JPH02301527A - Method for recovering platinum family metal - Google Patents
Method for recovering platinum family metalInfo
- Publication number
- JPH02301527A JPH02301527A JP12338989A JP12338989A JPH02301527A JP H02301527 A JPH02301527 A JP H02301527A JP 12338989 A JP12338989 A JP 12338989A JP 12338989 A JP12338989 A JP 12338989A JP H02301527 A JPH02301527 A JP H02301527A
- Authority
- JP
- Japan
- Prior art keywords
- platinum group
- metal
- family metal
- recovered
- chloride
- 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
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 27
- 239000002184 metal Substances 0.000 title claims abstract description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims description 23
- 238000000034 method Methods 0.000 title claims description 18
- 229910052697 platinum Inorganic materials 0.000 title description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 14
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- -1 platinum group metals Chemical class 0.000 claims description 13
- 239000010953 base metal Substances 0.000 claims description 12
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 abstract description 18
- 238000011084 recovery Methods 0.000 abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 7
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 abstract description 5
- 229910001634 calcium fluoride Inorganic materials 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 150000001805 chlorine compounds Chemical class 0.000 abstract 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 abstract 2
- 230000008016 vaporization Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- 229910052703 rhodium Inorganic materials 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000758 substrate Substances 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)
本発明は、白金族金属および/又はその酸化物と基体金
属酸化物を含む回収物にCa F 2又はNaFを混合
し加熱しながら塩素ガスを流すことにより、白金族金属
および/又はその酸化物の塩化反応を行い、基体金属酸
化物より、揮発分離することによる白金族の回収方法に
係る。Detailed Description of the Invention (Industrial Application Field) The present invention involves mixing CaF2 or NaF into a recovered material containing a platinum group metal and/or its oxide and a base metal oxide, and heating the mixture with chlorine gas. The present invention relates to a method for recovering platinum group metals by carrying out a chlorination reaction of platinum group metals and/or their oxides by flowing , and separating the platinum group metals by volatilization from the base metal oxide.
(従来技術とその問題点)
従来よりアルミナ、シリカ、シルコニ子等の金属酸化物
基体上に白金族金属および/又はその酸化物を担持した
触媒が、自動車排ガスの浄化、電解電極、石油化学工業
用等に大量に使用されている。(Prior art and its problems) Catalysts in which platinum group metals and/or their oxides are supported on metal oxide substrates such as alumina, silica, and silconium have been used in the purification of automobile exhaust gas, electrolytic electrodes, and petrochemical industries. It is used in large quantities for various purposes.
このような触媒は、使用中に白金族の活性が低下し、一
定の性能を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。When the activity of the platinum group metal in such a catalyst decreases during use and a certain level of performance cannot be maintained, it is necessary to replace it with a new catalyst.
こうした使用済の材料中には、なお相当量の高価な白金
族が残存し、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、白金族の回収方法としては、酸、王水などの溶解
法があるが、これらの方法は、溶解工程において長時間
の多段湿式処理を要する。Conventionally, methods for recovering platinum group metals include dissolution methods using acids, aqua regia, etc., but these methods require a long multi-stage wet treatment in the dissolution step.
また基体金属酸化物の洗浄の為に大量の水を必要とし、
さらに白金族と基体金属を分離する際、基体金属水酸化
物が析出するなどの問題があり甚だ回収効率が悪く、工
業的には不適な回収方法であった。Also, a large amount of water is required for cleaning the base metal oxide.
Furthermore, when separating the platinum group metal from the base metal, there are problems such as precipitation of base metal hydroxide, resulting in extremely low recovery efficiency, making the recovery method unsuitable for industrial use.
(発明の目的)
本発明は、上記の問題点を解決すべくなされたものであ
り、その目的は、基体金属酸化物に白金族金属および/
又はその酸化物を保持せしめた材料より白金族を簡便且
つ効率良く回収する方法を提供せんとするものである。(Object of the invention) The present invention has been made to solve the above problems, and its object is to provide a base metal oxide with a platinum group metal and/or
Another object of the present invention is to provide a method for simply and efficiently recovering platinum group metals from a material that retains their oxides.
(問題を解決するための手段)
上記問題を解決するための本発明の白金族の回収方法は
、白金族金Rおよび/又はその酸化物と基体金属酸化物
を含む回収物にCa F 2又はNaFを混合し、加熱
しながら塩素ガスを流すことにより、白金族金属および
/又はその酸化物を塩化物にして揮発分離することを特
徴とするものである。(Means for Solving the Problems) In order to solve the above-mentioned problems, the method for recovering platinum group metals of the present invention includes adding Ca F 2 or The method is characterized in that by mixing NaF and flowing chlorine gas while heating, the platinum group metal and/or its oxide is converted into chloride and separated by volatilization.
