JPH0499232A - Method for extracting palladium - Google Patents
Method for extracting palladiumInfo
- Publication number
- JPH0499232A JPH0499232A JP21339390A JP21339390A JPH0499232A JP H0499232 A JPH0499232 A JP H0499232A JP 21339390 A JP21339390 A JP 21339390A JP 21339390 A JP21339390 A JP 21339390A JP H0499232 A JPH0499232 A JP H0499232A
- Authority
- JP
- Japan
- Prior art keywords
- hydrochloric acid
- palladium
- contg
- phase
- soln
- 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.)
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- 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、パラジウムの溶媒抽出方法に関するもので、
不純物としてスズ、白金等が含有している塩酸溶液から
のパラジウムの抽出分離に関するものである。[Detailed Description of the Invention] (Industrial Application Field) The present invention relates to a method for solvent extraction of palladium.
This invention relates to the extraction and separation of palladium from a hydrochloric acid solution containing impurities such as tin and platinum.
（従来技術とその問題点）
従来、パラジウムを含む塩酸溶液からパラジウムを選択
的に抽出分離する方法として、ジアルキルサルファイド
を含む有機溶媒でパラジウムを抽出する方法があるが、
ジアルキルサルファイドは空気による酸化等でジアルキ
ルスルフオキシドが生成しやすく、また不純物してジア
ルキルスルフオキシドか存在している。(Prior art and its problems) Conventionally, as a method for selectively extracting and separating palladium from a hydrochloric acid solution containing palladium, there is a method of extracting palladium with an organic solvent containing dialkyl sulfide.
Dialkyl sulfoxides tend to generate dialkyl sulfoxides when oxidized by air, and dialkyl sulfoxides are also present as impurities.
このジアルキルスルフオキシドの存在は、０．１％と低
い量であっても白金やスズあるいは他の金属を抽出して
、パラジウムの選択的抽出に妨害となる欠点がある。The presence of this dialkyl sulfoxide, even in amounts as low as 0.1%, has the drawback of extracting platinum, tin or other metals, thereby interfering with the selective extraction of palladium.
（発明の目的）
本発明は、上記の欠点を解決するために成されたもので
、パラジウムを選択的に抽出するためにジアルキルサル
ファイドを含む有機溶媒で抽出した後、該抽出有機溶媒
相中の不純物を除去する方法を提供することを目的とす
る。(Objective of the Invention) The present invention has been made to solve the above-mentioned drawbacks, and after extracting palladium with an organic solvent containing dialkyl sulfide in order to selectively extract palladium, The purpose is to provide a method for removing impurities.
（問題点を解決するための手段）
本発明は、パラジウム含有溶液よりジ−アルキルサルフ
ァイドを含む有機溶媒でパラジウムを溶線抽出した後、
該パラジウムを抽出した有機溶媒相を１〜３Ｎの濃度の
塩酸で洗浄し、次いで０．１Ｎ以下の希塩酸で洗浄する
ことを特徴とするパラジウムの抽出方法で、パラジウム
含有溶液がスズおよび／または白金を含有している塩酸
酸性溶液であるパラジウムの抽出方法である。(Means for Solving the Problems) The present invention involves wire extraction of palladium from a palladium-containing solution with an organic solvent containing di-alkyl sulfide, and then
A palladium extraction method characterized in that the organic solvent phase from which the palladium has been extracted is washed with hydrochloric acid at a concentration of 1 to 3N, and then washed with diluted hydrochloric acid at a concentration of 0.1N or less. This is a method for extracting palladium using an acidic solution of hydrochloric acid containing.
本発明に用いるジ−アルキルサルファイド（Ｒ−８−Ｒ
）の官能基はＲ゛およびＲが同−或いは異なっていても
良く、硫黄原子に直接結合した炭素原子（炭素数６〜１
０が好ましい）を有し、ＲおよびＲはイオン交換基とし
て作用し得る活性官能基または錯体生成基を持たないよ
うなものが選ばれる。Di-alkyl sulfide (R-8-R
), R' and R may be the same or different, and the functional group may be a carbon atom directly bonded to a sulfur atom (having 6 to 1 carbon atoms).
0 is preferred), and R and R are selected such that they have no active functional group or complex-forming group that can act as an ion exchange group.
例えばアルキル、アリール、アラルキル基であり、アル
キル鎖は酸素原子で結合されていても良い。Examples include alkyl, aryl, and aralkyl groups, and the alkyl chains may be bonded via oxygen atoms.
この場合好ましい抽出溶媒は、ジ−ｎ−オクチルサルフ
ァイド、ジ−ｎ−ヘキシルサルファイド、デシル−メチ
ルサルファイドであり、濃度は５〜３０ｖｏ１％が用い
られる。In this case, preferred extraction solvents are di-n-octyl sulfide, di-n-hexyl sulfide, and decyl-methyl sulfide, and the concentration used is 5 to 30 vol%.
