JP2003247030A - Method for recovering noble metal - Google Patents

Method for recovering noble metal

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Publication number
JP2003247030A
JP2003247030A JP2002043712A JP2002043712A JP2003247030A JP 2003247030 A JP2003247030 A JP 2003247030A JP 2002043712 A JP2002043712 A JP 2002043712A JP 2002043712 A JP2002043712 A JP 2002043712A JP 2003247030 A JP2003247030 A JP 2003247030A
Authority
JP
Japan
Prior art keywords
metal
noble metal
noble
active
recovering
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.)
Granted
Application number
JP2002043712A
Other languages
Japanese (ja)
Other versions
JP3741275B2 (en
Inventor
Toru Okabe
徹 岡部
Masashi Maeda
正史 前田
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.)
Foundation for the Promotion of Industrial Science
Original Assignee
Foundation for the Promotion of Industrial Science
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 Foundation for the Promotion of Industrial Science filed Critical Foundation for the Promotion of Industrial Science
Priority to JP2002043712A priority Critical patent/JP3741275B2/en
Publication of JP2003247030A publication Critical patent/JP2003247030A/en
Application granted granted Critical
Publication of JP3741275B2 publication Critical patent/JP3741275B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Manufacture And Refinement Of Metals (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a new method for recovering noble metals where neither large amounts of acid nor steps such as copper refining are required. <P>SOLUTION: This method for noble metal recovery is a method for recovering a noble metal 2 from a base material 1 containing the noble metal 2 and/or its compound and comprises steps of: forming a metallic compound 3a of the noble metal 2 and an active metal (vapor) 3; and dissolving the metallic compound 3a by acid to leach it from the base material 1. <P>COPYRIGHT: (C)2003,JPO

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、貴金属の回収方法
に関するものであり、特に、電子材料や触媒のスクラッ
プ等から選択的に高効率で貴金属を回収する技術に関す
るものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for recovering precious metals, and more particularly to a technology for selectively recovering precious metals from scraps of electronic materials and catalysts with high efficiency.

【0002】[0002]

【従来の技術】電子材料や触媒などのスクラップ中の貴
金属を分離、回収する場合、スクラップ全体を溶解ある
いは熱分解し、目的の貴金属を抽出、分離する手法が従
来行われてきた。これは、貴金属が共存するスクラップ
よりも化学的に安定であるため、貴金属のみを選択的に
溶解させることが困難なためである。現状では、少量の
貴金属が含まれるスクラップからの回収を行う場合、ス
クラップ全体を溶解させるために多量の酸を必要とし、
同時に有用でない金属を含む多量の廃液が発生する。一
方、銅や水銀などを抽出剤(コレクターメタル)として
利用し、貴金属を回収する手法も古くから行われてお
り、乾式銅精練プロセスが利用できる場合、道中の貴金
属の回収を容易に行えるため、銅を抽出剤として利用す
ることができるが、地域や状況によっては銅精練プロセ
スを利用できない場合がある。また、水銀を抽出剤とし
て利用することは環境保全の観点から好ましくない。
2. Description of the Related Art In the case of separating and recovering noble metals in scraps such as electronic materials and catalysts, a method of dissolving or pyrolyzing the whole scraps and extracting and separating the target noble metal has been conventionally used. This is because it is chemically more stable than scrap in which precious metals coexist, and it is difficult to selectively dissolve only precious metals. Currently, when recovering from scrap containing a small amount of precious metal, a large amount of acid is required to dissolve the entire scrap,
At the same time, a large amount of waste liquid containing a non-useful metal is generated. On the other hand, the method of recovering precious metals using copper or mercury as an extractant (collector metal) has also been used for a long time, and if a dry copper scouring process is available, it is possible to easily recover precious metals in the road. Although copper can be used as an extractant, copper scouring processes may not be available in some areas and circumstances. Further, it is not preferable to use mercury as an extractant from the viewpoint of environmental protection.

【0003】[0003]

【発明が解決しようとする課題】本発明は、上記の課題
を解決するために成されたものであって、多量の酸を使
用することなく、また銅精練などの工程を必要としな
い、新規な貴金属の回収方法を提供することを目的とし
ている。
SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and does not use a large amount of acid and does not require steps such as copper scouring. The purpose is to provide a method of recovering precious metals.

