JPS58194745A - Recovery of ruthenium - Google Patents
Recovery of rutheniumInfo
- Publication number
- JPS58194745A JPS58194745A JP7565382A JP7565382A JPS58194745A JP S58194745 A JPS58194745 A JP S58194745A JP 7565382 A JP7565382 A JP 7565382A JP 7565382 A JP7565382 A JP 7565382A JP S58194745 A JPS58194745 A JP S58194745A
- Authority
- JP
- Japan
- Prior art keywords
- ruthenium
- base material
- oxide
- ruthenium oxide
- alkali
- 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
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、ルテニウム酸化物又は実質的にルテニウム酸
化物からなる混晶体を被覆した耐食性基体からルテニウ
ムを回収する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for recovering ruthenium from a corrosion-resistant substrate coated with ruthenium oxide or a mixed crystal consisting essentially of ruthenium oxide.
ルテニウム酸化物は、電気接点材料や抵抗ベーストなど
として電気部品や電子部品に広（使用されており、また
、か性ソーダ電解、発電所等の冷却水用海水電解および
アルカリ飲料水製造用電解電極として広く使用されてい
る。ルテニウム酸化物は多くの場合、アルミナ、シリカ
等の耐食性セラミックスやチタン、タンタル、ジルコニ
ウム、ニオブ等の耐食性金属に被覆されている。このル
テニウム酸化物を上記耐食性基体がら回収する方法とし
ては、従来、必要に応じてまずアルミナ粒などを吹き付
けて基体から物理的に剥離し、この剥離物を過酸化物を
含むアルカリ溶融塩中で処理しり溶性のルチン酸アルカ
リとした後、水や酸などで抽出し酸化性雰囲気中で四酸
化ルテニウムを生成揮発させ回収を行なっていた。Ruthenium oxide is widely used in electrical and electronic components as electrical contact materials and resistance bases, and is also used in caustic soda electrolysis, seawater electrolysis for cooling water in power plants, and electrolytic electrodes for alkaline drinking water production. Ruthenium oxide is often coated with corrosion-resistant ceramics such as alumina and silica, and corrosion-resistant metals such as titanium, tantalum, zirconium, and niobium.The ruthenium oxide is recovered from the above-mentioned corrosion-resistant substrate. Conventionally, the conventional method is to first physically peel off the substrate by spraying alumina grains, etc., if necessary, and then treat the peeled off material in an alkaline molten salt containing peroxide to make it a soluble rutinate alkali. Ruthenium tetroxide was recovered by extraction with water or acid, and ruthenium tetroxide was produced and volatilized in an oxidizing atmosphere.
しかしながら、従来の回収方法では、剥離のときに酸化
１ルテニウムは摩耗したアルミナ粒等と混り合いルテニ
ウム含有率の低い剥離物が得られる。However, in the conventional recovery method, monoruthenium oxide is mixed with worn alumina grains and the like during peeling, resulting in a peeled product with a low ruthenium content.
また、基体形状が複雑な場合は不必要な基体の部分まで
摩耗をせざるをえない、そして、ルテニウムがわずかに
もかかわらず剥離物全体を溶融塩とせざるをえず、且つ
、アルミナ粒等が溶融アルカリと反応するため必要以上
のアルカリ塩を投入しなければならなかった。そのため
、ルテニウムの抽出が困難で、また抽出した後の残液に
は多量のアルミニウムイオンなどが含まれこれもまた処
理する必要があり、不経済であった。In addition, if the shape of the substrate is complex, unnecessary parts of the substrate must be worn away, and even though there is only a small amount of ruthenium, the entire peeled off material must be converted into molten salt, and alumina particles, etc. reacts with the molten alkali, so more alkali salt than necessary had to be added. Therefore, it was difficult to extract ruthenium, and the residual liquid after extraction contained a large amount of aluminum ions, which also had to be treated, making it uneconomical.