パラジウムを含む塩酸溶液中のパラジウム濃度は特に限
定はなく、０． １〜１００ ｇ／ｉ！の範囲であれば
かまわない。The palladium concentration in the hydrochloric acid solution containing palladium is not particularly limited, and is 0. 1~100 g/i! It doesn't matter if it's within the range.
また、溶液中の酸濃度は０．３Ｎ以上の塩酸溶液であれ
ばよく、抽出条件は１〜ＩＯＮが好ましい。Further, the acid concentration in the solution may be a hydrochloric acid solution of 0.3N or more, and the extraction conditions are preferably 1 to ION.
上記のパラジウム含む塩酸溶液とジアルキルサルファイ
ドを含む有機溶媒（炭素数が６〜１５のアルコールを用
いるのが好ましい）に接触させてパラジウムを抽出した
後、該有機溶媒相と塩酸相を分離し、有機溶媒相を１〜
３Ｎの塩酸で洗浄する。After extracting palladium by contacting the above hydrochloric acid solution containing palladium with an organic solvent containing dialkyl sulfide (preferably an alcohol having 6 to 15 carbon atoms), the organic solvent phase and the hydrochloric acid phase are separated, and the organic Solvent phase from 1 to
Wash with 3N hydrochloric acid.
１〜３Ｎの塩酸で洗浄するのは、ジアルキルサルファイ
ドが操作中に空気酸化されてジアルキルスルフオキシド
が生成したり、あるいはジアルキルサルファイドの精製
が不十分で不純物としてジアルキルスルフオキシドが含
まれている場合が多く、パラジウムの抽出操作時に不純
物としてスズや白金を同時に抽出してしまい、そのまま
ではパラジウムを選択的に抽出分離させることができず
、１〜３Ｎ塩酸で洗浄して、スズや白金を分離する必要
かある。Washing with 1 to 3N hydrochloric acid is because the dialkyl sulfide is oxidized in the air during operation and dialkyl sulfoxide is generated, or the dialkyl sulfide is insufficiently purified and contains dialkyl sulfoxide as an impurity. In many cases, when palladium is extracted, tin and platinum are extracted as impurities at the same time, and palladium cannot be extracted and separated selectively, so tin and platinum are separated by washing with 1-3N hydrochloric acid. Is there a need to do that?
洗浄する塩酸濃度を１〜３Ｎとするのは、１Ｎ以下では
スズが水酸化物として沈澱生成しやす（，３Ｎ以上では
スズの洗浄効率が変化なく経済性に欠けるからである。The reason why the hydrochloric acid concentration for cleaning is set to 1 to 3N is that if it is less than 1N, tin tends to precipitate as hydroxide (and if it is more than 3N, the tin cleaning efficiency does not change and it is uneconomical).
また、洗浄回数は不純物の抽出量により異なるが、洗浄
する塩酸濃度は１〜３Ｎの範囲のものを用いて繰り返し
行えばよいものである。Further, although the number of washings varies depending on the amount of impurities extracted, it is sufficient to repeat the washing using a hydrochloric acid concentration in the range of 1 to 3N.
次いでＯ，１Ｎ以下の希塩酸で洗浄するのは、前記パラ
ジウムを抽出した有機溶媒相に白金を抽出していること
が多く、その白金を有機溶媒相より溶離するには０．１
Ｎ以下の希塩酸で洗浄することで可能とし、好ましくは
０，０Ｏ１Ｎ〜０．１Ｎである。The platinum is often extracted into the organic solvent phase from which the palladium has been extracted, and the platinum is then washed with dilute hydrochloric acid of 0.1 N or less.
This can be achieved by washing with dilute hydrochloric acid of N or less, preferably 0.001N to 0.1N.
また、洗浄回数については不純物としての白金の抽出量
により異なるが、洗浄する希塩酸濃度を上記の範囲のも
のを用いて繰り返し行えばよいものである。Further, the number of times of washing varies depending on the amount of platinum extracted as an impurity, but it is sufficient to repeat the washing using a dilute hydrochloric acid concentration within the above-mentioned range.
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）
２０ｖｏ１％シーｎ−へキシルサルファイド、２０ｖｏ
１％２−エチルーヘキシルアルコールに調整したケロシ
ン溶液１００ｍ１とＰｄ５０ｇ＃、Ｐｔ５０ｇ／ｊ７、
Ｓｎ１０ｇ／Ａを含む３Ｎ塩酸溶液１００−を分液ロー
トにて、３０分間振とうし、抽出操作した後、静置して
塩酸相と有機相を分離し、次に有機相を３Ｎ塩酸１００
ｍ１を加えて１０分間振とうして、静置したのち塩酸相
を分離し、次いで０．１Ｎ希塩酸ｔ ｏ ｏｒｒＩ！を
加えてｌＯ分間振とうして、静置したのち希塩酸相を分
離する洗浄操作を３回繰り返した。(Example 1) 20vo 1% sea n-hexyl sulfide, 20vo
100ml of kerosene solution adjusted to 1% 2-ethylhexyl alcohol and 50g of Pd#, 50g of Pt/j7,
A 3N hydrochloric acid solution containing 10g/A of Sn was shaken in a separatory funnel for 30 minutes, extracted, and left to stand to separate the hydrochloric acid phase and the organic phase.