【0004】[0004]

【課題を解決するための手段】上記の目的を達成するた
めに、本発明は以下の構成を採用した。本発明に係る貴
金属の回収方法は、貴金属及び/又はその化合物を含む
基材から前記貴金属を回収する方法であって、前記貴金
属と活性金属との金属化合物を生成する工程と、前記金
属化合物を酸により溶解し、前記基材から浸出させる工
程と、を含むことを特徴とする。上述のように、貴金属
は化学的に安定であり、廃触媒や電子機器部品からの貴
金属の回収には、溶けにくい貴金属を溶解するために多
量の酸を要し、またこのような多量の酸による溶解によ
り貴金属と共存する他の物質までも溶解される。そのた
め、多量の酸の消費と、多量の廃液の発生が問題となっ
ていたが、本発明に係る回収方法によれば、溶解工程を
行う前に、化学的に安定な貴金属を活性金属と合金化
し、酸に溶解し易い状態とするので、少量の酸を用いて
選択的に貴金属を含む金属化合物を浸出させることがで
きる。従って、係る回収方法によれば、選択的に貴金属
を浸出させることで回収効率を向上させることができ、
またその回収コストも大幅に低減させることができる。
また、本発明に係る回収方法では、活性金属と貴金属と
の化学的な親和力が強く、両者の金属化物が容易に生成
されることを利用している点にも大きな特徴を有してい
る。すなわち、活性金属は、被処理物に含まれる貴金属
と優先的に結合し、容易かつ速い溶解速度で溶解する金
属化合物を形成するため、酸による溶解で被処理物から
貴金属を選択的に浸出させることができる。
In order to achieve the above object, the present invention has the following constitutions. A method for recovering a noble metal according to the present invention is a method for recovering the noble metal from a base material containing a noble metal and / or a compound thereof, wherein a step of producing a metal compound of the noble metal and an active metal, and the metal compound Dissolving with an acid and leaching from the base material. As described above, precious metals are chemically stable, and recovery of precious metals from waste catalysts and electronic equipment parts requires a large amount of acid to dissolve the insoluble precious metal, and such a large amount of acid is also required. Other substances that coexist with the noble metal are also dissolved by the dissolution by. Therefore, consumption of a large amount of acid and generation of a large amount of waste liquid have been problems, but according to the recovery method of the present invention, a chemically stable noble metal and an active metal are alloyed with each other before performing the melting step. As a result, the metal compound containing the noble metal can be selectively leached out by using a small amount of acid because it is converted into a state in which it easily dissolves in an acid. Therefore, according to the recovery method, the recovery efficiency can be improved by selectively leaching the noble metal,
Also, the recovery cost can be significantly reduced.
In addition, the recovery method according to the present invention is also characterized in that it has a strong chemical affinity between the active metal and the noble metal and that a metallized product of both is easily produced. That is, the active metal preferentially binds to the noble metal contained in the object to be processed and forms a metal compound that dissolves easily and at a high dissolution rate, so that the noble metal is selectively leached from the object to be processed by acid dissolution. be able to.

【0005】次に、本発明に係る貴金属の回収方法にお
いては、前記金属化合物を生成する工程が、前記活性金
属の気相雰囲気中で、前記基材上の貴金属と前記活性金
属とを反応させる気相反応工程とされることが好まし
い。すなわち、本発明に係る回収方法では、基材に含ま
れる貴金属と、活性金属との反応を気相を介して行うこ
とができる。そのため、自動車用触媒などの複雑な形状
を有するスクラップから貴金属の回収を行う場合にも、
貴金属と活性金属とを反応させることが可能であり、回
収効率を高めることができる。また、被処理物を破砕し
なくとも貴金属と活性金属との金属化合物を生成させる
ことができるので、工数の減少による回収コストの低減
を図ることができる。
Next, in the method for recovering a noble metal according to the present invention, the step of producing the metal compound causes the noble metal on the base material to react with the active metal in a gas phase atmosphere of the active metal. A gas phase reaction step is preferred. That is, in the recovery method according to the present invention, the reaction between the noble metal contained in the base material and the active metal can be performed via the gas phase. Therefore, even when recovering precious metals from scraps with complicated shapes such as automobile catalysts,
It is possible to react the noble metal with the active metal, and the recovery efficiency can be improved. Further, since the metal compound of the noble metal and the active metal can be generated without crushing the object to be treated, it is possible to reduce the recovery cost due to the reduction of man-hours.

