JP2995217B2 - Extraction method of palladium - Google Patents
Extraction method of palladiumInfo
- Publication number
- JP2995217B2 JP2995217B2 JP2213393A JP21339390A JP2995217B2 JP 2995217 B2 JP2995217 B2 JP 2995217B2 JP 2213393 A JP2213393 A JP 2213393A JP 21339390 A JP21339390 A JP 21339390A JP 2995217 B2 JP2995217 B2 JP 2995217B2
- Authority
- JP
- Japan
- Prior art keywords
- hydrochloric acid
- palladium
- phase
- washing
- concentration
- 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.)
- Expired - Lifetime
Links
Landscapes
- Manufacture And Refinement Of Metals (AREA)
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。Description: TECHNICAL FIELD The present invention relates to a solvent extraction method for palladium, and more particularly to an extraction separation of palladium from a hydrochloric acid solution containing tin, platinum and the like as impurities. .
（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
ルキルスルフォキシドが生成しやすく、また不純物して
ジアルキルスルフォキシドが存在している。(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. However, dialkyl sulfide is oxidized by air or the like. , Dialkyl sulfoxide is easily produced, and dialkyl sulfoxide is present as an impurity.
このジアルキルスルフォキシドの存在は、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 has the drawback that it can extract platinum, tin or other metals even at as low as 0.1% and hinder 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。(Object of the Invention) The present invention has been made in order to solve the above-mentioned drawbacks. In order to selectively extract palladium, the present invention is performed by extracting with an organic solvent containing a dialkyl sulfide and then extracting the palladium from the organic solvent phase. It is an object 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 provides a method for extracting palladium from a palladium-containing solution with an organic solvent containing di-alkyl sulfide, and then extracting the palladium-extracted organic solvent phase with hydrochloric acid having a concentration of 1 to 3N. And then washing with 0.1N or less dilute hydrochloric acid, wherein the palladium-containing solution is a hydrochloric acid acidic solution containing tin and / or platinum.
本発明に用いるジ−アルキルサルファイド（Ｒ′−Ｓ
−Ｒ）の官能基はＲ′およびＲが同一或いは異なってい
ても良く、硫黄原子に直接結合した炭素原子（炭素数６
〜10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。The di-alkyl sulfide (R'-S) used in the present invention
In the functional group of —R), R ′ and R may be the same or different, and a carbon atom directly bonded to a sulfur atom (C 6
R 'and R are selected so as to have no active functional group or complex-forming group capable of acting 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。For example, it is an alkyl, aryl, or aralkyl group, and the alkyl chain may be bonded by an oxygen atom.
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５〜30vol％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 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、0.1〜100g/の範囲であればかまわない。The concentration of palladium in the hydrochloric acid solution containing palladium is not particularly limited, and may be in the range of 0.1 to 100 g /.
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１〜10Nが好ましい。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 10N.
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 hydrochloric acid solution containing palladium and an organic solvent containing dialkyl sulfide (preferably an alcohol having 6 to 15 carbon atoms) to extract palladium, the organic solvent phase and the hydrochloric acid phase are separated. Solvent phase 1
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ォキシド
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ォキシドが含
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
がある。Washing with 1 to 3N hydrochloric acid may result in the dialkyl sulfide being air-oxidized during operation to produce dialkyl sulfoxide, or the dialkyl sulfide is not sufficiently purified and contains dialkyl sulfoxide as an impurity. In many cases, tin and platinum were simultaneously extracted as impurities during the palladium extraction operation, and palladium could not be selectively extracted and separated as it was, washed with 1 to 3N hydrochloric acid to separate tin and platinum. There is a need to.
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く、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 concentration of hydrochloric acid to be washed is set to 1 to 3 N because tin tends to precipitate and form as hydroxide at 1 N or less, and at 3 N or more, the washing efficiency of tin is not changed and lacks economy.
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, the number of times of washing varies depending on the amount of extracted impurities, but the concentration of hydrochloric acid to be washed may be repeated using a solution in the range of 1 to 3N.
次いで0.1N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0.1N以下
の希塩酸で洗浄することで可能とし、好ましくは0.001N
〜0.1Nである。Then, washing with 0.1 N or less dilute hydrochloric acid often involves extracting platinum into the organic solvent phase from which the palladium has been extracted, and washing with 0.1 N or less dilute hydrochloric acid to elute the platinum from the organic solvent phase. Possible, preferably 0.001N
~ 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。Although the number of times of washing differs depending on the amount of platinum extracted as an impurity, the washing may be performed repeatedly using a diluted hydrochloric acid concentration in the above 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。Hereinafter, examples according to the present invention will be described, but the examples do not limit the present invention.