本発明は上記欠点に鑑みなされたものであり、古島でか
つ高回収−率をうるルテニウムの回収方法を提供するも
のである。The present invention has been made in view of the above-mentioned drawbacks, and provides a method for recovering ruthenium from old islands and achieving a high recovery rate.
本発明は、ルテニウム酸化物又は実質的にルテニウム酸
化物からなる混晶体を被覆した耐食性基体からルテニウ
ムを回収する方法において、当該ルテニウム酸化物又は
実質的にルテニウム酸化物からなる混晶体を還元して金
属ルテニウムとした後、塩素ガス又は酸化性の塩素化合
物を含むアルカリ溶液中でその金属ルテニウムをルチン
酸アルカリ （Ｍ”、 Ｒｕ Ｏ，を又はＭ” Ｒｕ
Ｏ４、ただし、Ｍ＋は１価のアルカリ金属、Ｍ’４よ２
価のアルカリ金属をいう。）として耐食性基体から溶離
させることを特徴とするルテニウムの回収方法である。The present invention provides a method for recovering ruthenium from a corrosion-resistant substrate coated with ruthenium oxide or a mixed crystal consisting essentially of ruthenium oxide, in which the ruthenium oxide or the mixed crystal consisting essentially of ruthenium oxide is reduced. After making metal ruthenium, the metal ruthenium is converted into alkali rutinate (M”, Ru O, or M” Ru
O4, where M+ is a monovalent alkali metal, M'4 yo 2
valence alkali metal. ) is a method for recovering ruthenium, characterized by elution from a corrosion-resistant substrate.
すなわち、本発明はルテニウム酸化物を金属ルテニウふ
とした後これを基体から溶離させることを骨子とする０
本発明において最初にルテニウム酸化物又は実質的にル
テニウム酸化物からなる混晶体を還元して金属ルテニウ
ムとするのは、ルテニウム酸化物の溶解が困難だからで
ある。還元方法としては、通常の水素還元、逆電解還元
、テルミット還元などが適用できる。金属ルテニウムと
した後その金属ルテニウムは塩素ガス又は酸化性の塩素
化合物を含むアルカリ水溶液に浸漬される。That is, the main point of the present invention is to convert ruthenium oxide into metal ruthenium and then elute it from the substrate.
In the present invention, ruthenium oxide or a mixed crystal consisting essentially of ruthenium oxide is first reduced to metal ruthenium because it is difficult to dissolve ruthenium oxide. As the reduction method, ordinary hydrogen reduction, reverse electrolytic reduction, thermite reduction, etc. can be applied. After being made into metal ruthenium, the metal ruthenium is immersed in chlorine gas or an alkaline aqueous solution containing an oxidizing chlorine compound.
ここで、塩素ガス又は酸化性の塩素化合物を含むアルカ
リ水溶液を用いるのは、単に塩素化合物を含むアルカリ
水溶液では金属ルテニウムが溶解しないからである。酸
化性の塩素化合物としては、塩Ｓ酸アンモニウムや塩素
酸カリウムなどの塩素酸塩や過塩素酸マグネシウムや過
塩素酸カルシウムなどの過塩素酸塩や酸化塩素や次亜塩
素酸などがあり、耐食性基体の材質に応じて適宜選択で
き ！”する。実質的にルテニウム酸化物から
なる混晶体を還元した場合などで溶解速度が遅いときは
、電解又は加熱により溶解することもできる。これらの
浴で金属ルテニウムを溶解すると金属ルテニウムのみル
チン酸アルカリとして溶離させることができる。アルカ
リ溶液として１価のアルカリ金属を用いれば、金属ルテ
ニウムはＭ；ＲｕＯ４の形で溶解し、２ｈｌｉのアルカ
リ金属を用いればＭ”ＲｕＯ９の形で溶解する。いずれ
の形のルチン酸アルカリでも溶液中には他の妨害金属元
素が含まれていないので容島に生成揮発させ金属ルテニ
ウムを回収することができる。以下、実施例について説
