JPH03153830A - Solvent extraction method of iridium - Google Patents

Solvent extraction method of iridium

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Publication number
JPH03153830A
JPH03153830A JP29284689A JP29284689A JPH03153830A JP H03153830 A JPH03153830 A JP H03153830A JP 29284689 A JP29284689 A JP 29284689A JP 29284689 A JP29284689 A JP 29284689A JP H03153830 A JPH03153830 A JP H03153830A
Authority
JP
Japan
Prior art keywords
iridium
hydrochloric acid
soln
solvent
oxidizing agent
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
JP29284689A
Other languages
Japanese (ja)
Other versions
JP2805689B2 (en
Inventor
Yamaji Nishimura
西村 山治
Makoto Sano
誠 佐野
Tomoshi Ichiishi
市石 知史
Akihiko Okuda
晃彦 奥田
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.)
Tanaka Kikinzoku Kogyo KK
Original Assignee
Tanaka Kikinzoku Kogyo KK
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 Tanaka Kikinzoku Kogyo KK filed Critical Tanaka Kikinzoku Kogyo KK
Priority to JP1292846A priority Critical patent/JP2805689B2/en
Publication of JPH03153830A publication Critical patent/JPH03153830A/en
Application granted granted Critical
Publication of JP2805689B2 publication Critical patent/JP2805689B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Extraction Or Liquid Replacement (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

PURPOSE:To easily and almost completely extract iridium with a solvent from an iridium-contg. hydrochloric acid soln. by controlling the hydrochloric acid concn. of the hydrochloric acid soln. contg. iridium and adding an oxidizing agent thereto while heating the soln., then extracting the iridium with the org. solvent. CONSTITUTION:The iridium is extracted by using the org. solvent as an extracting reagent. The hydrochloric acid concn. of the above-mentioned iridium- contg. hydrochloric acid soln. is controlled prior to the extraction with the above mentioned org. solvent and while this soln. is kept heated, the oxidizing agent is added to the soln. to oxidize the iridium ions in the soln. from tervalent to quadrivalent. The hydrochloric acid concn. of the above-mentioned iridium- contg. hydrochloric acid soln. is adequately controlled to 0.1 to 5 N hydrochloric acid concn. The above-mentioned oxidation treatment is preferably executed by maintaining the heating temp. at >=50 deg.C and using chlorine water as the oxidizing agent to attain >=0.01% effective chlorine in the soln. The iridium in the soln. is extracted to the org. solvent at about 100% extraction rate in this way.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、イリジウム含有溶液からイリジウムを溶媒抽
出する方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for solvent extraction of iridium from an iridium-containing solution.

(従来技術とその問題点) 従来、イリジウムのように用途の限られた金属について
の抽出分離に関する研究は少ない。
(Prior art and its problems) Until now, there has been little research on the extraction and separation of metals such as iridium, which have limited uses.

イリジウムは塩化物水溶液中でクロロ錯陰イオンあるい
はクロロ−アクアク複合錯体として溶存していることか
ら溶媒抽出法としては塩素水で酸化してTBPで抽出し
、水で逆抽出後塩化アンモニウム溶液でアンミン錯化合
物として分離回収する方法やalamine336と3
10の混合第3級アミン25%と5olvesso15
0とケロシンの混合物75%の抽出剤で塩素ガスを通過
させたイリジウム溶液よりイリジウムを抽出し亜硝酸塩
、ヒドラジン、蓚酸塩等のような還元剤溶液で逆抽出す
る方法がある。
Since iridium is dissolved as a chloro complex anion or a chloro-aqueous complex in an aqueous chloride solution, the solvent extraction method is to oxidize it with chlorine water, extract it with TBP, back-extract it with water, and then use ammonium chloride solution to remove the amine. A method of separating and recovering as a complex compound and alamine 336 and 3
10 mixed tertiary amines 25% and 5olvesso15
There is a method of extracting iridium from an iridium solution through which chlorine gas is passed using an extractant containing a mixture of 0 and kerosene at 75%, and then back-extracting it with a solution of a reducing agent such as nitrite, hydrazine, oxalate, etc.

他にAl1quat336を抽出剤とし適当な有機溶媒
で希釈して抽出する方法も提案されている。
In addition, a method of extraction using Al1quat336 as an extractant and diluting it with a suitable organic solvent has also been proposed.

