JPH01234531A - Method of recovering platinum group metal - Google Patents
Method of recovering platinum group metalInfo
- Publication number
- JPH01234531A JPH01234531A JP6268688A JP6268688A JPH01234531A JP H01234531 A JPH01234531 A JP H01234531A JP 6268688 A JP6268688 A JP 6268688A JP 6268688 A JP6268688 A JP 6268688A JP H01234531 A JPH01234531 A JP H01234531A
- Authority
- JP
- Japan
- Prior art keywords
- platinum group
- group metal
- chloride
- recovered
- group metals
- 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.)
- Pending
Links
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 28
- 239000002184 metal Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 14
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 11
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 11
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- -1 platinum group metals Chemical class 0.000 claims description 23
- 239000010953 base metal Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 6
- 150000001805 chlorine compounds Chemical class 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims 2
- 238000010494 dissociation reaction Methods 0.000 claims 1
- 230000005593 dissociations Effects 0.000 claims 1
- 239000002516 radical scavenger Substances 0.000 claims 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 5
- 235000019270 ammonium chloride Nutrition 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 229910052878 cordierite Inorganic materials 0.000 description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910001510 metal chloride Inorganic materials 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明の方法は、反応部分において白金族金属の塩化反
応を行い揮発してくる白金族金属塩化物をアンモニウム
塩の錯塩形成剤で捕集回収することによる白金族金属の
回収方法に係るものである。Detailed Description of the Invention (Industrial Application Field) The method of the present invention involves carrying out a chlorination reaction of a platinum group metal in a reaction part and collecting the volatilized platinum group metal chloride using an ammonium salt complex forming agent. This invention relates to a method for recovering platinum group metals by recovery.
(従来技術とその問題点)
酸化チタン、酸化コバルト、アルミナ、シリカ、ジルコ
ニア、マグネシア、ムライト、コージェライト等の金属
酸化物基体上に、Pt、Pd、Rh、Ir、Ru等の白
金族金属を担持した触媒や白金族金属を基体金属酸化物
上に被覆したものが、化学工業、電子工業等で大量に使
用されている。(Prior art and its problems) Platinum group metals such as Pt, Pd, Rh, Ir, and Ru are deposited on metal oxide substrates such as titanium oxide, cobalt oxide, alumina, silica, zirconia, magnesia, mullite, and cordierite. Supported catalysts or platinum group metals coated on base metal oxides are used in large quantities in the chemical industry, electronic industry, etc.
このような触媒は、使用中に白金族金属の活性が低下し
、一定の性能が維持できなくなった際には新しい触媒に
取り替える必要がある。In such a catalyst, when the activity of the platinum group metal decreases during use and a certain level of performance cannot be maintained, it is necessary to replace it with a new catalyst.
また、電子材料についても装置ならびに部品の寿命にな
ると取り替えられる。Furthermore, electronic materials are also replaced when devices and parts reach the end of their service life.
こうした使用済の材料中には尚相当量の高価な白金族金
属が残存し、これを回収し有効利用することは工業上重
要である。A considerable amount of expensive platinum group metals still remain in these used materials, and it is industrially important to recover and utilize them effectively.
従来の方法としては、硫酸、王水等の溶解法があるが、
これらの方法は溶解工程に長時間の処理を要する。Conventional methods include dissolution using sulfuric acid, aqua regia, etc.
These methods require a long dissolution process.
また基体金属酸化物と白金族金属を分離する際、基体金
属酸化物が析出するこよや、洗浄に大量の水を必要とす
る等の問題があった。Further, when separating the base metal oxide from the platinum group metal, there were problems such as the base metal oxide precipitating out and the need for a large amount of water for cleaning.
また塩化揮発法においても白金族塩化物の捕集法として
活性炭吸着捕集や、スクラバによる洗浄捕集等があるが
、活性炭吸着は温度を下げて捕集する必要があるばかり
でなく、捕集後の処理が面倒であるという問題。In addition, in the chloride volatilization method, there are activated carbon adsorption collection and cleaning collection using a scrubber as methods for collecting platinum group chlorides, but activated carbon adsorption not only requires lowering the temperature but also The problem is that the subsequent processing is troublesome.