【0006】次に、本発明に係る貴金属の回収方法は、
前記貴金属と活性金属との金属化合物を生成した後、前
記金属化合物を酸化させる酸化工程を含む回収方法とす
ることができる。本発明に係る回収方法では、貴金属と
活性金属との金属化合物を生成し、この金属化合物を酸
により浸出させることで、基材と貴金属との分離を行う
ようになっているが、この浸出工程において、金属化合
物が溶解される際に水素が発生する。これは、金属化合
物に含まれる活性金属が酸化されるために起こる現象で
あるが、本構成では、金属化合物を予め酸化させておく
ので、酸による浸出を行う際の水素発生量を低減するこ
とができ、同時に溶解に必要な酸の量を低減することが
できる。
Next, the method for recovering precious metals according to the present invention is as follows.
After the metal compound of the noble metal and the active metal is generated, the recovery method may include an oxidation step of oxidizing the metal compound. In the recovery method according to the present invention, a metal compound of a noble metal and an active metal is produced, and the metal compound is leached with an acid to separate the base material and the noble metal. In, hydrogen is generated when the metal compound is dissolved. This is a phenomenon that occurs because the active metal contained in the metal compound is oxidized. In this configuration, the metal compound is pre-oxidized, so the amount of hydrogen generated during leaching with an acid should be reduced. And at the same time the amount of acid required for dissolution can be reduced.

【0007】次に、本発明に係る貴金属の回収方法は、
複数種の貴金属及び/又はその化合物が含まれた基材に
対して活性金属と貴金属との反応処理を行い、その後、
酸により前記貴金属を浸出させて前記複数種の貴金属の
回収を行うことを特徴とする。すなわち、本発明に係る
回収方法によれば、液体あるいはガスを貴金属の抽出剤
として使用するため、複数種の貴金属を含む基材から一
様に貴金属を分離することが可能である。従って、例え
ば触媒と電子材料とを同時に処理することもでき、Pt
とRh、PtとAu等の複数の貴金属を含む被処理物も
一括に処理することが可能である。
Next, the method for recovering precious metals according to the present invention is
A reaction treatment of an active metal and a noble metal is performed on a base material containing a plurality of kinds of noble metals and / or compounds thereof, and then,
It is characterized in that the precious metal is leached with an acid to recover the plurality of types of precious metals. That is, according to the recovery method of the present invention, since the liquid or the gas is used as the noble metal extractant, it is possible to uniformly separate the noble metal from the base material containing plural kinds of noble metals. Therefore, for example, the catalyst and the electronic material can be treated at the same time.
It is also possible to collectively process objects to be processed containing a plurality of noble metals such as Rh, Rh, Pt, and Au.

【0008】次に、本発明に係る貴金属の回収方法にお
いては、前記活性金属として、処理温度で10-4atm
以上の蒸気圧を有する金属を用いることが好ましい。上
記範囲の蒸気圧を有する金属を用いることで、貴金属と
反応させるに十分な蒸気圧を保持することができ、貴金
属との反応を促進させることができるとともに、反応速
度を高めて処理時間を短縮することができる。
Next, in the method for recovering a noble metal according to the present invention, the active metal is 10 -4 atm at a processing temperature.
It is preferable to use a metal having the above vapor pressure. By using a metal having a vapor pressure in the above range, it is possible to maintain a sufficient vapor pressure to react with the noble metal, promote the reaction with the noble metal, and increase the reaction rate to shorten the treatment time. can do.

【0009】次に、本発明に係る貴金属の回収方法にお
いては、前記活性金属として、Ca,Mg,Li,N
a,Kから選ばれる1種又は2種以上を用いることが好
ましい。上記に挙げた活性金属を用いるならば、高温で
高い蒸気圧を実現することができるので、高効率で貴金
属と反応させることができ、貴金属を効率的に回収する
ことができる。
Next, in the method of recovering a noble metal according to the present invention, Ca, Mg, Li, N are used as the active metals.
It is preferable to use one or two or more selected from a and K. If the active metals listed above are used, a high vapor pressure can be realized at a high temperature, so that they can be reacted with a noble metal with high efficiency, and the noble metal can be efficiently recovered.