しかし、それぞれイリジウムの抽出率が低い等の欠点が
あった。
However, each had drawbacks such as a low extraction rate of iridium.

(発明の目的) 本発明は、従来法の欠点を解決するために成されたもの
で、イリジウムを有機溶媒に抽出する際の抽出率を約1
00%とする方法を提供することを目的とする。
(Objective of the Invention) The present invention was made to solve the drawbacks of the conventional method, and the extraction rate when extracting iridium into an organic solvent is reduced to about 1.
00%.

(問題点を解決するための手段) 本発明は、イリジウムを含有する塩酸溶液より抽出剤と
して有機溶媒を用いてイリジウムを抽出する方法に於い
て、イリジウムを有機溶媒で抽出する前に該イリジウム
を含有する塩酸溶液の塩酸濃度を調節し、該溶液を加熱
しながら酸化剤を加えて酸化することを特徴とするイリ
ジウムの溶媒抽出法で、前記イリジウムを含有する塩酸
溶液の塩酸濃度がO,1〜5規定に調節するイリジウム
の溶媒抽出法であり、前記加熱温度が50℃以上で、酸
化剤が塩素水で、溶液中の有効塩素が0.01%以上で
あるイリジウムの溶媒抽出法である。
(Means for Solving the Problems) The present invention provides a method for extracting iridium from a hydrochloric acid solution containing iridium using an organic solvent as an extractant. A solvent extraction method for iridium characterized in that the hydrochloric acid concentration of the hydrochloric acid solution containing iridium is adjusted and the solution is oxidized by adding an oxidizing agent while heating the solution, and the hydrochloric acid concentration of the hydrochloric acid solution containing iridium is O. This is a solvent extraction method for iridium in which the heating temperature is adjusted to 50° C. or higher, the oxidizing agent is chlorine water, and the available chlorine in the solution is 0.01% or more. .

イリジウムを有機溶媒に抽出する前に、該イリジウムを
含有する塩酸溶液の塩酸濃度を0. 1〜5規定に調節
するのは、0. 1規定以下ではイリジウム錯体が安定
性に欠けるためであり、5規定以上ではイリジウムを■
価に酸化しても抽出率が低下するからである。
Before extracting iridium into an organic solvent, the hydrochloric acid concentration of the iridium-containing hydrochloric acid solution is adjusted to 0. Adjustment to 1 to 5 regulations is 0. This is because the iridium complex lacks stability when it is less than 1N, and when it is more than 5N, the iridium is
This is because the extraction rate decreases even if oxidized to oxidation.

また、イリジウムの■価を■価に酸化させる反応温度を
50℃以上に加熱しながら酸化するのは、該イリジウム
が塩酸溶液中で■価に安定させるためで、好ましくは8
0〜95℃である。
In addition, the reason why the reaction temperature for oxidizing iridium to 50° C. or higher is to stabilize the iridium at 50° C. in a hydrochloric acid solution, preferably 8
The temperature is 0 to 95°C.

前記加熱温度が50℃以下では不安定で■価のイリジウ
ムイオンが■価に還元される恐れがあるからで、■価の
イリジウムイオンは極めて有機溶媒に抽出するのに時間
を要するためであり、加熱温度を100℃以下とするの
は酸化剤として加える塩素が揮発して十分に酸化させる
ことができなくなるからと上記の塩酸濃度が不安定とな
るからである。
This is because if the heating temperature is below 50°C, it is unstable and the iridium ions with a valence of 2 may be reduced to the valence of 2, and the iridium ions with a valence of 2 take a very long time to be extracted into an organic solvent. The reason why the heating temperature is set to 100° C. or lower is that the chlorine added as an oxidizing agent volatilizes, making it impossible to oxidize sufficiently and making the above-mentioned hydrochloric acid concentration unstable.

また、酸化剤として塩素水を加えているのは酸化条件を
定め易く、しかも取り扱いが容易であるからで、イリジ
ウムの■価を■価に酸化させるための有効塩素濃度を0
.01%以上としているのは加熱温度、イリジウムの■
価イオンの量等の変化に影響されず、完全に■価に酸化
させることができるからである。
In addition, chlorine water is added as an oxidizing agent because it is easy to set oxidation conditions and easy to handle.
.. 01% or more is the heating temperature, iridium ■
This is because it is not affected by changes in the amount of valence ions, etc., and can be completely oxidized to valence ions.