（実施例１） 20vol％ジ−ｎ−ヘキシルサルファイド、20vol％２−
エチル−ヘキシルアルコールに調整したケロシン溶液10
0mlとPd50g/、Pt50g/、Sn10g/を含む3N塩酸溶液1
00ml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100ml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100mlを加えて10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) 20 vol% di-n-hexyl sulfide, 20 vol% 2-
Kerosene solution adjusted to ethyl-hexyl alcohol 10
3N hydrochloric acid solution containing 0ml and Pd50g /, Pt50g /, Sn10g / 1
00 ml was shaken in a separating funnel for 30 minutes, and after the extraction operation, the mixture was allowed to stand to separate the hydrochloric acid phase and the organic phase, and then the organic phase was 3N
A washing operation of adding 100 ml of hydrochloric acid, shaking for 10 minutes, allowing the mixture to stand, separating the hydrochloric acid phase, adding 100 ml of 0.1N diluted hydrochloric acid, shaking for 10 minutes, allowing the mixture to stand, and separating the diluted hydrochloric acid phase, was performed in three steps. Repeated times.
洗浄した後の有機相に25％アンモニア水100mlを加え2
0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。100 ml of 25% aqueous ammonia is added to the organic phase after washing, and 2
After shaking for 0 minutes and allowing to stand, the aqueous ammonia phase was separated and the concentration of palladium in the aqueous ammonia was analyzed.
また、Pt、Snはそれぞれ1mg/以下であった。 Further, Pt and Sn were each 1 mg / or less.
（実施例２） 20vol％ジ−ｎ−ヘキシルサルファイド、20vol％２−
エチル−ヘキシルアルコールに調整したケロシン溶液10
0mlとPd10g/、Pt90g/、Sn10g/を含む3N塩酸溶液1
00ml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100ml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100mlを加えて10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 2) 20 vol% di-n-hexyl sulfide, 20 vol% 2-
Kerosene solution adjusted to ethyl-hexyl alcohol 10
0 ml and 3N hydrochloric acid solution 1 containing Pd10g /, Pt90g /, Sn10g /
00 ml was shaken in a separating funnel for 30 minutes, and after the extraction operation, the mixture was allowed to stand to separate the hydrochloric acid phase and the organic phase, and then the organic phase was 3N
A washing operation of adding 100 ml of hydrochloric acid, shaking for 10 minutes, allowing the mixture to stand, separating the hydrochloric acid phase, adding 100 ml of 0.1N diluted hydrochloric acid, shaking for 10 minutes, allowing the mixture to stand, and separating the diluted hydrochloric acid phase, was performed in three steps. Repeated times.
洗浄した後の有機相に25％アンモニア水100mlを加え2
0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、Pd19.5g/であった。100 ml of 25% aqueous ammonia is added to the organic phase after washing, and 2
After shaking for 0 minutes and allowing to stand, the aqueous ammonia phase was separated, and the concentration of palladium in the aqueous ammonia was analyzed. The result was 19.5 g / Pd.
また、Pt、Snは3mg/、Snは1mg/以下であった。 Further, Pt and Sn were 3 mg / and Sn was 1 mg / or less.
（実施例３） 20vol％ジ−ｎ−オクチルサルファイド、20vol％ｎ−
ヘキシルアルコールに調整したケロシン溶液100mlをPd5
0g/、Pt50g/、Sn10g/を含む3N塩酸溶液100ml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100m
lを加えて10分間振とうして、静置したのち塩酸相を分
離して洗浄し、次いで0.1N希塩酸100mlを加えて10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 3) 20 vol% di-n-octyl sulfide, 20 vol% n-
100 ml of a kerosene solution adjusted to hexyl alcohol was added to Pd5
100 g of a 3N hydrochloric acid solution containing 0 g /, 50 g of Pt /, and 10 g of Sn was shaken in a separatory funnel for 30 minutes, subjected to an extraction operation, allowed to stand still to separate a hydrochloric acid phase and an organic phase, and then the organic phase was separated. 3N hydrochloric acid 100m
l, shake for 10 minutes, leave to stand, separate and wash the hydrochloric acid phase, then wash with 100 ml of 0.1N diluted hydrochloric acid, shake for 10 minutes, leave to stand, and separate 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50ml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、Pd48.5g/であった。To the organic phase after washing, add 50 ml of 25% aqueous ammonia and add 20 ml.
After shaking for a minute and allowing to stand, the aqueous ammonia phase was separated, and the concentration of palladium in the aqueous ammonia was analyzed. The result was 48.5 g / Pd.