基体金属酸化物に白金族金Rおよび/又はその酸化物を
保持させる方法としては、基体金属酸化物自体が触媒と
して充分な単位表面積を有しているr−フルミナなどの
場合は、直接その部分に保持し、基体金属酸化物自体が
充分な単位表面積を有していない場合は、この表面にγ
−アルミナなどの触媒活性層を設け、そこに保持する方
法が採られている。As a method for retaining platinum group gold R and/or its oxide in the base metal oxide, in the case of r-Flumina where the base metal oxide itself has a sufficient unit surface area as a catalyst, it is possible to directly hold the platinum group gold R and/or its oxide. If the base metal oxide itself does not have a sufficient unit surface area, γ
- A method is adopted in which a catalytically active layer such as alumina is provided and the catalyst is held there.
本発明の方法による回収操作を行った場合、白金族を保
持しであるT−アルミナの触媒活性層も白金族の揮発に
伴い徐々に反応して行く。When the recovery operation according to the method of the present invention is performed, the catalytically active layer of T-alumina that holds the platinum group also gradually reacts as the platinum group volatilizes.
Ca F 2又はNaFを混合すると、T−アルミナ触
媒活性層および白金族の揮発が促進されるが、その作用
は明らかではないが、一種の触媒作用によるものと考え
られる。When CaF2 or NaF is mixed, the volatilization of the T-alumina catalyst active layer and the platinum group is promoted, but the effect is not clear, but it is thought to be due to a type of catalytic effect.
白金族を保持している触媒活性層をも徐々に反応させて
行くことが、白金族を効率良く揮発させる一因となって
いるものと考えられる。Gradually reacting the catalyst active layer holding the platinum group is considered to be a factor in efficiently volatilizing the platinum group.
触媒活性層の反応はT−アルミナの塩化反応により塩化
アルミニウムを生ずる反応で次の様に表せる。The reaction in the catalytic active layer is a reaction in which aluminum chloride is produced by the chlorination reaction of T-alumina, and can be expressed as follows.
Afz O+(r)+3(12
CaF2、NaF(触媒)
AIICfl、+ 3/202
この反応により生成した塩化アルミニウムは、182、
7℃に昇華点を持つものであり白金族塩化物との分離は
容易に行なえる。Afz O+(r)+3(12 CaF2, NaF (catalyst) AIICfl, + 3/202 The aluminum chloride produced by this reaction is 182,
It has a sublimation point of 7°C and can be easily separated from platinum group chlorides.
CaF、又はNaFの添加量は、0.5%〜10%の範
囲で行うことが望ましい。The amount of CaF or NaF added is preferably in the range of 0.5% to 10%.
0.5%より低い値では、添加の効果が見られず添加し
ないものと同様の反応を示す。At a value lower than 0.5%, no effect of addition is observed and the reaction is similar to that without addition.
また10%以上添加した場合は、逆に反応の阻害を生じ
添加の効果が薄れてくるためである。On the other hand, if it is added in an amount of 10% or more, the reaction will be inhibited and the effect of the addition will be weakened.
(実施例) 本発明の白金族回収方法の実施例と従来例を説明する。(Example) Examples and conventional examples of the platinum group recovery method of the present invention will be described.
先ず本発明の白金族回収方法の実施例について説明する
。First, an example of the platinum group recovery method of the present invention will be described.
(1)コーディエライトのハニカム担体に触媒活性層を
この担体に対して9゜ht%保持したものに、PtO,
059%、Pd0.052%、Rh0.028%を担持
した自動車排ガス浄化用触媒を粉砕しフルイを使って7
10μm〜420μm、 420μm〜210μm1
210μm〜90μmの3種類に分級した。各々の割合
は、44.3%、23.1%、301%で、90μm以
下のものが2.4%であった。(1) PtO,
A catalyst for automobile exhaust gas purification carrying Pd 0.059%, Pd 0.052%, and Rh 0.028% was crushed and purified using a sieve.
10μm~420μm, 420μm~210μm1
It was classified into three types, 210 μm to 90 μm. The respective percentages were 44.3%, 23.1%, and 301%, with 2.4% having a diameter of 90 μm or less.