After adding m1 and shaking for 10 minutes and allowing it to stand, the hydrochloric acid phase was separated, and then 0.1N diluted hydrochloric acid to orrI! was added, shaken for 10 minutes, allowed to stand, and the washing operation of separating the dilute hydrochloric acid phase was repeated three times.
洗浄した後の有機相に２５％アンモニア水１００−を加
え２０分間振とうして、静置したのち、アンモニア水相
を分離して、アンモニア水中のパラジウム濃度を分析し
たところ、Ｐｄ４９ｇ＃であった。After washing, 25% ammonia water 100% was added to the organic phase, shaken for 20 minutes, and allowed to stand.The ammonia water phase was separated and the palladium concentration in the ammonia water was analyzed, and it was found to be Pd49g#. .
また、Ｐｔ、Ｓｎはそれぞれ１ｍｇ／Ｉ！以下であった
。Also, Pt and Sn are each 1 mg/I! It was below.
（実施例２）
２０ｖｏ１％シーｎ−ヘキシルサルファイド、２０ｖｏ
１％２−エチルーヘキシルアルコールに調整したケロシ
ン溶液１００１ｎｌとＰｄ１０ｇ＃、Ｐｔ９０ｇ／Ｉ！
、Ｓｎ１０ｇ／Ｉ！を含む３Ｎ塩酸溶液１００１ｎｌを
分液ロートにて、３０分分間上うし、抽出操作した後、
静置して塩酸相と有機相を分離し、次に有機相を３Ｎ塩
酸１００ｍＡ’を加えてｌＯ分間振とうして、静置した
のち塩酸相を分離し、次いて０．１Ｎ希塩酸１００−を
加えて１０分分間上うして、静置したのち希塩酸相を分
離する洗浄操作を３回繰り返した。(Example 2) 20vo 1% sea n-hexyl sulfide, 20vo
1001 nl of kerosene solution adjusted to 1% 2-ethylhexyl alcohol and 10 g of Pd#, 90 g of Pt/I!
, Sn10g/I! Add 1001 nl of 3N hydrochloric acid solution containing
The hydrochloric acid phase and the organic phase were separated by standing, and then the organic phase was added with 100 mA' of 3N hydrochloric acid, shaken for 10 minutes, left to stand, the hydrochloric acid phase was separated, and then 0.1N diluted hydrochloric acid 100 mA' was added. was added to the solution, the mixture was allowed to stand for 10 minutes, and the washing operation of separating the dilute hydrochloric acid phase was repeated three times.
洗浄した後の有機相に２５％アンモニア水１００−を加
え２０分分間上うして、静置したのち、アンモニア水相
を分離して、アンモニア水中のパラジウム濃度を分析し
たところ、Ｐｄ１９．５ｇ／βであった。After washing, 25% ammonia water (100%) was added to the organic phase, the mixture was allowed to rise for 20 minutes, and the ammonia water phase was separated, and the palladium concentration in the ammonia water was analyzed and found to be Pd 19.5 g/β. Met.
また、ｐｔは３ｍｇ／Ｃ８ｎは１． ｍ ｇ ／ ｌ以
下てあった。Also, pt is 3mg/C8n is 1. mg/l or less.
（実施例３）
２０ｖｏ１％ジーｎ−オクチルサルファイド、２０ｖｏ
１％ｎ−ヘキシルアルコールに調整したケロシン溶液１
００７ｄをＰｄ ５０ ｇ／Ｉ！、 Ｐ ｔ５０ ｇ／
１２． Ｓｎ Ｉ Ｏｇ／Ｉ２を含む３Ｎ塩酸溶液１０
０、ｖ２７７を分液ロートにて、３０分分間上うし、抽
出操作した後、静置して塩酸相と有機相を分離し、次に
有機相を３Ｎ塩酸＋００１ｎｌを加えて１゜分間振とう
して、静置したのち塩酸相を分離して洗浄し、次いで０
、１Ｎ希塩酸１００ｍＡ’を加えて１０分分間上うして
、静置したのち希塩酸相を分離する洗浄操作を３回繰り
返した。(Example 3) 20vo 1% G-n-octyl sulfide, 20vo
Kerosene solution 1 adjusted to 1% n-hexyl alcohol
007d to Pd 50 g/I! , P t50 g/
12. 3N hydrochloric acid solution containing Sn I Og/I2 10
0, v277 in a separatory funnel for 30 minutes, and after the extraction operation, leave it to stand to separate the hydrochloric acid phase and the organic phase.Next, add 3N hydrochloric acid + 001nl to the organic phase and shake for 1 degree. After standing still, the hydrochloric acid phase was separated and washed, and then
, 100 mA' of 1N diluted hydrochloric acid was added, the mixture was heated for 10 minutes, left to stand, and the washing operation of separating the diluted hydrochloric acid phase was repeated three times.