【0010】[0010]

【発明の実施の形態】以下、本発明の実施の形態を図面
を参照して詳細に説明する。図1は、本発明に係る貴金
属の回収方法の一実施の形態を示す断面工程図である。
本実施形態では、図1Aに示すように、基材1上に担持
された貴金属粒子2を回収する場合の回収工程について
説明する。図1Aに示す貴金属を含む基材1は、例えば
自動車等の触媒や、電子機器部品、装飾品等の貴金属担
持部分を概念的に示すものである。さらに図1Aは基材
1の貴金属粒子2と活性金属が反応する場合を例示して
いるが、貴金属は面状であっても、複雑に入り組んだ構
造でもかまわない。また、本回収法により効果的に回収
できる貴金属粒子2としては、Au,Ag,Pt,R
h,Pd,Ir等である。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. FIG. 1 is a sectional process drawing showing an embodiment of a method for recovering a noble metal according to the present invention.
In the present embodiment, as shown in FIG. 1A, a recovery process for recovering the noble metal particles 2 carried on the base material 1 will be described. The base material 1 containing a noble metal shown in FIG. 1A conceptually shows a noble metal-carrying portion such as a catalyst of an automobile or the like, an electronic device part, a decorative article, or the like. Further, FIG. 1A exemplifies the case where the noble metal particles 2 of the base material 1 react with the active metal, but the noble metal may have a planar shape or a complicated intricate structure. The precious metal particles 2 that can be effectively recovered by this recovery method include Au, Ag, Pt, and R.
h, Pd, Ir, etc.

【0011】本発明に係る回収方法により基材1から貴
金属粒子2を回収するには、まず、図1Bに示すように
基材1を活性金属の蒸気3中に導入する。この活性金属
の蒸気雰囲気は、反応室内でCa,Mg,Li,Na,
K等の金属を高温に加熱し、蒸発させることで形成する
ことができる。すなわち、被処理物である基材1ととも
に、これらの活性金属を反応室内へ導入し、反応室内を
500〜1200℃程度とすることで、容易に活性金属
の蒸気雰囲気に基材1を曝すことができる。この工程に
より、貴金属粒子2と活性金属の蒸気3とが反応して、
両者の金属化合物が生成される。尚、上記活性金属とし
ては、貴金属との化学的親和性の点で上記に挙げた金属
を用いることが好ましいが、10-4atm以上の蒸気圧
を有する金属であれば適用可能である。
In order to recover the noble metal particles 2 from the base material 1 by the recovery method according to the present invention, first, the base material 1 is introduced into the vapor 3 of the active metal as shown in FIG. 1B. The vapor atmosphere of this active metal is Ca, Mg, Li, Na,
It can be formed by heating a metal such as K to a high temperature and evaporating it. That is, by introducing these active metals into the reaction chamber together with the substrate 1 which is the object to be treated and keeping the temperature inside the reaction chamber at about 500 to 1200 ° C., the substrate 1 is easily exposed to the active metal vapor atmosphere. You can By this step, the precious metal particles 2 and the active metal vapor 3 react with each other,
Both metal compounds are produced. As the active metal, it is preferable to use the metals listed above in terms of chemical affinity with the noble metal, but any metal having a vapor pressure of 10 −4 atm or higher is applicable.

【0012】そして、図1Cに示すように、貴金属粒子
2と活性金属の蒸気3との反応により金属化合物3aが
基材1上に形成されたならば、基材1上の金属化合物3
aを酸により浸出させる。この工程は、王水や塩酸、硝
酸等の酸に基材1を浸漬することで、容易に行うことが
できる。その際の酸を30℃以上に加熱しておけば、金
属化合物3aの浸出が促進され、より短時間での処理が
可能となる。そして、図1Cに示す金属化合物3aは、
酸に対する溶解性が高いため、図1Dに示すように、浸
出工程に供された後の基材1はほとんど溶解されずに残
る。従って、上記浸出工程により、不要な金属が少ない
金属化合物3aの溶液を得ることができる。
Then, as shown in FIG. 1C, if the metal compound 3a is formed on the substrate 1 by the reaction of the noble metal particles 2 and the vapor 3 of the active metal, the metal compound 3 on the substrate 1 is formed.
Leach a with acid. This step can be easily performed by immersing the base material 1 in an acid such as aqua regia or hydrochloric acid or nitric acid. If the acid at that time is heated to 30 ° C. or higher, the leaching of the metal compound 3a is promoted, and the treatment can be performed in a shorter time. Then, the metal compound 3a shown in FIG. 1C is
Due to its high solubility in acid, as shown in FIG. 1D, the substrate 1 after being subjected to the leaching step remains almost undissolved. Therefore, the solution of the metal compound 3a containing less unnecessary metal can be obtained by the leaching step.