各粒度の触媒500gにCaF、を5%混合し図に示す
ごとく反応管(内管)2に塩素ガス加熱用のシリカサン
ド5を充填し、その上方に、塩素ガス分散を目的とした
多孔質セラミック4とセラミックフィルター3をセット
した反応器にこの回収物1を入れた。500g of catalyst of each particle size is mixed with 5% CaF, and as shown in the figure, the reaction tube (inner tube) 2 is filled with silica sand 5 for heating chlorine gas, and above it is a porous material for the purpose of dispersing chlorine gas. This recovered material 1 was put into a reactor in which a ceramic 4 and a ceramic filter 3 were set.
その後、反応管(外管) 10に装填した。Thereafter, it was loaded into a reaction tube (outer tube) 10.
反応管(外管)10は上部に捕集剤層を有しておりここ
にB a Cl 2を充填した。The reaction tube (outer tube) 10 had a scavenger layer at the top, and was filled with B a Cl 2 .
電気炉(A)7により1000℃に加熱しながら、塩素
ガス吹込管6より塩素ガスを流し、流動床で塩化反応を
行わせた。While heating to 1000° C. in an electric furnace (A) 7, chlorine gas was flowed through a chlorine gas blowing pipe 6 to carry out a chlorination reaction in a fluidized bed.
各粒径の触媒の流動反応の塩素流量は、710μm 〜
420μm、 8 f/min、420μm〜210%
m。The flow rate of chlorine in the flow reaction of catalysts of each particle size is 710 μm ~
420μm, 8 f/min, 420μm~210%
m.
4 f/min 、 210%m〜90μm、 11
!7 minで行った。4 f/min, 210% m to 90 μm, 11
! It took 7 minutes.
反応ガスは、電気炉(B)8により830℃に加熱され
た捕集剤9に充填したB a Cl 2層を通し、白金
族塩化物の捕集を行った。The reaction gas was passed through two layers of B a Cl filled in a collector 9 heated to 830° C. in an electric furnace (B) 8 to collect platinum group chlorides.
この反応を3時間行った後、捕集剤層9に充填したB
a CIt 2を取り出し水で溶かし、S’BHで還元
し回収したところ、P、t、Pd、Rhの回収率は下記
の表−1の通りであった。After carrying out this reaction for 3 hours, the B
a CIt 2 was taken out, dissolved in water, and reduced and recovered with S'BH. The recovery rates of P, t, Pd, and Rh were as shown in Table 1 below.
表−1
(2)触媒用T−アルミナペレット(平均粒径2mm)
にRuを1.91%担持したガス改質触媒を粉砕しフル
イを使い710μm〜210μmのものを集めた。Table-1 (2) T-alumina pellets for catalyst (average particle size 2mm)
A gas reforming catalyst carrying 1.91% Ru was crushed and collected with a size of 710 μm to 210 μm using a sieve.
この分級物400gにN a F 10%を添加し、実
施例(1)と同様にこの回収物1をセットした。10% of NaF was added to 400 g of this classified material, and this recovered material 1 was set in the same manner as in Example (1).
捕集剤層9にはKClを充填した。The collector layer 9 was filled with KCl.
電気炉(A)7により850℃に加熱しながら塩素ガス
吹込管6より塩素ガスを6β/min流して流動反応を
行わせた。While heating to 850° C. with an electric furnace (A) 7, chlorine gas was flowed through the chlorine gas blowing pipe 6 at a rate of 6β/min to perform a fluid reaction.
反応ガスは電気炉(B) 8により730℃に加熱され
だ捕集剤9に充填したKCji層を通し、Ru塩化物の
捕集を行った。The reaction gas was heated to 730° C. in an electric furnace (B) 8 and passed through a KCji layer filled with a collector 9 to collect Ru chloride.
この反応を3時間行った後、捕集剤9に充填した、KC
lを取り出し水で溶かしSBHで還元し回収したところ
、Ruの回収率は、97.4%であった。After carrying out this reaction for 3 hours, the KC
When Ru was taken out, dissolved in water, reduced with SBH, and recovered, the recovery rate of Ru was 97.4%.
