JP2001152259A - Method for separating and recovering silver - Google Patents
Method for separating and recovering silverInfo
- Publication number
- JP2001152259A JP2001152259A JP33361999A JP33361999A JP2001152259A JP 2001152259 A JP2001152259 A JP 2001152259A JP 33361999 A JP33361999 A JP 33361999A JP 33361999 A JP33361999 A JP 33361999A JP 2001152259 A JP2001152259 A JP 2001152259A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- extraction
- palladium
- solution
- separating
- 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
Links
Classifications
-
- 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
Description
【０００１】[0001]
【発明の属する技術分野】本発明はパラジウム等の金属
中に不純物として含まれる銀を選択的に分離し、更にこ
の銀を効率的に回収する銀の分離・回収方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for selectively separating silver contained as an impurity in a metal such as palladium and further recovering the silver efficiently.
【０００２】[0002]
【従来の技術】銀はそれ自体が有用な金属である一方、
他の有用な金属中に不純物として微量含まれていること
がある。この場合不純物として扱われる銀は、当該他の
金属の高純度化を図る必要がある場合には除去しなけれ
ばならない。BACKGROUND OF THE INVENTION While silver is a useful metal in itself,
Trace amounts of impurities may be contained in other useful metals. In this case, silver treated as an impurity must be removed when it is necessary to purify the other metal.
【０００３】この一例として、パラジウム中に含まれて
いる銀の問題がある。パラジウムは近年、電気・電子材
料として注目を浴びている貴金属であるが、市販のパラ
ジウム地金には微量の銀が含有されている。一般に、電
気・電子材料として用いられる金属材料にはその電気特
性を保持するため、この市販の地金から不純物として存
在する銀を除去しなければならない。One example of this is the problem of silver contained in palladium. Palladium is a precious metal that has recently attracted attention as an electric / electronic material, but commercially available palladium metal contains a trace amount of silver. Generally, in order to maintain the electrical characteristics of a metal material used as an electric / electronic material, silver which is present as an impurity must be removed from this commercially available metal.
【０００４】このパラジウムの高純度化、即ち不純物で
ある銀の除去方法として溶媒抽出法が用いられる。溶媒
抽出法とは、相互に溶解度の低い２液相間における目的
成分の分配を利用した分離方法で、通常、目的成分を含
む水溶液と、目的成分と反応性を有する抽出剤を含有す
る有機相（抽出溶媒）とを接触させ、目的成分を有機相
へと移行させ目的成分を分離する方法である。そして、
パラジウムの高純度化にあたっては地金を塩酸、硝酸な
どの酸溶液に溶解させ、この溶液と抽出溶媒とを接触さ
せることにより行われている。A solvent extraction method is used as a method for purifying the palladium, that is, removing silver as an impurity. The solvent extraction method is a separation method utilizing the distribution of a target component between two liquid phases having low solubility, and is usually an aqueous solution containing the target component and an organic phase containing an extractant reactive with the target component. (Extraction solvent) to transfer the target component to the organic phase to separate the target component. And
In purifying palladium, a base metal is dissolved in an acid solution such as hydrochloric acid or nitric acid, and the solution is brought into contact with an extraction solvent.
【０００５】従来、溶媒抽出法によるパラジウムの高純
度の手法としては、例えば、特開平７−３３１３４９に
開示されたものがある。これは、下記化３で示されるア
ミン化合物と、化４で示される高級アルコール又はトリ
アルキル燐酸エステルとの混合物を抽出溶媒として、パ
ラジウムと銀とを含有する硝酸水溶液に接触させる方法
がある。Conventionally, a high-purity method of palladium by a solvent extraction method is disclosed in, for example, JP-A-7-331349. In this method, a mixture of an amine compound represented by the following formula (3) and a higher alcohol or a trialkyl phosphate represented by the following formula (4) is used as an extraction solvent and brought into contact with an aqueous nitric acid solution containing palladium and silver.