スクラバ洗浄法は乾式法で生成される無水白金族塩化物
は、そのほとんどが酸またはアルカリに対して難溶であ
るため、大量の洗浄液を濾過しなければならないことや
、洗浄液中に溶は出した少々の白金族塩化物を回収しな
ければならない等の問題に加え、塩素ガスを再利用する
ためには乾燥工程を設ける等の必要があった。In the scrubber cleaning method, most of the anhydrous platinum group chlorides produced by the dry method are poorly soluble in acids or alkalis, so a large amount of cleaning solution must be filtered, and the solution does not come out in the cleaning solution. In addition to problems such as the need to recover a small amount of platinum group chlorides, it was also necessary to provide a drying process in order to reuse the chlorine gas.
(発明の目的)
本発明は、如上の事情に鑑みなされたもので、その目的
は、基体金属酸化物に白金族金属を保持せしめた材料よ
り、白金族金属を簡便かつ効率良く回収する方法を提供
することにある。(Object of the Invention) The present invention has been made in view of the above circumstances, and its purpose is to provide a method for simply and efficiently recovering platinum group metals from a material in which platinum group metals are retained in a base metal oxide. It is about providing.
(発明の構成)
本発明は、白金族金属を回収する方法において、白金族
金属と基体金属酸化物を含む回収物を加熱しながら塩素
を流すことにより白金族金属を塩化物にして揮発させる
。(Structure of the Invention) The present invention is a method for recovering platinum group metals, in which the platinum group metals are converted into chlorides and volatilized by flowing chlorine while heating a recovered material containing platinum group metals and base metal oxides.
一般的に使用される基体金属酸化物は塩化反応を起こし
にくく白金族金属塩化物と共に移動しない。Commonly used base metal oxides do not undergo chlorination reactions and do not migrate together with platinum group metal chlorides.
反応部の温度は300℃以上が好ましい。The temperature of the reaction section is preferably 300°C or higher.
これは、この温度以下になると白金族塩化物の揮発が良
好に行えなくなる為である。This is because platinum group chlorides cannot be volatilized well below this temperature.
また、1200℃よりも高い温度では、白金族塩化物が
白金族金属と塩素とに解離してしまい揮発効率が大きく
低下する。Further, at a temperature higher than 1200° C., platinum group chloride dissociates into platinum group metal and chlorine, resulting in a significant decrease in volatilization efficiency.
揮発してくる白金族塩化物は、アンモニウム塩の錯塩形
成剤によって捕集される。The volatilized platinum group chloride is collected by an ammonium salt complex forming agent.
アンモニウム塩の捕集剤を用いる理由は、アンモニウム
塩は、白金族塩化物と錯塩を形成することにより白金族
塩化物の捕集効率は他のものと比べて飛躍的に良いもの
となる。The reason why an ammonium salt collector is used is that ammonium salt forms a complex salt with platinum group chlorides, so that the collection efficiency of platinum group chlorides is dramatically better than that of other agents.
なおアンモニウム塩の錯塩形成剤の代表的なものは以下
の通りである。Note that typical ammonium salt complex forming agents are as follows.