明する。The reason why an alkaline aqueous solution containing chlorine gas or an oxidizing chlorine compound is used here is simply because metal ruthenium does not dissolve in an alkaline aqueous solution containing a chlorine compound. Oxidizing chlorine compounds include chlorates such as ammonium sulfate and potassium chlorate, perchlorates such as magnesium perchlorate and calcium perchlorate, chlorine oxide, and hypochlorous acid, which have corrosion resistance. You can select the appropriate one according to the material of the base! When the dissolution rate is slow, such as when reducing a mixed crystal consisting essentially of ruthenium oxide, it is also possible to dissolve it by electrolysis or heating.When metal ruthenium is dissolved in these baths, only the metal ruthenium becomes rutinic acid. It can be eluted as an alkali. If a monovalent alkali metal is used as the alkaline solution, metal ruthenium will dissolve in the form of M;RuO4, and if a 2hli alkali metal is used, it will dissolve in the form of M''RuO9. Since the solution of any form of alkali rutinate does not contain other interfering metal elements, it is possible to recover metal ruthenium by forming and volatilizing it in Yojima. Examples will be described below.
〔実施例１〕
１０ＸＩＯＸＩ鶴のルテニウム酸化物被覆チタン基体６
０枚を５００℃水素雰囲気中で２０分間還元処理し、微
量の酸化ルテニウムを金属ルテニウムに還元した。これ
を３０％か性ソーダ、溶液８０ｍ１と有効塩素１２％の
次亜塩ｓＭンーダ１０ｍ１に１０枚入れ攪拌しながら室
温で２時間反応させた。この手順をくり返し残りの５０
枚を処理した。水洗後、基体表面をＸ線マイクロアナラ
イザーで分析したところルテニウムは検出できなかった
。次にルチン酸アルカリを含む溶液を８０℃に加熱しな
がら塩素ガスを吹込みルテニウムを酸化揮発させ塩酸溶
液で吸収させ塩化ルテニウムとした。この溶液を濃縮乾
固したところ褐色の塩化ルテニウムの結晶１．４ｇを得
た。[Example 1] Ruthenium oxide coated titanium substrate 6 of 10XIOXI Tsuru
0 sheets were subjected to reduction treatment in a hydrogen atmosphere at 500° C. for 20 minutes to reduce a trace amount of ruthenium oxide to metal ruthenium. Ten pieces of this were placed in 80 ml of a solution of 30% caustic soda and 10 ml of hypochlorite sM powder containing 12% available chlorine, and the mixture was allowed to react at room temperature for 2 hours with stirring. Repeat this procedure until the remaining 50
Processed the pieces. After washing with water, the surface of the substrate was analyzed using an X-ray microanalyzer, and no ruthenium was detected. Next, while heating the solution containing alkali rutinate to 80° C., chlorine gas was blown into the solution to oxidize and volatilize the ruthenium, which was then absorbed by a hydrochloric acid solution to produce ruthenium chloride. When this solution was concentrated to dryness, 1.4 g of brown ruthenium chloride crystals were obtained.
〔実施例２〕
３Ｘ３Ｘ１ｗｍのルテニウム酸化物がガラスとともに焼
成されたアルミナ基体 １００枚を６００℃水素雰囲気
中で６０分間還元処理し、金属ルテニウムに還元した。[Example 2] 100 alumina substrates in which 3×3×1 wm of ruthenium oxide was fired together with glass were subjected to reduction treatment in a hydrogen atmosphere at 600° C. for 60 minutes to reduce them to metallic ruthenium.
