight. This ruthenium content was sufficiently reduced in the case of using recycled platinum as a target. Further, if the reaction temperature between the aqua regia solution and ammonium chloride is 40 ° C. or higher, the same platinum purity and ruthenium reduction can be achieved.
  • Example 3 In Example 3, the scrap of the magnetic material target containing platinum, cobalt, chromium and ruthenium was dissolved in aqua regia to remove the residue, and then diluted with water to have a platinum concentration of 16 g / L and a ruthenium concentration of 5 g / L.
  • the aqua regia solution This aqua regia solution and ammonium chloride are reacted at 50 ° C. to precipitate an ammonium chloroplatinate salt, which is baked at 800 ° C. to form a platinum sponge.
  • the ruthenium content was measured. The results are shown in Table 1.
  • the platinum recovery rate reached 99.2%, and the ruthenium content in the platinum salt decreased to 1.7% by weight. This ruthenium content was sufficiently reduced in the case of using recycled platinum as a target. Further, if the reaction temperature between the aqua regia solution and ammonium chloride is 40 ° C. or higher, the same platinum purity and ruthenium reduction can be achieved.
  • Cobalt, chromium, copper, iron, nickel, silicon, etc. mixed in scrap such as scraps, cutting scraps, flat polishing scraps, etc., generated in the manufacturing process of platinum for sputtering and platinum-containing targets are removed in a relatively simple process, It has an excellent effect that high-purity platinum that can be reused for platinum and a target containing these can be recovered in a high yield.
  • ruthenium which is said to be particularly difficult to separate from platinum, has the effect that it can be reduced in a relatively simple method, so it is useful to recover high-purity platinum at a low cost and in a high yield. Can provide a simple method.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne un procédé de récupération de platine de haute pureté qui permet d'obtenir une éponge de platine en dissolvant un alliage de platine contenant du ruthénium dans de l'eau régale, en retirant le résidu puis en faisant réagir l'acide dans lequel le platine est dissous et une solution de chlorure d'ammonium, en séparant le chloroplatinate d'ammonium, et en réduisant le chloroplatinate d'ammonium. Le procédé est caractérisé en ce que l'on fait réagir l'acide dans lequel le platine est dissous et la solution de chlorure d'ammonium à une température d'au moins 40 °C. Ledit procédé permet de récupérer avec un rendement élevé du platine de haute pureté qui peut être réutilisé dans des cibles contenant du platine ou un alliage de platine, et duquel le ruthénium, le cobalt, le chrome, le cuivre, le fer, le nickel et le silicium, entre autres, mélangés dans des rebuts tels que les copeaux de fraisage, la poussière de sciage ou les rebuts de surfaçage générés entre autres dans le procédé de fabrication d'une cible ou présents dans une cible de pulvérisation cathodique en alliage de platine usagée ont été efficacement retirés.
PCT/JP2011/064096 2010-09-03 2011-06-21 Procédé de récupération de platine de haute pureté Ceased WO2012029379A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2011539574A JP5399510B2 (ja) 2010-09-03 2011-06-21 高純度白金の回収方法
US13/813,354 US20130139648A1 (en) 2010-09-03 2011-06-21 Recovery Method for High Purity Platinum
CN201180030294.7A CN102959103B (zh) 2010-09-03 2011-06-21 高纯度铂的回收方法
SG2012093555A SG186401A1 (en) 2010-09-03 2011-06-21 Recovery method for high purity platinum

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010-198024 2010-09-03
JP2010198024 2010-09-03

Publications (1)

Publication Number Publication Date
WO2012029379A1 true WO2012029379A1 (fr) 2012-03-08

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US (1) US20130139648A1 (fr)
JP (1) JP5399510B2 (fr)
CN (1) CN102959103B (fr)
MY (1) MY160898A (fr)
SG (1) SG186401A1 (fr)
WO (1) WO2012029379A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103627902A (zh) * 2013-04-25 2014-03-12 上海派特贵金属有限公司 一种从失效贵金属催化剂中回收铑的方法
AU2014201077B2 (en) * 2013-03-05 2015-08-13 Heraeus Precious Metals Gmbh & Co. Kg Method for producing highly pure platinum powder, as well as platinum powder that can be obtained according to said method, and use thereof
CN111926195A (zh) * 2020-06-24 2020-11-13 重庆材料研究院有限公司 一种从铂合金废料中制备高纯铂的方法
CN112126789A (zh) * 2020-09-17 2020-12-25 朱俊 一种氯铂酸溶液浓缩工艺及设备