【0013】次に、上記浸出工程により得られた金属化
合物3aの溶液に、所定の処理を施すことで、貴金属を
回収することができる。この溶液の処理工程としては、
例えば金属化合物3aとして活性金属とPtとの金属化
合物を形成し、王水による浸出を行う場合には、以下の
方法でPtを回収することができる。まず、浸出工程で
得られた溶液を加熱して液体を蒸発させた後、塩酸と、
過酸化水素水とを混合した溶液に溶解させ、その後、飽
和塩化アンモニウム溶液により(NH42PtCl6
沈殿物を析出させる。そして、得られた沈殿物を濾過
し、乾燥させた後、沈殿物を焼成することでPtを回収
することができる。また、上述したように、本発明に係
る回収方法では、貴金属化合物3aの溶液に含まれる不
純物が少ないため、溶液から高純度の貴金属を得ること
ができる。
Next, the precious metal can be recovered by subjecting the solution of the metal compound 3a obtained by the leaching step to a predetermined treatment. The processing steps for this solution include:
For example, when a metal compound of an active metal and Pt is formed as the metal compound 3a and leaching with aqua regia is performed, Pt can be recovered by the following method. First, after heating the solution obtained in the leaching step to evaporate the liquid, hydrochloric acid and
It is dissolved in a mixed solution of hydrogen peroxide water, and then a precipitate of (NH 4 ) 2 PtCl 6 is deposited with a saturated ammonium chloride solution. Then, Pt can be recovered by filtering the obtained precipitate, drying it, and then baking the precipitate. Further, as described above, in the recovery method according to the present invention, since the solution of the precious metal compound 3a contains few impurities, it is possible to obtain a highly pure precious metal from the solution.

【0014】上記実施の形態では、貴金属粒子2と活性
金属との反応を、活性金属の蒸気3を用いて気相で行っ
たが、貴金属粒子2と活性金属との反応により金属化合
物を生成する工程は、気相反応に限定されず、固相ある
いは液相での反応も適用することができる。活性金属
は、貴金属との化学的親和性が極めて高いため、例えば
固相で反応させるために、活性金属の酸化物を用いたと
しても反応温度等の反応条件を適切に設定することで、
容易に活性金属と貴金属との金属化合物を生成させるこ
とができる。
In the above embodiment, the reaction between the noble metal particles 2 and the active metal is carried out in the gas phase using the active metal vapor 3. However, the reaction between the noble metal particles 2 and the active metal produces a metal compound. The process is not limited to the gas phase reaction, and a solid phase or liquid phase reaction can also be applied. Since the active metal has extremely high chemical affinity with the noble metal, for example, in order to react in the solid phase, even if an oxide of the active metal is used, by appropriately setting the reaction conditions such as the reaction temperature,
A metal compound of an active metal and a noble metal can be easily produced.

【0015】さらに、上記実施の形態では、基材1上に
金属化合物3aを形成した後、酸による浸出を行う場合
について説明したが、この酸による浸出の前に、金属化
合物3aを酸化させ、酸化後の金属化合物3aを酸によ
り浸出させても良い。このような工程とすることで、浸
出工程における水素の発生を抑え、安全かつ迅速に浸出
工程を行うことができ、また、浸出工程で必要とされる
酸の量も低減することができる。尚、上記金属化合物3
aの酸化は、例えば、400℃以上で合金を大気中の酸
素と反応させ酸化させることにより容易に行うことがで
きる。
Further, in the above-mentioned embodiment, the case where the metal compound 3a is formed on the substrate 1 and then the leaching with the acid is carried out, but the metal compound 3a is oxidized before the leaching with the acid, The metal compound 3a after oxidation may be leached with an acid. With such a step, generation of hydrogen in the leaching step can be suppressed, the leaching step can be performed safely and quickly, and the amount of acid required in the leaching step can be reduced. The above metal compound 3
The oxidation of a can be easily performed, for example, by reacting the alloy with oxygen in the atmosphere at 400 ° C. or higher to oxidize the alloy.

【0016】[0016]

【実施例】次に、実施例により本発明を更に詳細に説明
するが、以下の実施例は本発明を限定するものではな
い。
EXAMPLES Next, the present invention will be described in more detail by way of examples, but the following examples do not limit the present invention.

