JP2005146326A - Method for solvent extraction of palladium - Google Patents

Method for solvent extraction of palladium Download PDF

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JP2005146326A
JP2005146326A JP2003383682A JP2003383682A JP2005146326A JP 2005146326 A JP2005146326 A JP 2005146326A JP 2003383682 A JP2003383682 A JP 2003383682A JP 2003383682 A JP2003383682 A JP 2003383682A JP 2005146326 A JP2005146326 A JP 2005146326A
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palladium
solvent
extraction
extracted
continuous
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Hidemasa Nagai
秀昌 永井
Soji Nakamura
壮志 中村
Takenori Moriya
剛憲 守谷
Takashi Hashikawa
隆至 橋川
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Sumitomo Metal Mining Co Ltd
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Sumitomo Metal Mining Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

<P>PROBLEM TO BE SOLVED: To prevent the occurrence of crud in solvent extraction of palladium with dihexyl sulfide (DHS) from an acid solution of hydrochloric acid using a continuous solvent extractor such as a mixer-settler. <P>SOLUTION: Palladium is extracted with DHS from the acid solution of hydrochloric acid, and palladium is back-extracted with aqueous ammonia from the DHS where palladium is extracted. Subsequently, water droplets containing infinitesimal amounts of ammonia and suspended in the solvent after the back-extraction of palladium are continuously filtered using a filter aid such as activated alumina to suppress the occurrence of crud caused by the remaining water droplets. By this method, the continuous operating time of the solvent in the palladium extraction using the continuous solvent extractor such as a mixer-settler can be prolonged. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、パラジウムの溶媒抽出方法に関し、特にパラジウムの抽出に使用する有機溶媒であるジヘキシルサルファイド（ＤＨＳ）の連続使用時間を延長できるパラジウムの溶媒抽出方法に関するものである。   The present invention relates to a palladium solvent extraction method, and more particularly to a palladium solvent extraction method capable of extending the continuous use time of dihexyl sulfide (DHS), which is an organic solvent used for palladium extraction.

金をはじめとする貴金属元素を含有する塩化物溶液から有価金属を順次回収する方法は、たとえば、特公平１−３０８９６号公報に記載されており、特にパラジウムに関しては、硫化ジアルキルを用い溶媒抽出する方法が記載されている。   A method for sequentially recovering valuable metals from a chloride solution containing noble metal elements such as gold is described in, for example, Japanese Examined Patent Publication No. 1-30896, and particularly for palladium, solvent extraction is performed using dialkyl sulfide. A method is described.

また、特開平１０−１３０７４４号公報には、パラジウムを含む塩酸酸性溶液中のパラジウムを硫化ジアルキル中に抽出し、塩酸を用いてスクラビングした後、スクラビング後の硫化ジアルキルから、アンモニア水を用いて、パラジウムを逆抽出する方法において、逆抽出したアンモニア水をろ過する方法が報告されている。   Japanese Patent Laid-Open No. 10-130744 discloses palladium in an acidic hydrochloric acid solution containing palladium extracted into dialkyl sulfide, scrubbed with hydrochloric acid, and from dialkyl sulfide after scrubbing using aqueous ammonia, In the method of back-extracting palladium, a method of filtering back-extracted ammonia water has been reported.

さらに、特開２００２−９７５２７号公報には、前記方法において、パラジウムを溶媒抽出する硫化ジアルキルとしては、ジヘキシルサルファイド（ＤＨＳ）の使用が好ましいことが記載されている。   Furthermore, Japanese Patent Application Laid-Open No. 2002-97527 describes that in the above method, dihexyl sulfide (DHS) is preferably used as the dialkyl sulfide for solvent extraction of palladium.