これを３０％水酸化カリウム溶液１００ ｍ ｌとｌθ
％塩素酸カリウム溶１３０ｍ ｌに入れ攪拌しながら２
４時間反応させた。水洗後、基体表面をＸ線マイクロア
ナライザーで分析したところルテニウムは検出できなか
った。次にルチン酸ア゛ルカリを含む溶液を８０℃に加
熱しながら塩素ガスを吹込み酸化揮発させたルテニウム
を塩酸溶液で吸収させ塩化ルテニウム酸とした。この溶
液を濃縮乾固したところ褐色の塩化ルテニウムの結晶２
．５ｇを得た。This was mixed with 100 ml of 30% potassium hydroxide solution and lθ
% potassium chlorate solution and add it to 130 ml while stirring.
The reaction was allowed to proceed for 4 hours. After washing with water, the surface of the substrate was analyzed using an X-ray microanalyzer, and no ruthenium was detected. Next, while heating the solution containing alkali rutate to 80° C., chlorine gas was blown into the solution to absorb the oxidized and volatilized ruthenium with a hydrochloric acid solution to obtain ruthenic chloride. When this solution was concentrated to dryness, brown crystals of ruthenium chloride 2 were obtained.
．． 5g was obtained.
〔実施例３〕
ｍ１４４２φ鶴のりベット型電気鋼接点の表面に約２μ
ｍのルテニウム酸化物を被覆したものを１００個はど５
００℃水素雰囲気中でｌＯ分間還元処理した後か性ソー
ダ溶液８０ｍ１中に浸漬し８０℃に加温した。そして、
塩素ガスを吹込んであらかじめ還元した酸化ルテニウム
を酸化揮発させ塩酸溶液で吸収させ塩化ルテニウム酸と
した。この溶液を濃縮乾固したところ褐色の塩化ルテニ
ウムの結晶０．５ｇを得た。銅接点台材にはルテニウム
が検出できなかった。[Example 3] Approximately 2 μm on the surface of m1442φ crane glue bed type electrical steel contact
How many 100 pieces are coated with m ruthenium oxide?
After reduction treatment for 10 minutes in a hydrogen atmosphere at 00°C, it was immersed in 80ml of caustic soda solution and heated to 80°C. and,
Ruthenium oxide, which had been reduced in advance by blowing in chlorine gas, was oxidized and volatilized and absorbed with a hydrochloric acid solution to produce ruthenium chloride. When this solution was concentrated to dryness, 0.5 g of brown ruthenium chloride crystals were obtained. Ruthenium was not detected in the copper contact base material.
以上詳述したように、本発明によるルテニウムの回収方
法によれば、基体表面上の酸化ルテニウムを金属ルテニ
ウムに還元することにより基体を溶解することなくルテ
ニウムが回収できるため、工程が短縮化されると同時に
経済的で、しかも＾品質のものがえられるという優れた
効果がある。As detailed above, according to the ruthenium recovery method according to the present invention, ruthenium can be recovered without dissolving the substrate by reducing ruthenium oxide on the surface of the substrate to metal ruthenium, thereby shortening the process. At the same time, it is economical and has the excellent effect of producing quality products.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
る混晶体を被覆した耐食性基体からルテニウムを回収す
る方法において、当該ルテニウム酸化物又は実質的にル
テニウム酸化物からなる混晶体を還元して金属ルテニウ
ムとした後、塩素ガス又は酸化性の塩素化合物を含むア
ルカリ溶液中でその金属ルテニウムをルチン酸アルカリ
（ＭｔＲｕ０４又はＭ”ＲｕＯ，＋ただし、Ｍ＋は１
価のアルカリ金属、Ｍ７＋は２価のアルカリ金属をいう
。 として耐食性基体から溶離させることを特徴とするルテ
ニウムの回収方法。[Claims] A method for recovering ruthenium from a corrosion-resistant substrate coated with ruthenium oxide or a mixed crystal consisting essentially of ruthenium oxide, wherein the ruthenium oxide or the mixed crystal consisting essentially of ruthenium oxide is reduced. After that, the metal ruthenium is converted into alkali rutate (MtRu04 or M”RuO, + where M+ is 1) in an alkaline solution containing chlorine gas or an oxidizing chlorine compound.