【0017】(実施例1)本例では、本発明に係る回収
方法により、貴金属を選択的に酸に溶解させることがで
き、また高収率で回収できることを検証するために、各
種の貴金属の紛体を試料とし、これらの試料を活性金属
と反応させて酸に溶解させ、この溶解液から再度貴金属
を回収する実験を行った。活性金属にはCa及びMgを
用い、貴金属にはPtを用いた。まず、活性金属と貴金
属との反応実験及び生成した化合物の酸への溶解実験に
ついて以下に説明する。ステンレス鋼製の円筒容器(内
径20mm、高さ36mm)の底部に活性金属(Ca,
Mg)を配置し、容器内のこれらの活性金属の上方にス
テンレス鋼製の試料皿を配置し、この皿にPt片0.1
〜1.0gを載せ、円筒容器を封止した。各試料におけ
る活性金属の種類/重量と、試料皿に載せたPt重量と
の組み合わせを表1に示す。
(Example 1) In this example, in order to verify that the noble metal can be selectively dissolved in an acid by the recovery method according to the present invention and can be recovered in high yield, various noble metals can be recovered. An experiment was conducted in which powder was used as a sample, these samples were reacted with an active metal, dissolved in an acid, and the precious metal was recovered again from this solution. Ca and Mg were used as the active metals, and Pt was used as the noble metal. First, a reaction experiment between an active metal and a noble metal and a dissolution experiment of a produced compound in an acid will be described below. At the bottom of a stainless steel cylindrical container (inner diameter 20 mm, height 36 mm), an active metal (Ca,
Mg) is placed and a stainless steel sample pan is placed above these active metals in the vessel and the Pt strip 0.1
~ 1.0 g was placed and the cylindrical container was sealed. Table 1 shows the combination of the type / weight of the active metal in each sample and the weight of Pt placed on the sample dish.

【0018】次に、上記にて用意した円筒容器のうち数
セットを、ステンレス鋼製の反応容器に装入し、反応容
器の底部に脱酸剤としてスポンジチタンを入れた後、溶
接封入した。そして、封入後の反応容器を電気炉内に設
置し、表1に示す温度、時間で反応させ、その後、所定
時間一定温度に保持した後に電気炉から取り出し冷却し
た。次いで、反応容器を切断して内部の円筒容器を取り
出し、円筒容器から試料皿上の合金粉末を回収した。
Next, several sets of the cylindrical containers prepared above were charged into a stainless steel reaction container, titanium sponge was added as a deoxidizing agent to the bottom of the reaction container, and then welded and sealed. Then, the sealed reaction container was placed in an electric furnace, reacted at the temperature and time shown in Table 1, and then kept at a constant temperature for a predetermined time and then taken out from the electric furnace and cooled. Then, the reaction container was cut to take out the inner cylindrical container, and the alloy powder on the sample dish was recovered from the cylindrical container.

【0019】[0019]

【表1】 [Table 1]

【0020】次に、上記にて得られた各試料を、王水で
溶解してPtを含む水溶液を作製した。この溶解工程に
おいて、いずれの試料も王水に良好に溶解され、Pt粉
末を王水に溶解する場合に比して、極めて迅速かつ容易
に溶解を行うことができ、また、溶解に必要な王水の量
も大幅に少ない量であった。また、上記にて得られた合
金を、酸で溶解する前に合金を大気中で酸化した場合
も、極めて迅速かつ容易に溶解を行うことができ、更に
少ない王水使用量で溶解を行うことができた。
Next, each of the samples obtained above was dissolved in aqua regia to prepare an aqueous solution containing Pt. In this dissolving step, all the samples are well dissolved in aqua regia, and the Pt powder can be dissolved extremely quickly and easily as compared with the case where Pt powder is dissolved in aqua regia, and the amount of royal water required for dissolution is The amount of water was also much smaller. In addition, the alloy obtained above can be dissolved extremely quickly and easily even when the alloy is oxidized in the atmosphere before being dissolved with an acid, and the dissolution should be performed with a smaller amount of aqua regia. I was able to.

【0021】上記工程にて得られるPtを含む水溶液か
らPtを回収できることを検証するために、表2に示す
合金の水溶液に対して以下の操作を行った。まず、各合
金の水溶液から硝酸を取り除くため、溶解液を140℃
のホットプレートで溶液が無くなるまで加熱した。この
脱硝処理後に1Nの塩酸10ml、酸化剤としてH22
(過酸化水素水)1mlを加えた後、飽和塩化アンモニ
ウム(NH4Cl)溶液を約40ml注ぎ、黄色の(N
42PtCl6の沈殿物を生成させた。そして、さら
に反応を促進させるために飽和塩化アンモニウム溶液を
追加して、その後約1時間加温状態(70〜80℃)に
保持した。その後、吸引濾過により沈殿物を濾過し、濾
紙上の沈殿物を140℃のホットプレートにより乾燥さ
せた。そして、この沈殿物をアルミナ坩堝中でガスバー
ナーを用いて焼成することにより、Ptを回収し、回収
されたPtの重量を測定した。その結果を表2に併記す
る。
In order to verify that Pt can be recovered from the Pt-containing aqueous solution obtained in the above step, the following operations were performed on the alloy aqueous solutions shown in Table 2. First, to remove nitric acid from the aqueous solution of each alloy, dissolve the solution at 140 ° C.
The solution was heated on the hot plate of the above until the solution was exhausted. After this denitration treatment, 10 ml of 1N hydrochloric acid, H 2 O 2 as an oxidizing agent
After adding 1 ml of (hydrogen peroxide solution), about 40 ml of a saturated ammonium chloride (NH 4 Cl) solution was poured to give a yellow (N 4
H 4) to produce a precipitate of 2 PtCl 6. Then, a saturated ammonium chloride solution was added in order to further accelerate the reaction, and then the mixture was kept in a heated state (70 to 80 ° C.) for about 1 hour. Then, the precipitate was filtered by suction filtration, and the precipitate on the filter paper was dried by a 140 ° C. hot plate. Then, Pt was recovered by firing the precipitate in an alumina crucible using a gas burner, and the weight of the recovered Pt was measured. The results are also shown in Table 2.