以下、本発明に係わる実施例を記載するが、該実施例は
本発明を限定するものではない。
Examples related to the present invention will be described below, but the examples are not intended to limit the present invention.

(実施例1) 3価あるいは4価で溶存するlrを塩化物水溶液から抽
出剤として0.  l Kmo l/m’ A I 1
qua t 336の1.2ジクロロエタン希釈液をも
ちいて抽出した場合の結果を第1図に示す。
(Example 1) Trivalent or tetravalent dissolved lr was extracted from an aqueous chloride solution using 0.0. l Kmol l/m' A I 1
The results of extraction using a 1.2 dichloroethane solution of qua t 336 are shown in FIG.

Irの抽出特性は金属の価数により異なり、Ir(IV
)の抽出は広い塩酸濃度範囲で高く、一方Ir(III
)の抽出は比較的低く、塩酸濃度の増加と共に著しく低
下する。
The extraction characteristics of Ir differ depending on the valence of the metal, and Ir(IV
) extraction is high over a wide hydrochloric acid concentration range, while Ir(III
) extraction is relatively low and decreases significantly with increasing hydrochloric acid concentration.

以上の結果から、効率良<Irを抽出するためには、溶
液中のIrをI r (IV)として溶存させることが
重要で、酸化剤として塩素水を用い、塩酸溶液中のIr
(I[)を酸化し、抽出されやすいIr(IV)の錯体
に変化させた。
From the above results, in order to efficiently extract Ir, it is important to dissolve Ir in the solution as Ir (IV), and by using chlorine water as the oxidizing agent, Ir in the hydrochloric acid solution
(I[) was oxidized and converted into a complex of Ir(IV) that is easily extracted.

塩−素水添加後のIrの溶存状態の変化をUVスペクト
ルで観察した。
Changes in the dissolved state of Ir after addition of salt-hydrogen water were observed using UV spectroscopy.

反応温度363K、塩酸濃度3 K m o I / 
m ’の条件で酸化を行い、得られた結果を第3図に示
す。Ir(IV)の錯体に対応する吸光ピーク位置(3
05,420,440,490nm付近)での吸光度の
増大が観察され、Ir(III)が塩素により酸化され
ることがわかる。
Reaction temperature 363K, hydrochloric acid concentration 3K m o I /
The oxidation was carried out under the conditions of m', and the results obtained are shown in FIG. The absorption peak position (3
05, 420, 440, and 490 nm), indicating that Ir(III) is oxidized by chlorine.

塩素水の添加によるIrの溶存状態の変化傾向は塩酸濃
度、反応温度により異なる。
The tendency of the dissolved state of Ir to change due to the addition of chlorine water differs depending on the concentration of hydrochloric acid and the reaction temperature.

次いで、抽出剤濃度を10  ’Kmo l/m’ −
定の下で、金属濃度を変化させてIr(IV)の抽出を
行い、得られた結果を抽出剤と有機相中の抽出された金
属濃度とのモル比として第2図に示す。
Then, the extractant concentration was adjusted to 10'Kmol/m'-
Extraction of Ir(IV) was carried out under constant conditions with varying metal concentrations, and the results obtained are shown in FIG. 2 as the molar ratio of the extractant to the extracted metal concentration in the organic phase.

モル比は金属濃度の増加と共に減少し、その値は2に漸
近する。
The molar ratio decreases with increasing metal concentration and its value asymptotically approaches 2.

この結果は抽出剤濃度範囲10−’から4×lOKmo
l/m3でスロープ解析した結果と一致する。
This result shows that the extractant concentration ranges from 10-' to 4 x l OKmo.
This agrees with the results of slope analysis in l/m3.