塩化アンモニウム (Ni1. ) 昇華点33
8℃硫酸アンモニウムC(NH4) 2SO−3融 点
357℃(実施例I)
触媒用ペレット (δ−アルミナ)に白金(Pt)(1
wt%)を担持した材料500gを図に示す如くこの回
収物1を塩化物化容器4中に入れ電気炉2により塩化物
化容器4を900℃に加熱し、塩素ガスを塩素ガス導入
管3から3A/min流すことにより白金を塩化物にし
て揮発させ、それをアンモニウム塩の捕集剤層5に装填
した塩化アンモニウム(NH,Cj?)により捕捉した
。Ammonium chloride (Ni1.) Sublimation point 33
8℃ Ammonium sulfate C (NH4) 2SO-3 Melting point 357℃ (Example I) Platinum (Pt) (1
As shown in the figure, the recovered material 1 was placed in a chloride container 4, and the chloride container 4 was heated to 900°C using an electric furnace 2, and chlorine gas was introduced from the chlorine gas introduction pipe 3 to 3A. /min to volatilize platinum into chloride, which was captured by ammonium chloride (NH, Cj?) loaded in the ammonium salt collector layer 5.
これを6時間続けた後、塩化アンモニウムを取り出し、
水で溶解し残渣を回収する方法で白金を回収したところ
回収率は92%であった。After continuing this for 6 hours, remove the ammonium chloride and
When platinum was recovered by dissolving it in water and recovering the residue, the recovery rate was 92%.
(実施例2)
触媒用ハニカム(コージェライト)にパラジウム(Pd
)(1wt%)を担持した材料500 gを図に示す如
くこの回収物1を塩化物化容器4中に入れ電気炉2によ
り塩化物化容器4を1000℃に加熱し、塩素ガスを塩
素ガス導入管3から3j?/min流すことによりパラ
ジウムを塩化物にして揮発させ、それをアンモニウム塩
の錯塩形成剤層5に装填した硫酸アンモニウム[(NH
4)2 So、)1mより捕捉した。(Example 2) Palladium (Pd) was added to the catalyst honeycomb (cordierite).
) (1 wt%) was put into the chloride container 4 as shown in the figure, and the chloride container 4 was heated to 1000°C using the electric furnace 2, and the chlorine gas was introduced into the chlorine gas introduction pipe. 3 to 3j? /min, palladium is converted into chloride and volatilized, and this is converted into ammonium sulfate [(NH
4)2So,) Captured from 1m.
これを4時間続けた後、硫酸アンモニウムを取り出し、
水で溶解し水素化ホウ素ナトリウムで還元し回収したと
ころ回収率は93%であった。After continuing this for 4 hours, remove the ammonium sulfate and
When it was recovered by dissolving it in water and reducing it with sodium borohydride, the recovery rate was 93%.
(従来例↑)
触媒用ペレット (δ−アルミナ)に白金(Pt)(1
wt%)を担持した材料500gを実施例同様の操作で
白金塩化物を揮発させスクラバで水洗して白金塩化物を
捕捉した。(Conventional example ↑) Platinum (Pt) (1
The platinum chloride was volatilized from 500 g of the material carrying 500 g of the material (wt%) in the same manner as in the example, and the platinum chloride was captured by washing with water using a scrubber.
これを6時間続けた後、洗浄水を全て取り出し、pH調
整後塩化アンモニウム(NH,(1)で白金を沈澱させ
る方法で白金を回収したところ回収率は87%であった
。After this continued for 6 hours, all of the washing water was taken out, and platinum was recovered by a method of precipitating platinum with ammonium chloride (NH, (1)) after adjusting the pH, and the recovery rate was 87%.
この際、pH調製や沈澱工程、スクラバに入る手前の洗
浄液で冷やされた部分の壁に白金塩化物が付着し回収に
多大な労力を要した。At this time, platinum chloride adhered to the walls of the parts cooled by the cleaning solution during the pH adjustment and precipitation steps and before entering the scrubber, requiring a great deal of effort to recover.
(従来例2)
触媒用ハニカム(コージェライト)にパラジウム(Pd
)(1wt%)を担持した材料500gを王水中で浸出
し、濾過によりパラジウム王水液を取り出しpH調整後
水素化ホウ素ナトリウムで還元する方法で行ったところ
回収率は92%であった。(Conventional example 2) Palladium (Pd) is added to the catalyst honeycomb (cordierite).
) (1 wt%) was leached in aqua regia, the palladium aqua regia solution was taken out by filtration, the pH was adjusted, and then reduced with sodium borohydride. The recovery rate was 92%.