【0022】[0022]

【表2】 [Table 2]

【0023】表2に示すように、本発明に係る貴金属の
回収方法を適用するならば、極めて高い収率で貴金属を
回収できることが確認された。このように、本発明に係
る貴金属の回収方法によれば、基材上に担持された貴金
属を容易かつ選択的に浸出させることができ、また、浸
出により得られる溶液から、高収率で貴金属を回収する
ことができる。
As shown in Table 2, it was confirmed that the noble metal can be recovered in an extremely high yield if the method for recovering the noble metal according to the present invention is applied. As described above, according to the method for recovering a noble metal according to the present invention, the noble metal supported on the substrate can be easily and selectively leached out, and the noble metal can be highly yielded from the solution obtained by the leaching. Can be recovered.

【0024】[0024]

【発明の効果】以上、詳細に説明したように、本発明に
係る貴金属の回収方法は、貴金属及び/又はその化合物
を含む基材から前記貴金属を回収する方法であって、前
記貴金属と活性金属との金属化合物を生成する工程と、
前記金属化合物を酸により溶解し、前記基材から浸出さ
せる工程と、を含む回収方法とされたことで、貴金属を
選択的、かつ迅速に酸に溶解させることができるので、
得られた浸出溶液から効率よく貴金属を回収することが
できる。
As described above in detail, the method for recovering a noble metal according to the present invention is a method for recovering the noble metal from a base material containing the noble metal and / or its compound, A step of producing a metal compound with
By dissolving the metal compound with an acid and leaching from the base material, the recovery method includes the step of selectively and rapidly dissolving the noble metal in the acid.
The precious metal can be efficiently recovered from the obtained leaching solution.

【0025】次に、本発明に係る貴金属の回収方法にお
いて、前記金属化合物を生成する工程が、前記活性金属
の気相雰囲気中で、前記基材上の貴金属と前記活性金属
とを反応させる気相反応工程とするならば、自動車用触
媒などの複雑な形状を有するスクラップから貴金属の回
収を行う場合にも、貴金属と活性金属とを反応させるこ
とが可能であり、回収効率を高めることができる。
Next, in the method for recovering a noble metal according to the present invention, the step of forming the metal compound is a gas for reacting the noble metal on the base material with the active metal in a gas phase atmosphere of the active metal. If it is a phase reaction process, it is possible to react the noble metal with the active metal even when recovering the noble metal from scrap having a complicated shape such as an automobile catalyst, so that the recovery efficiency can be improved. .

【0026】次に、本発明に係る貴金属の回収方法にお
いて、前記貴金属と活性金属との金属化合物を生成した
後、前記金属化合物を酸化させる酸化工程を含む回収方
法とするならば、浸出工程における水素発生量および溶
解に必要な酸の量を低減することができ、安全かつ効率
良く貴金属の回収を行うことができる。
Next, in the recovery method of the noble metal according to the present invention, if the recovery method includes an oxidation step of oxidizing the metal compound after the metal compound of the noble metal and the active metal is produced, in the leaching step, The amount of hydrogen generated and the amount of acid required for dissolution can be reduced, and the precious metal can be recovered safely and efficiently.

【図面の簡単な説明】[Brief description of drawings]

【図1】 図1は、本発明に係る貴金属の回収方法を示
す概念図である。
FIG. 1 is a conceptual diagram showing a precious metal recovery method according to the present invention.