(実施例2) イリジウム100mg/fを含む塩酸溶液の塩酸濃度を
2規定に調節したのち、塩素水を加えて有効塩素濃度を
0.01%とし、90℃で60分間加熱して反応させた
のち、抽出剤として0゜■mo1/IlのA11qua
t336/l、2ジクロロエタン100−と該イリジウ
ム溶液100m/を分液漏斗に入れ混合して30分間攪
拌し静置して塩酸溶液相とイリジウムを抽出した有機溶
媒相を分離し、塩酸溶液相中のイリジウムをICPで分
析したところ検出できなかった。
(Example 2) After adjusting the hydrochloric acid concentration of a hydrochloric acid solution containing 100 mg/f of iridium to 2N, chlorine water was added to make the effective chlorine concentration 0.01%, and the mixture was heated at 90°C for 60 minutes to react. Later, A11qua of 0゜■mo1/Il was used as an extractant.
t336/l, 100-2 dichloroethane and 100 m/l of the iridium solution were mixed in a separatory funnel, stirred for 30 minutes, and allowed to stand to separate the hydrochloric acid solution phase and the organic solvent phase from which iridium was extracted. Iridium could not be detected when analyzed by ICP.

(実施例3) イリジウム1(1’Omg/i’を含む塩酸溶液の塩酸
濃度を5規定に調節したのち、塩素水を加えて有効塩素
濃度を0.01%とし、55℃で60分間加熱して反応
させたのち、抽出剤として0. 1mo1/lのA11
quat336/I、2ジクロロエタン100−と該イ
リジウム溶液10〇−を分液漏斗に入れ混合して30分
間攪拌し静置して塩酸溶液相とイリジウムを抽出した有
機溶媒相を分離し、塩酸溶液相中のイリジウムをICP
で分析したところo、08rng検出され、イリジウム
の抽出率は99.2%であった。
(Example 3) After adjusting the hydrochloric acid concentration of a hydrochloric acid solution containing iridium 1 (1'Omg/i') to 5N, add chlorine water to make the effective chlorine concentration 0.01%, and heat at 55°C for 60 minutes. After reaction, 0.1mol/l of A11 was added as an extractant.
quat336/I, 2 dichloroethane 100- and the iridium solution 10- ICP the iridium inside
When analyzed, 0.08 rng was detected, and the iridium extraction rate was 99.2%.

(比較例) イリジウム100mg/I!を含む塩酸溶液の塩酸濃度
を2規定に調節したのち、塩素水を加えて有効塩素濃度
を0.01%とし、20℃で60分間反応させたのち、
抽出剤として0゜1mol/lのA11quat336
/1,2ジクoロエタン100−と該イリジウム溶液1
00−を分液漏斗に入れ混合して30分間攪拌し静置し
て塩酸溶液相とイリジウムを抽出した有機溶媒相を分離
し、塩酸溶液相中のイリジウムをICPで分析したとこ
ろ0.16mg検出され、イリジウムの抽出率は98.
4%であった。
(Comparative example) Iridium 100mg/I! After adjusting the hydrochloric acid concentration of the hydrochloric acid solution containing 2N to 2N, chlorine water was added to make the effective chlorine concentration 0.01%, and after reacting at 20°C for 60 minutes,
0°1 mol/l A11quat336 as extractant
/1,2 dichloroethane 100- and the iridium solution 1
00- was mixed in a separatory funnel, stirred for 30 minutes, left to stand, and the hydrochloric acid solution phase and the organic solvent phase from which iridium was extracted were separated. When the iridium in the hydrochloric acid solution phase was analyzed by ICP, 0.16 mg was detected. The extraction rate of iridium was 98.
It was 4%.

(発明の効果) 以上説明したように、従来イリジウムを■価から■価に
酸化するのに室温で反応させて有機溶媒に抽出していた
がイリジウムの抽出率が十分でなく、本発明の方法によ
ればイリジウムを100%抽出することが容易となりイ
リジウムという極めて稀少価値の高く、しかも高価な金
属の回収精製に関しての技術の発展に大いに寄与するも
と言えるものである。
(Effects of the Invention) As explained above, conventionally, iridium was oxidized from ■ valence to ■ valence by reacting it at room temperature and extracting it into an organic solvent, but the extraction rate of iridium was insufficient, and the method of the present invention According to this method, it is easy to extract 100% of iridium, and it can be said that this method will greatly contribute to the development of technology related to the recovery and purification of iridium, an extremely rare and expensive metal.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は3価および4価のイリジウム塩化物水溶液の各
種塩酸濃度に於いて、抽出剤として0.1mol/I!
のAl 1qua t 336/l、  2ジクロロエ
タンを用いて、イリジウムを抽出した場合の結果を示す
図、第2図は抽出剤と有機相中の抽出された金属濃度と
のモル比を示す図、第3図はイリジウムの溶存状態の変
化をUVスペクトルで観察した結果を示す図である。
Figure 1 shows trivalent and tetravalent iridium chloride aqueous solutions at various hydrochloric acid concentrations of 0.1 mol/I! as an extractant.
Figure 2 shows the results of extracting iridium using Al 1quat 336/l, 2 dichloroethane. Figure 3 is a diagram showing the results of observing changes in the dissolved state of iridium using a UV spectrum.