A valent alkali metal, M7+, refers to a divalent alkali metal. A method for recovering ruthenium, the method comprising eluting ruthenium from a corrosion-resistant substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7565382A JPS58194745A (en) | 1982-05-06 | 1982-05-06 | Recovery of ruthenium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7565382A JPS58194745A (en) | 1982-05-06 | 1982-05-06 | Recovery of ruthenium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58194745A true JPS58194745A (en) | 1983-11-12 |
| JPH0321490B2 JPH0321490B2 (en) | 1991-03-22 |
Family
ID=13582413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7565382A Granted JPS58194745A (en) | 1982-05-06 | 1982-05-06 | Recovery of ruthenium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58194745A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS616129A (en) * | 1984-06-21 | 1986-01-11 | Tanaka Kikinzoku Kogyo Kk | Manufacture of soluble salt |
| JPS63243232A (en) * | 1987-03-31 | 1988-10-11 | Ishikawajima Harima Heavy Ind Co Ltd | Method for recovering ruthenium from radioactive waste |
| DE19928029A1 (en) * | 1999-06-18 | 2000-12-21 | Heraeus Gmbh W C | Process for dissolving precious metals from scrap materials containing precious metals |
| JP2002206122A (en) * | 2000-11-06 | 2002-07-26 | Dowa Mining Co Ltd | Method for recovering ruthenium metal |
| WO2007064027A1 (en) | 2005-11-30 | 2007-06-07 | Sumitomo Chemical Company, Limited | Method for production of supported ruthenium and method for production of chlorine |
| WO2007074129A1 (en) * | 2005-12-23 | 2007-07-05 | Basf Se | Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts |
| WO2008062785A1 (en) * | 2006-11-21 | 2008-05-29 | Furuya Metal Co., Ltd. | Method for recovering ruthenium |
| WO2008099747A1 (en) * | 2007-02-16 | 2008-08-21 | Tanaka Kikinzoku Kogyo K.K. | Method for recovering platinum group metal from waste |
| EP2157198A1 (en) | 2008-08-22 | 2010-02-24 | Bayer MaterialScience AG | Method for generating metallic ruthenium or ruthenium compounds from solids containing ruthenium |
| WO2010076297A2 (en) | 2008-12-30 | 2010-07-08 | Basf Se | Method for recovering ruthenium from spent catalysts containing ruthenium oxide |
| US8097089B2 (en) | 2007-12-19 | 2012-01-17 | Quantum Global Technologies LLC | Methods for cleaning process kits and chambers, and for ruthenium recovery |
| JP2012213733A (en) * | 2011-04-01 | 2012-11-08 | Sumitomo Chemical Co Ltd | Method of manufacturing supported ruthenium and method of manufacturing chlorine |
| CN109574097A (en) * | 2019-02-01 | 2019-04-05 | 江苏欣诺科催化剂有限公司 | The preparation method of six ammino ruthenium of trichlorine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56114835A (en) * | 1980-02-15 | 1981-09-09 | Toyota Motor Corp | Recovery of platinum metals from platinum catalyst |
| JPS56160331A (en) * | 1980-05-12 | 1981-12-10 | Toyota Motor Corp | Recovering method for platinum group metal from used catalyst |
-
1982
- 1982-05-06 JP JP7565382A patent/JPS58194745A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56114835A (en) * | 1980-02-15 | 1981-09-09 | Toyota Motor Corp | Recovery of platinum metals from platinum catalyst |
| JPS56160331A (en) * | 1980-05-12 | 1981-12-10 | Toyota Motor Corp | Recovering method for platinum group metal from used catalyst |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS616129A (en) * | 1984-06-21 | 1986-01-11 | Tanaka Kikinzoku Kogyo Kk | Manufacture of soluble salt |