【符号の説明】[Explanation of symbols]

1 基材 2 貴金属 3 活性金属蒸気 3a 活性金属と貴金属との金属化合物 1 base material 2 precious metals 3 Active metal vapor 3a Metal compound of active metal and noble metal

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】 貴金属及び/又はその化合物を含む基材
から前記貴金属を回収する方法であって、 前記貴金属と活性金属との金属化合物を生成する工程
と、 前記金属化合物を酸により溶解し、前記基材から浸出さ
せる工程と、 を含むことを特徴とする貴金属の回収方法。
1. A method for recovering the noble metal from a base material containing a noble metal and / or a compound thereof, the method comprising: forming a metal compound of the noble metal and an active metal; dissolving the metal compound with an acid; And a step of leaching from the base material.
【請求項2】 前記金属化合物を生成する工程が、前記
活性金属の気相雰囲気中で、前記基材上の貴金属と前記
活性金属とを反応させる気相反応工程とされたことを特
徴とする請求項1に記載の貴金属の回収方法。
2. The step of forming the metal compound is a gas phase reaction step of reacting a noble metal on the base material with the active metal in a gas phase atmosphere of the active metal. The precious metal recovery method according to claim 1.
【請求項3】 前記貴金属と活性金属との金属化合物を
生成した後、前記金属化合物を酸化させる酸化工程を含
むことを特徴とする請求項1又は2に記載の貴金属の回
収方法。
3. The method for recovering a noble metal according to claim 1, further comprising an oxidation step of oxidizing the metal compound after forming a metal compound of the noble metal and an active metal.
【請求項4】 複数種の貴金属及び/又はその化合物が
含まれた基材に対して活性金属と貴金属との反応処理を
行い、その後、酸により前記貴金属を浸出させて前記複
数種の貴金属の回収を行うことを特徴とする請求項1か
ら3のいずれか1項に記載の貴金属の回収方法。
4. A substrate containing a plurality of noble metals and / or compounds thereof is subjected to a reaction treatment of an active metal and a noble metal, and then the noble metal of the plurality of noble metals is leached with an acid. The precious metal recovery method according to claim 1, wherein the precious metal is recovered.
【請求項5】 前記活性金属として、処理温度で10-4
atm以上の蒸気圧を有する金属を用いることを特徴と
する請求項1から4のいずれか1項に記載の貴金属の回
収方法。
5. The active metal is 10 −4 at a processing temperature.
The method for recovering a noble metal according to any one of claims 1 to 4, wherein a metal having a vapor pressure of atm or higher is used.
【請求項6】 前記活性金属として、Ca,Mg,N
a,Kから選ばれる1種又は2種以上を用いることを特
徴とする請求項1から5のいずれか1項に記載の貴金属
の回収方法。
6. The active metal is Ca, Mg, N.
The method for recovering a noble metal according to any one of claims 1 to 5, wherein one or more selected from a and K is used.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005248280A (en) * 2004-03-05 2005-09-15 Foundation For The Promotion Of Industrial Science Method for recovering noble metal
JP2009256745A (en) * 2008-04-18 2009-11-05 Foundation For The Promotion Of Industrial Science Method for recovering noble metal
JP2009256744A (en) * 2008-04-18 2009-11-05 Foundation For The Promotion Of Industrial Science Method for recovering noble metal
WO2010021341A1 (en) * 2008-08-20 2010-02-25 国立大学法人東京大学 Method for recovering noble metal
JP2015178652A (en) * 2014-03-19 2015-10-08 日本電信電話株式会社 Metallic material recovery method

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Publication number Priority date Publication date Assignee Title
CN102212704A (en) * 2011-05-23 2011-10-12 贵研铂业股份有限公司 Dissolution method of noble metal material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005248280A (en) * 2004-03-05 2005-09-15 Foundation For The Promotion Of Industrial Science Method for recovering noble metal
JP4595082B2 (en) * 2004-03-05 2010-12-08 財団法人生産技術研究奨励会 Precious metal recovery method
JP2009256745A (en) * 2008-04-18 2009-11-05 Foundation For The Promotion Of Industrial Science Method for recovering noble metal
JP2009256744A (en) * 2008-04-18 2009-11-05 Foundation For The Promotion Of Industrial Science Method for recovering noble metal
WO2010021341A1 (en) * 2008-08-20 2010-02-25 国立大学法人東京大学 Method for recovering noble metal
JP5354305B2 (en) * 2008-08-20 2013-11-27 国立大学法人 東京大学 Precious metal recovery method
JP2015178652A (en) * 2014-03-19 2015-10-08 日本電信電話株式会社 Metallic material recovery method

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