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3026110B1 (fr) * 2014-09-24 2016-11-18 Commissariat Energie Atomique Procede de recuperation du platine present dans un assemblage membrane-electrode.
TWI623623B (zh) * 2017-04-17 2018-05-11 國立中山大學 回收貴金屬的處理方法
DE102019217188A1 (de) * 2019-11-07 2021-05-12 Robert Bosch Gmbh Verfahren zur Gewinnung von Platin und/oder Ruthenium
CN110964912A (zh) * 2019-12-20 2020-04-07 有研亿金新材料有限公司 一种从铂钨合金回收提纯铂的方法
CN111676371A (zh) * 2020-04-27 2020-09-18 励福(江门)环保科技股份有限公司 一种从钨坩埚中分离提纯铂的方法
CN111690819A (zh) * 2020-06-24 2020-09-22 广东金正龙科技有限公司 一种铂金提纯方法及一种反应釜
CN115125398A (zh) * 2022-08-09 2022-09-30 顾秀华 一种金属铂的半金属化合物制备工艺
CN116967460A (zh) * 2023-05-08 2023-10-31 英特派铂业股份有限公司 一种从铂铑合金中制备高纯铂粉的方法

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JPS5322114A (en) * 1976-06-21 1978-03-01 Nat I Fuoa Metaraajii Separating and refining method of ruthenium
JPH09316560A (ja) * 1996-05-27 1997-12-09 Nikko Kinzoku Kk 白金の回収方法
JP2006183099A (ja) * 2004-12-28 2006-07-13 Nippon Mining & Metals Co Ltd 白金中の不純物除去方法
JP2009144183A (ja) * 2007-12-12 2009-07-02 Mitsubishi Materials Corp 白金の回収方法
JP2010222613A (ja) * 2009-03-20 2010-10-07 Mitsubishi Materials Corp 白金の回収処理方法

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JP4865156B2 (ja) * 2001-07-18 2012-02-01 Ｊｘ日鉱日石金属株式会社 高純度白金及びパラジウムの回収方法
JP2003129145A (ja) * 2001-10-22 2003-05-08 Nikko Materials Co Ltd 白金の回収方法
JP2004141824A (ja) * 2002-10-28 2004-05-20 Nikko Materials Co Ltd 白金等の有価金属回収方法
CN101358287A (zh) * 2008-09-10 2009-02-04 灵宝市金源矿业有限责任公司 一种难熔合质金中金、银及铂族金属的分离方法
JP5339068B2 (ja) * 2009-03-20 2013-11-13 三菱マテリアル株式会社 ルテニウムの精製回収方法
CN101797649B (zh) * 2010-01-19 2012-09-05 兰州大学 一种制备高纯钌的方法及装置

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
JPS5322114A (en) * 1976-06-21 1978-03-01 Nat I Fuoa Metaraajii Separating and refining method of ruthenium
JPH09316560A (ja) * 1996-05-27 1997-12-09 Nikko Kinzoku Kk 白金の回収方法
JP2006183099A (ja) * 2004-12-28 2006-07-13 Nippon Mining & Metals Co Ltd 白金中の不純物除去方法
JP2009144183A (ja) * 2007-12-12 2009-07-02 Mitsubishi Materials Corp 白金の回収方法
JP2010222613A (ja) * 2009-03-20 2010-10-07 Mitsubishi Materials Corp 白金の回収処理方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2014201077B2 (en) * 2013-03-05 2015-08-13 Heraeus Precious Metals Gmbh & Co. Kg Method for producing highly pure platinum powder, as well as platinum powder that can be obtained according to said method, and use thereof
CN103627902A (zh) * 2013-04-25 2014-03-12 上海派特贵金属有限公司 一种从失效贵金属催化剂中回收铑的方法
CN111926195A (zh) * 2020-06-24 2020-11-13 重庆材料研究院有限公司 一种从铂合金废料中制备高纯铂的方法
CN112126789A (zh) * 2020-09-17 2020-12-25 朱俊 一种氯铂酸溶液浓缩工艺及设备

Also Published As

Publication number Publication date
SG186401A1 (en) 2013-01-30
CN102959103A (zh) 2013-03-06
CN102959103B (zh) 2014-03-05
JP5399510B2 (ja) 2014-01-29
US20130139648A1 (en) 2013-06-06
JPWO2012029379A1 (ja) 2013-10-28
MY160898A (en) 2017-03-31

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