また、Ptは4mg/で、Snは1mg/であった。 Further, Pt was 4 mg / and Sn was 1 mg /.
（比較例１） 洗浄する塩酸濃度を0.1N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) When the same operation as in Example 1 was performed except that the concentration of hydrochloric acid to be washed was only 0.1 N, 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49
g/と同じであったが、Ptが80mg/と高く、Snは10mg/
で洗浄が十分されなかった。(Comparative Example 2) The same operation as in Example 1 was carried out except that the concentration of hydrochloric acid to be washed was only 3N.
g /, but Pt was as high as 80 mg / and Sn was 10 mg /
Cleaning was not sufficient.
（発明の効果） 以上の説明で明らかのように、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
的な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 description, when palladium is extracted and separated with an organic solvent containing di-alkyl sulfide, 1
By washing with ~ 3N hydrochloric acid and then with 0.1N or less dilute hydrochloric acid, selective palladium extraction without precipitation during operation and without mixing platinum or tin as impurities And then back-extracting the palladium with aqueous ammonia to effectively separate the palladium
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平２−59551（ＪＰ，Ａ) 特開 昭51−84702（ＪＰ，Ａ) 特開 平１−263228（ＪＰ，Ａ) 特開 昭63−128135（ＪＰ，Ａ) 特開 昭63−128136（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) C22B 11/04 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-2-59551 (JP, A) JP-A-51-84702 (JP, A) JP-A-1-263228 (JP, A) JP-A-63-63 128135 (JP, A) JP-A-63-128136 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) C22B 11/04
Claims (1)
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。A palladium-containing solution containing tin and / or platinum is subjected to solvent extraction of palladium with an organic solvent containing di-alkyl sulfide, and the organic solvent phase from which the palladium is extracted is treated with hydrochloric acid having a concentration of 1 to 3N. A method for extracting palladium, comprising washing, followed by washing with dilute hydrochloric acid of 0.1 N or less.
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 JPH0499232A (en) | 1992-03-31 |
| JP2995217B2 true 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 |
|---|---|
| JPH0499232A (en) | 1992-03-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100230826B1 (en) | Method of recovering gold | |
| WO2005083131A1 (en) | Extractants for palladium and process for separation and recovery of palladium | |
| JP3079034B2 (en) | How to recover platinum | |
| JP2995217B2 (en) | Extraction method of palladium | |
| CA1230977A (en) | Process for separating and purifying metals of the platinum group (i) | |
| EP0404327B1 (en) | Recovery of pure platinum and palladium | |
| JPH09279264A (en) | Continuous extraction and recovery method for precious metals | |
| JPH0499233A (en) | Method for extracting palladium | |
| JPS55164042A (en) | Method of separating and recovering platinum from platinum plating waste liquid | |
| JP3164262B2 (en) | Noble metal extractant and method for separating noble metal using the extractant | |
| JPH07331349A (en) | Method for separating and recovering palladium and silver | |
| RU2108294C1 (en) | Method of recovering and purifying platinum group metals and gold | |
| JP3611992B2 (en) | Extraction method of palladium | |
| FR2656150A1 (en) | PROCESS FOR RECOVERING USING A PLUTONIUM CROWN ETHER PRESENT IN SOLUTIONS SUCH AS AQUEOUS EFFLUENTS, CONCENTRATED FISSION PRODUCT SOLUTIONS AND CONCENTRATED PLUTONIUM SOLUTIONS | |
| RU2121517C1 (en) | Method of recovering and separating platinum and palladium | |
| RU2378402C2 (en) | Extraction method of germanium from sulfuric solutions | |
| JP3225188B2 (en) | Extractant for palladium extraction and recovery method of palladium | |
| JP2892465B2 (en) | Extractant regeneration method | |
| JP2504810B2 (en) | Method for reducing sulfoxide in organic solvent and method for extracting noble metal using the reduction | |
| JP3081920B1 (en) | Selective extraction agent for palladium and method for selective extraction and recovery of palladium using the same | |
| JPS63286528A (en) | Recovering method for pd from pd-containing aqueous solution | |
| JPH0499136A (en) | Method for extracting paradium | |
| RU2156818C1 (en) | Method of preparing platinum group metals from tin- containing solution | |
| JPH06335601A (en) | Extracting agent for pt, pd and au and separation of pt, pd and/or au using the same agent | |
| JPS63286529A (en) | Recovering method for pd from pd-containing aqueous solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081029 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101029 Year of fee payment: 11 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101029 Year of fee payment: 11 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101029 Year of fee payment: 11 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101029 Year of fee payment: 11 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101029 Year of fee payment: 11 |