近年、工業的には、ジヘキシルサルファイド等による溶媒抽出を使用したパラジウム抽出は、ミキサセトラ等の連続溶媒抽出装置を使用することが主流であり、作業量の低減や夜間の自動運転が可能な点でバッチ法と比較して有利である。しかし、溶媒を連続使用することにより、溶媒中に懸濁した水滴が、パラジウム抽出時に大量のクラッド（抽出段にて有機相にも水相にも溶解しない相）の発生を引き起こす原因となっていた。
このような状態に陥った場合、有機溶媒そのものを新しい溶媒に交換する必要があり、溶媒使用量の増加によるコストの増加や、溶媒交換のための工数が必要であるなどの問題の原因となっていた。
特公平１−３０８９６号公報 特開平１０−１３０７４４号公報 特開２００２−９７５２７号公報 In recent years, industrially, palladium extraction using solvent extraction with dihexyl sulfide or the like has been mainly performed using a continuous solvent extraction device such as mixer-settler, so that the amount of work can be reduced and automatic operation at night is possible. It is advantageous compared to the batch method. However, the continuous use of the solvent causes water droplets suspended in the solvent to cause a large amount of clad (phase that does not dissolve in the organic phase or aqueous phase in the extraction stage) during palladium extraction. It was.
In such a situation, it is necessary to replace the organic solvent itself with a new solvent, which causes problems such as an increase in cost due to an increase in the amount of solvent used and a man-hour for solvent replacement. It was.
Japanese Patent Publication No.1-30896 JP-A-10-130744 JP 2002-97527 A

本発明は、このような従来の問題を解決するため、溶媒の寿命すなわち、溶媒の連続使用時間を延長し、溶媒の再生に関わる工数および薬品代を抑えることを目的とする。   In order to solve such a conventional problem, an object of the present invention is to extend the life of the solvent, that is, the continuous use time of the solvent, and to reduce the man-hour and the chemical cost related to the regeneration of the solvent.

上記課題を克服するため、本発明が提供する方法は、パラジウムを含む塩酸酸性溶液をジヘキシルサルファイドに接触させることにより、パラジウムを溶媒中に抽出し、抽出したパラジウムをアンモニア水を用いて逆抽出するパラジウムの溶媒抽出方法において、アンモニア水で逆抽出した後のジヘキシルサルファイドを連続的にろ過し、水滴を除去することを特徴とするパラジウムの溶媒抽出方法であり、ジヘキシルサルファイドのろ過助剤として活性アルミナを使用することを特徴とする溶媒抽出方法である。   In order to overcome the above problems, the method provided by the present invention is to extract palladium in a solvent by contacting an acidic hydrochloric acid solution containing palladium with dihexyl sulfide, and back-extract the extracted palladium using aqueous ammonia. Palladium solvent extraction method is a palladium solvent extraction method characterized by continuously filtering dihexyl sulfide after back extraction with aqueous ammonia and removing water droplets, and activated alumina as a filter aid for dihexyl sulfide. It is a solvent extraction method characterized by using.

すなわち、ジヘキシルサルファイドを連続的に使用する際に溶媒中に懸濁する極微
量の水滴を活性アルミナ等のろ過助剤を使用した連続ろ過により除去する方法である。 In other words, when dihexyl sulfide is continuously used, a very small amount of water suspended in a solvent is removed by continuous filtration using a filter aid such as activated alumina.

本発明の方法により、ミキサセトラ等の連続溶媒抽出装置を使用したジヘキシルサルファイド（ＤＨＳ）によるパラジウム溶媒抽出において、溶媒の入れ替えをすることなく、連続運転時間を延長することができる。   According to the method of the present invention, in palladium solvent extraction with dihexyl sulfide (DHS) using a continuous solvent extraction device such as mixer setra, the continuous operation time can be extended without replacing the solvent.

本発明を適用する、ミキサセトラ等の連続溶媒抽出装置を使用したジヘキシルサルファイド（ＤＨＳ）によるパラジウムを溶媒抽出する用途においては、パラジウムを抽出した溶媒は、アンモニア水にて逆抽出され、洗浄した後に再度パラジウム抽出工程に使用される。   In applications where the present invention is applied to extract palladium with dihexyl sulfide (DHS) using a continuous solvent extraction device such as mixer-settler, the solvent from which palladium has been extracted is back-extracted with aqueous ammonia and washed again after washing. Used in the palladium extraction process.