(従来例)
(1)コーディエライトのハニカム担体に触媒活性層を
この担体に対して9.8wt%保持したものにPtO,
059%、PdO,052%、Rh0.028%を担持
した自動車排ガス浄化用触媒を粉砕しフルイ分けしたも
の(実施例1と同様のもの)を図に示す如く (実施例
1と同じ装置)に入れ、実施例(1)と同じ条件で3時
間反応させ、Pt、Pd、Rhを回収したところ各々の
回収率は下記の表−2の通りであった。(Conventional Example) (1) PtO,
A catalyst for automobile exhaust gas purification carrying 0.059%, PdO, 0.52%, and Rh 0.028% was crushed and sieved (similar to Example 1) as shown in the figure (using the same apparatus as Example 1). When Pt, Pd, and Rh were recovered by reacting for 3 hours under the same conditions as in Example (1), the recovery rates of each were as shown in Table 2 below.
(以下余白)
表−2
(2)、(1)と同じ触媒を5280.25g塩酸6N
溶液に浸漬し、これを60℃に加熱し、そこに塩素ガス
を吹き込み白金族を溶解したこの反応を4時間行った後
、濾過により塩酸液を取り出し、H2Sで白金族を硫化
物として沈殿させる方法で回収したところPt、Pd、
Rhの回収率はそれぞれ93.1% 94.3% 80
.2%であった。(Left below) Table 2: 5280.25g of the same catalyst as in (2) and (1) in 6N hydrochloric acid.
Immerse it in a solution, heat it to 60°C, blow chlorine gas into it and dissolve the platinum group. After this reaction for 4 hours, remove the hydrochloric acid solution by filtration, and precipitate the platinum group as sulfide with H2S. When recovered using this method, Pt, Pd,
The recovery rate of Rh was 93.1% 94.3% 80
.. It was 2%.
この回収において回収率を高くする為、濾過の際の洗浄
液で液量が大幅に増えるという問題が生じた。In order to increase the recovery rate in this recovery, a problem arose in that the amount of washing liquid used during filtration increased significantly.
(発明の効果)
以上の説明で判るように本発明の方法によれば白金族を
基体金属酸化物から極めて効率良く分離回収することが
でき、また従来のような湿式の濾過、洗浄工程を必要と
しないので簡便に短時間に回収できるという優れた効果
がある。(Effects of the Invention) As can be seen from the above explanation, according to the method of the present invention, platinum group metals can be separated and recovered from the base metal oxide very efficiently, and the conventional wet filtration and washing steps are not required. It has the excellent effect of being able to be easily recovered in a short time because it does not cause any damage.
図は本発明の白金族の回収方法の実施例を示す図である
。The figure shows an example of the platinum group metal recovery method of the present invention.
Claims (1)
化物を含む回収物にCaF_2又はNaFを0.5〜1
0wt%を混合し、600℃〜1200℃に加熱しなが
ら塩素ガスを流し、白金族金属および/又はその酸化物
を塩化物に変えて揮発させ、基体金属酸化物と分離し、
回収することを特徴とする白金族の回収方法。(1) Add 0.5 to 1 of CaF_2 or NaF to the recovered material containing the platinum group metal and/or its oxide and the base metal oxide.
0 wt% is mixed and heated to 600°C to 1200°C while flowing chlorine gas to convert the platinum group metal and/or its oxide into chloride and volatilize it, separating it from the base metal oxide,
1. A method for collecting platinum group metals, the method comprising: recovering platinum group metals;
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP12338989A JPH02301527A (en) | 1989-05-17 | 1989-05-17 | Method for recovering platinum family metal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP12338989A JPH02301527A (en) | 1989-05-17 | 1989-05-17 | Method for recovering platinum family metal |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH02301527A true JPH02301527A (en) | 1990-12-13 |
Family
ID=14859363
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP12338989A Pending JPH02301527A (en) | 1989-05-17 | 1989-05-17 | Method for recovering platinum family metal |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH02301527A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009256744A (en) * | 2008-04-18 | 2009-11-05 | Foundation For The Promotion Of Industrial Science | Method for recovering noble metal |
CN111900425A (en) * | 2020-07-03 | 2020-11-06 | 广东邦普循环科技有限公司 | Method for recycling hydrogen fuel cell of new energy automobile |
-
1989
- 1989-05-17 JP JP12338989A patent/JPH02301527A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009256744A (en) * | 2008-04-18 | 2009-11-05 | Foundation For The Promotion Of Industrial Science | Method for recovering noble metal |
CN111900425A (en) * | 2020-07-03 | 2020-11-06 | 广东邦普循环科技有限公司 | Method for recycling hydrogen fuel cell of new energy automobile |
US11699796B1 (en) | 2020-07-03 | 2023-07-11 | Guangdong Brunp Recycling Technology Co., Ltd. | Method for recycling hydrogen fuel cell of new energy vehicle |
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