しかし回収率を高くするために濾過の際の洗浄等で液量
が大幅に増える等の問題がある。However, in order to increase the recovery rate, there is a problem that the amount of liquid increases significantly due to washing during filtration.
(発明の効果)
以上詳述のように本発明によれば、従来に比し効率良く
白金族金属を基体金属酸化物から分離回収することがで
き、しかも従来のように多大な労力を必要としない為、
経済的にしかも短時間で回収することができるという効
果がある。(Effects of the Invention) As detailed above, according to the present invention, platinum group metals can be separated and recovered from base metal oxides more efficiently than before, and without requiring a great deal of labor as in the past. In order not to
It has the effect of being economical and can be recovered in a short time.
図は本発明の回収方法を示す概略図である。 出願人 田中貴金属工業株式会社 tK素カ・ス導入菅 道化物化容へ 回収物 ・組気欠戸 The figure is a schematic diagram showing the recovery method of the present invention. Applicant: Tanaka Kikinzoku Kogyo Co., Ltd. tK elementary school introduction tube To the clown monster recovered items ・Kumikichido
Claims (1)
しながら塩素ガスを流すことにより白金族金属を塩化物
にして揮発分離し、アンモニウム塩の捕集剤により捕集
回収することを特徴とする白金族金属を回収する方法。 2、加熱温度が白金族塩化物の解離又は分解温度以上で
あることを特徴とする請求項1記載の白金族金属を回収
する方法。 3、加熱温度が300〜1200℃であることを特徴と
する請求項1又は2に記載の白金族金属を回収する方法
。 4、白金族塩化物を捕集するための捕集剤の温度が、そ
の捕集剤の融点又は分解温度以下であることを特徴とす
る請求項1乃至3に記載の白金族金属を回収する方法。[Claims] 1. The collected material containing platinum group metals and base metal oxides is vaporized and separated by converting the platinum group metals into chlorides by flowing chlorine gas while heating them, and then using an ammonium salt scavenger. A method for recovering platinum group metals, characterized by collecting and recovering them. 2. The method for recovering platinum group metals according to claim 1, wherein the heating temperature is higher than the dissociation or decomposition temperature of the platinum group chloride. 3. The method for recovering platinum group metals according to claim 1 or 2, wherein the heating temperature is 300 to 1200°C. 4. Recovering platinum group metals according to claims 1 to 3, wherein the temperature of the collecting agent for collecting platinum group chlorides is below the melting point or decomposition temperature of the collecting agent. Method.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6268688A JPH01234531A (en) | 1988-03-16 | 1988-03-16 | Method of recovering platinum group metal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6268688A JPH01234531A (en) | 1988-03-16 | 1988-03-16 | Method of recovering platinum group metal |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH01234531A true JPH01234531A (en) | 1989-09-19 |
Family
ID=13207414
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP6268688A Pending JPH01234531A (en) | 1988-03-16 | 1988-03-16 | Method of recovering platinum group metal |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH01234531A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001073043A (en) * | 1999-07-27 | 2001-03-21 | Anglo American Platinum Corp Ltd | Improvement in refining |
WO2005007903A1 (en) * | 2003-07-22 | 2005-01-27 | Ressources Minieres Pro-Or Inc. | A process for recovering platinum group metals from ores and concentrates |
-
1988
- 1988-03-16 JP JP6268688A patent/JPH01234531A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001073043A (en) * | 1999-07-27 | 2001-03-21 | Anglo American Platinum Corp Ltd | Improvement in refining |
WO2005007903A1 (en) * | 2003-07-22 | 2005-01-27 | Ressources Minieres Pro-Or Inc. | A process for recovering platinum group metals from ores and concentrates |
US7972412B2 (en) | 2003-07-22 | 2011-07-05 | Ressources Minieres Pro-Or Inc. | Process for recovering platinum group metals from ores and concentrates |
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