この洗浄後の溶媒に存在する微細な水滴が、アンモニア分を含んでいるため、抽出段において抽出元液中の白金族元素の一部をアンモニア錯体に変化させる。これが水相に不溶であるため、抽出段にて有機相にも水相にも溶解しない“クラッド”呼ばれる相となり、分相性を悪化させてしまうこととなる。   Since the fine water droplets present in the solvent after washing contain an ammonia component, a part of the platinum group element in the extraction source liquid is changed to an ammonia complex in the extraction stage. Since this is insoluble in the aqueous phase, it becomes a phase called “cladding” that does not dissolve in the organic phase or the aqueous phase in the extraction stage, and the phase separation property is deteriorated.

このような問題を防止するため、逆抽後洗浄した溶媒中に含まれる微細な“水滴”を活性アルミナ等のろ過助剤を使用した連続ろ過により除去することで上記不具合を解消する。   In order to prevent such a problem, the above-mentioned problem is solved by removing fine “water droplets” contained in the solvent washed after reverse extraction by continuous filtration using a filter aid such as activated alumina.

本発明の方法において、洗浄後のジヘキシルサルファイド（ＤＨＳ）をろ過する際に、使用するろ過助剤としては、クロマトグラフ用活性アルミナや、クロマトグラフ用ラジオライト、あるいは、吸着精製用活性アルミナ粉末等が使用できるが、経済的に入手可能な吸着精製用活性アルミナ粉末を用いることで十分効果が発揮できる。
In the method of the present invention, when filtering the washed dihexyl sulfide (DHS), as a filter aid to be used, activated alumina for chromatography, radiolite for chromatography, activated alumina powder for adsorption purification, etc. However, the effect can be sufficiently exhibited by using an activated alumina powder for adsorption purification that is economically available.

（従来例）
パラジウムを含む塩酸酸性溶液をケロシンにて２０％に希釈したジヘキシルサルファイド（ＤＨＳ）使用し、ミキサセトラで連続溶媒抽出法によりパラジウムを抽出した。 (Conventional example)
Palladium was extracted by a continuous solvent extraction method using mixer-settler using dihexyl sulfide (DHS) diluted to 20% with kerosene as an acidic hydrochloric acid solution containing palladium.

パラジウムを抽出後、パラジウムをアンモニア水で逆抽出された溶媒をそのままパラジウム抽出に回し、連続的に使用した。   After extracting palladium, the solvent in which palladium was back-extracted with aqueous ammonia was directly used for palladium extraction and continuously used.

その結果、２００〜５００時間の使用時間で溶媒の交換が必要なほどのクラッドがミキサセトラ内に堆積し、溶媒の交換をすると共に装置内のクラッドの除去作業が必要であった。
（実施例）
パラジウムを含む塩酸酸性溶液をケロシンにて２０％に希釈したジヘキシルサルファイド（ＤＨＳ）使用し、ミキサセトラで連続溶媒抽出法によりパラジウムを抽出した。 As a result, a clad that needs to be replaced with a solvent after 200 to 500 hours of use was deposited in the mixer setra, and it was necessary to replace the solvent and remove the cladding in the apparatus.
(Example)
Palladium was extracted by a continuous solvent extraction method using mixer-settler using dihexyl sulfide (DHS) diluted to 20% with kerosene as an acidic hydrochloric acid solution containing palladium.