洗浄した後の有機相に２５％アンモニア水５゜ｉを加え
２０分分間上うして、静置したのち、アンモニア水相を
分離して、アンモニア水中のパラジウム濃度を分析した
ところ、Ｐｄ４８．５ｇ／ｌであった。25% ammonia water was added to the washed organic phase for 20 minutes, and the ammonia water phase was separated and the palladium concentration in the ammonia water was analyzed. It was l.
また、Ｐｔは４ ｍ ｇ ／ ｌで、Ｓｎは１ｍｇ／ｌ
であった。In addition, Pt is 4 mg/l and Sn is 1 mg/l.
Met.
（比較例１）
洗浄する塩酸濃度を０．１．Ｎだけで行った以外実施例
１と同様に操作したところ、洗浄操作中に多量の沈澱が
発生してしまった。(Comparative Example 1) The concentration of hydrochloric acid for washing was set to 0.1. When the same procedure as in Example 1 was carried out except that only N was used, a large amount of precipitate was generated during the washing operation.
（比較例２）
洗浄する塩酸濃度を３Ｎだけで行った以外実施例１と同
様に操作したところ、アンモニア水中のパラジウムは４
９ ｇ／ｌと同じであったが、Ｐｔが８０ｍｇ／ｆと高
く、Ｓｎはｌ０ｍｇ／ｉ’で洗浄が十分されなかった。(Comparative Example 2) The same procedure as in Example 1 was carried out except that the concentration of hydrochloric acid for washing was 3N, and the palladium in the ammonia water was 4.
Although it was the same as 9 g/l, Pt was high at 80 mg/f, and Sn was 10 mg/i', which was not sufficiently washed.
（発明の効果）
以上の説明で明らかのように、シーアルキルサルファイ
ドを含む有機溶媒でパラジウムを抽出分離する際に１〜
３Ｎの塩酸で洗浄し、次いで０． １Ｎ以下の希塩酸
で洗浄することで、操作中に沈澱を発生させることがな
く、また不純物として白金やスズを混入させることもな
く、選択的にパラジウムを抽出させ、次いでアンモニア
水でパラジウムを逆抽出させることで、パラジウムの分
離が効果的に行えるものである。(Effect of the invention) As is clear from the above explanation, when extracting and separating palladium with an organic solvent containing sea alkyl sulfide,
Wash with 3N hydrochloric acid, then 0. By washing with dilute hydrochloric acid of 1N or less, palladium is selectively extracted without generating precipitation during operation, and without mixing platinum or tin as impurities, and then back-extracting palladium with aqueous ammonia. By doing so, palladium can be effectively separated.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (2)
ドを含む有機溶媒でパラジウムを溶媒抽出した後、該パ
ラジウムを抽出した有機溶媒相を１〜３Ｎの濃度の塩酸
で洗浄し、次いで０．１Ｎ以下の希塩酸で洗浄すること
を特徴とするパラジウムの抽出方法。(1) After extracting palladium from a palladium-containing solution with an organic solvent containing di-alkyl sulfide, the organic solvent phase from which the palladium was extracted is washed with hydrochloric acid at a concentration of 1 to 3N, and then diluted hydrochloric acid at a concentration of 0.1N or less. A palladium extraction method characterized by washing with.
含有している塩酸酸性溶液である請求項１に記載のパラ
ジウムの抽出方法。(2) The palladium extraction method according to claim 1, wherein the palladium-containing solution is an acidic hydrochloric acid solution containing tin and/or platinum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2213393A JP2995217B2 (en) | 1990-08-10 | 1990-08-10 | Extraction method of palladium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2213393A JP2995217B2 (en) | 1990-08-10 | 1990-08-10 | Extraction method of palladium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0499232A true JPH0499232A (en) | 1992-03-31 |
| JP2995217B2 JP2995217B2 (en) | 1999-12-27 |
Family
ID=16638462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2213393A Expired - Lifetime JP2995217B2 (en) | 1990-08-10 | 1990-08-10 | Extraction method of palladium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2995217B2 (en) |
-
1990
- 1990-08-10 JP JP2213393A patent/JP2995217B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2995217B2 (en) | 1999-12-27 |
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