| JPS63243232A (en) * | 1987-03-31 | 1988-10-11 | Ishikawajima Harima Heavy Ind Co Ltd | Method for recovering ruthenium from radioactive waste |
| US6440376B1 (en) | 1999-06-18 | 2002-08-27 | W. C. Heraeus Gmbh & Co. Kg. | Method for dissolving noble metals out of segregated ores containing noble metals |
| DE19928029A1 (en) * | 1999-06-18 | 2000-12-21 | Heraeus Gmbh W C | Process for dissolving precious metals from scrap materials containing precious metals |
| JP2002206122A (en) * | 2000-11-06 | 2002-07-26 | Dowa Mining Co Ltd | Method for recovering ruthenium metal |
| WO2007064027A1 (en) | 2005-11-30 | 2007-06-07 | Sumitomo Chemical Company, Limited | Method for production of supported ruthenium and method for production of chlorine |
| WO2007074129A1 (en) * | 2005-12-23 | 2007-07-05 | Basf Se | Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts |
| KR101379160B1 (en) * | 2005-12-23 | 2014-03-28 | 바스프 에스이 | Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts |
| US7704469B2 (en) | 2005-12-23 | 2010-04-27 | Basf Aktiengesellschaft | Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts |
| WO2008062785A1 (en) * | 2006-11-21 | 2008-05-29 | Furuya Metal Co., Ltd. | Method for recovering ruthenium |
| JP2008127629A (en) * | 2006-11-21 | 2008-06-05 | Furuya Kinzoku:Kk | Method for recovering ruthenium |
| DE112007002803T5 (en) | 2006-11-21 | 2009-10-01 | Furuya Metal Co., Ltd. | Process for the recovery of ruthenium |
| US8454914B2 (en) | 2006-11-21 | 2013-06-04 | Furuya Metal Co., Ltd. | Method for recovering ruthenium |
| WO2008099747A1 (en) * | 2007-02-16 | 2008-08-21 | Tanaka Kikinzoku Kogyo K.K. | Method for recovering platinum group metal from waste |
| JP2008202063A (en) * | 2007-02-16 | 2008-09-04 | Tanaka Kikinzoku Kogyo Kk | Method for recovering platinum group metal from waste |
| US8097089B2 (en) | 2007-12-19 | 2012-01-17 | Quantum Global Technologies LLC | Methods for cleaning process kits and chambers, and for ruthenium recovery |
| EP2157198A1 (en) | 2008-08-22 | 2010-02-24 | Bayer MaterialScience AG | Method for generating metallic ruthenium or ruthenium compounds from solids containing ruthenium |
| DE102008039278A1 (en) | 2008-08-22 | 2010-02-25 | Bayer Materialscience Ag | Process for recovering metallic ruthenium or ruthenium compounds from ruthenium-containing solids |
| JP2012513893A (en) * | 2008-12-30 | 2012-06-21 | ビーエーエスエフ ソシエタス・ヨーロピア | Method for recovering ruthenium from spent ruthenium oxide containing catalysts |
| US8252253B2 (en) | 2008-12-30 | 2012-08-28 | Basf Se | Process for recovering ruthenium from used ruthenium oxide-comprising catalysts |
| WO2010076297A2 (en) | 2008-12-30 | 2010-07-08 | Basf Se | Method for recovering ruthenium from spent catalysts containing ruthenium oxide |
| JP2012213733A (en) * | 2011-04-01 | 2012-11-08 | Sumitomo Chemical Co Ltd | Method of manufacturing supported ruthenium and method of manufacturing chlorine |
| CN109574097A (en) * | 2019-02-01 | 2019-04-05 | 江苏欣诺科催化剂有限公司 | The preparation method of six ammino ruthenium of trichlorine |
| CN109574097B (en) * | 2019-02-01 | 2021-11-16 | 江苏欣诺科催化剂有限公司 | Preparation method of trichloro-hexa-amino ruthenium |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0321490B2 (en) | 1991-03-22 |
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