パラジウムを抽出後、パラジウムをアンモニア水で逆抽出された溶媒を活性アルミナをろ過助剤として使用し、ジヘキシルサルファイド中に含まれる微量のアンモニアを含む水滴を連続的に除去した後、再度パラジウム抽出に連続的に使用した。   After extraction of palladium, a solvent in which palladium was back-extracted with aqueous ammonia was used as a filter aid for activated alumina, and water droplets containing trace amounts of ammonia contained in dihexyl sulfide were continuously removed, and then extracted again with palladium. Used continuously.

その結果、クラッドの生成が極めた少なく、溶媒の交換をすることなく、約４０００時間の連続使用が可能であった。なお、ろ過に使用したろ過助剤は、クロマトグラフ用活性アルミナと比較して比較的安価な吸着精製用活性アルミナ粉末を用い、前記アルミナ粉末５ｋｇを直径４００ｍｍのろ過器に充填し、前記溶媒を６０ｍｌ／分のろ過速度で連続ろ過を実施した。   As a result, the generation of cladding was extremely small, and continuous use for about 4000 hours was possible without exchanging the solvent. The filter aid used for the filtration was an activated alumina powder for adsorption purification, which is relatively inexpensive compared with the activated alumina for chromatograph, and 5 kg of the alumina powder was packed in a 400 mm diameter filter, and the solvent was added. Continuous filtration was performed at a filtration rate of 60 ml / min.

以上説明したように、本発明によれば、ミキサセトラ等の連続溶媒抽出装置を使用したジヘキシルサルファイド（ＤＨＳ）によるパラジウム溶媒抽出において、従来の問題点である、連続使用時間が短い、工数と薬品代の多く掛かる溶媒の入れ替えの作業が頻繁に必要である、等の問題点を解決し、連続運転時間を従来の８倍以上に引き上げることが可能である。   As described above, according to the present invention, in palladium solvent extraction with dihexyl sulfide (DHS) using a continuous solvent extraction device such as mixer setra, the conventional problem is short, continuous use time, man-hours and chemical cost It is possible to solve the problems such as frequent replacement work of the solvent, and to increase the continuous operation time to 8 times or more of the conventional operation time.

本発明は、ミキサセトラ等の連続溶媒抽出装置を使用する方法において、溶媒の寿命すなわち、溶媒の連続使用時間を延長し、溶媒の再生に関わる工数および薬品代を抑える方法として有用である。
INDUSTRIAL APPLICABILITY The present invention is useful as a method for extending the life of a solvent, that is, the continuous use time of a solvent, and reducing the man-hour and chemical cost related to the regeneration of the solvent in a method using a continuous solvent extraction apparatus such as mixer setra.

Claims (2)

パラジウムを含む塩酸酸性溶液をジヘキシルサルファイドに接触させることにより、パラジウムを溶媒中に抽出し、抽出したパラジウムをアンモニア水を用いて逆抽出するパラジウムの溶媒抽出方法において、アンモニア水で逆抽出した後のジヘキシルサルファイドを連続的にろ過し、水滴を除去することを特徴とするパラジウムの溶媒抽出方法。 In the palladium solvent extraction method in which palladium is extracted into a solvent by contacting a hydrochloric acid acidic solution containing palladium with dihexyl sulfide, and the extracted palladium is back-extracted with aqueous ammonia. A method for solvent extraction of palladium, comprising continuously filtering dihexyl sulfide and removing water droplets. ジヘキシルサルファイドのろ過助剤として活性アルミナを使用することを特徴とする請求項１記載のパラジウムの溶媒抽出方法。 2. The palladium solvent extraction method according to claim 1, wherein activated alumina is used as a filter aid for dihexyl sulfide.
JP2003383682A 2003-11-13 2003-11-13 Method for solvent extraction of palladium Pending JP2005146326A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010059533A (en) * 2008-01-15 2010-03-18 National Institute Of Advanced Industrial Science & Technology Extractant for palladium and method of rapidly separating and recovering palladium using the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010059533A (en) * 2008-01-15 2010-03-18 National Institute Of Advanced Industrial Science & Technology Extractant for palladium and method of rapidly separating and recovering palladium using the same

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