Claims (3)

【特許請求の範囲】[Claims] (1)イリジウムを含有する塩酸溶液より抽出剤として
有機溶媒を用いてイリジウムを抽出する方法に於いて、
イリジウムを有機溶媒で抽出する前に該イリジウムを含
有する塩酸溶液の塩酸濃度を調節し、該溶液を加熱しな
がら酸化剤を加えて酸化することを特徴とするイリジウ
ムの溶媒抽出法。
(1) In a method of extracting iridium from a hydrochloric acid solution containing iridium using an organic solvent as an extractant,
1. A method for solvent extraction of iridium, which comprises adjusting the hydrochloric acid concentration of a hydrochloric acid solution containing iridium before extracting iridium with an organic solvent, and adding an oxidizing agent to the solution while heating it for oxidation.
(2)前記イリジウムを含有する塩酸溶液の塩酸濃度が
0.1〜5規定に調節する請求項1に記載のイリジウム
の溶媒抽出法。
(2) The method for solvent extraction of iridium according to claim 1, wherein the hydrochloric acid concentration of the iridium-containing hydrochloric acid solution is adjusted to 0.1 to 5 normal.
(3)前記加熱温度が50℃以上で、酸化剤が塩素水で
、溶液中の有効塩素が0.01%以上である請求項1お
よび2に記載のイリジウムの溶媒抽出法。
(3) The method for solvent extraction of iridium according to Claims 1 and 2, wherein the heating temperature is 50° C. or higher, the oxidizing agent is chlorine water, and the available chlorine in the solution is 0.01% or higher.
JP1292846A 1989-11-10 1989-11-10 Solvent extraction method for iridium Expired - Lifetime JP2805689B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1292846A JP2805689B2 (en) 1989-11-10 1989-11-10 Solvent extraction method for iridium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1292846A JP2805689B2 (en) 1989-11-10 1989-11-10 Solvent extraction method for iridium

Publications (2)

Publication Number Publication Date
JPH03153830A true JPH03153830A (en) 1991-07-01
JP2805689B2 JP2805689B2 (en) 1998-09-30

Family

ID=17787123

Family Applications (1)

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Country Status (1)

Country Link
JP (1) JP2805689B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007139876A (en) * 2005-11-15 2007-06-07 Cosmo Japan:Kk Supporter for stringed instrument
JP2008144269A (en) * 2006-11-15 2008-06-26 Semiconductor Energy Lab Co Ltd Method for collecting metal
CN118190689A (en) * 2024-05-15 2024-06-14 贵研检测科技(云南)有限公司 Method for accurately measuring high-content rhodium in iridium-containing noble metal sample

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5183801A (en) * 1974-12-12 1976-07-22 Rhone Poulenc Ind Aruminakeitantai hatsukin oyobi irijiumuyorinaru shokubaiseibun no kaishuhoho
JPS5316316A (en) * 1976-06-21 1978-02-15 Nat I Fuoa Metaraajii Recovering and refining method of iridium

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5183801A (en) * 1974-12-12 1976-07-22 Rhone Poulenc Ind Aruminakeitantai hatsukin oyobi irijiumuyorinaru shokubaiseibun no kaishuhoho
JPS5316316A (en) * 1976-06-21 1978-02-15 Nat I Fuoa Metaraajii Recovering and refining method of iridium

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007139876A (en) * 2005-11-15 2007-06-07 Cosmo Japan:Kk Supporter for stringed instrument
JP2008144269A (en) * 2006-11-15 2008-06-26 Semiconductor Energy Lab Co Ltd Method for collecting metal
CN118190689A (en) * 2024-05-15 2024-06-14 贵研检测科技(云南)有限公司 Method for accurately measuring high-content rhodium in iridium-containing noble metal sample

Also Published As

Publication number Publication date
JP2805689B2 (en) 1998-09-30

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