【０００６】[0006]
【化３】 〔式中、Ｒ１は炭素数が１〜２５の直鎖又は側鎖を有す
るアルキル基、アルコキシ基、アリル基又はアカリル基
である。Ｒ２，Ｒ３はそれぞれ水素原子若しくは炭素数
が１〜２５の直鎖又は側鎖を有するアルキル基、アルコ
キシ基、アリル基又はアカリル基である。〕Embedded image [In the formula, R 1 is an alkyl group, an alkoxy group, an allyl group, or an acalyl group having a linear or side chain having 1 to 25 carbon atoms. R 2 and R 3 are a hydrogen atom or an alkyl group, an alkoxy group, an allyl group, or an acaryl group having a linear or side chain having 1 to 25 carbon atoms. ]
【０００７】[0007]
【化４】 〔式中、Ｒ４は炭素数が１〜２５の直鎖又は側鎖を有す
るアルキル基、アルコキシ基である。〕Embedded image [In the formula, R 4 is an alkyl group or alkoxy group having a linear or side chain having 1 to 25 carbon atoms. ]
【０００８】[0008]
【発明が解決しようとする課題】ここで、この従来の溶
媒抽出法における抽出剤であるアミン化合物は、不純物
である銀ではなく、富化目的のパラジウムに対する選択
性が高いため、まず溶媒にパラジウムを抽出し、その後
この抽出溶媒からパラジウムを逆抽出させるという工程
を採らざるを得ない。しかしながら、溶液中に多量に含
まれているパラジウムを選択抽出する手法は、製造され
るパラジウム量が水溶液から溶媒へパラジウムを抽出さ
せる際の収率（抽出率）とパラジウム抽出後の溶媒から
パラジウムを抽出させる際の収率（逆抽出率）との双方
により左右され、わずかな収率の低下によってもパラジ
ウム量が低下し採取されるパラジウム量にロスが生じる
こととなるため効率的な方法とはいいがたい。即ち、パ
ラジウム中に含まれている不純物（銀）を除去するのが
目的であるのならば、むしろ銀を選択的に選択抽出でき
るような方法の方がより効率的であると考えられる。The amine compound, which is an extractant in the conventional solvent extraction method, has high selectivity for palladium for enrichment, not silver, which is an impurity. , And then back-extracting palladium from the extraction solvent. However, the method of selectively extracting palladium contained in a large amount in a solution is based on the fact that the amount of palladium produced is determined by extracting palladium from an aqueous solution to a solvent (extraction rate) and extracting palladium from the solvent after palladium extraction. An efficient method because it depends on both the yield at the time of extraction (back-extraction rate) and even a slight decrease in the yield decreases the amount of palladium and causes a loss in the amount of collected palladium. I'm sorry. That is, if the purpose is to remove impurities (silver) contained in palladium, it is considered that a method capable of selectively extracting silver is more efficient.
【０００９】このパラジウムの例ように、銀が不純物と
して含まれている金属の高純度化を目的とする溶媒抽出
法においては、不純物である銀に対する選択性の高い抽
出剤を用いて銀を抽出する方が効率的であるが、本発明
者らの知る限り、銀の抽出剤についてはあまり検討され
ておらず、その抽出挙動についても不明点が多いことか
ら、銀を直接分離回収する技術にとして溶媒抽出法はほ
とんど利用されていないのが現状である。In the solvent extraction method for purifying a metal containing silver as an impurity, as in the case of palladium, silver is extracted using an extractant having high selectivity for silver as an impurity. Although it is more efficient to do so, as far as the present inventors know, silver extractants have not been studied much, and there are many unclear points regarding their extraction behavior. At present, the solvent extraction method is hardly used.
【００１０】また、上述のように銀もそれ自体が有用な
金属であり、装飾用材料、電気材料等多くの用途がある
金属である。従って、不純物として取り扱われるもので
あっても、効率よく回収することが経済的観点からして
望ましいといえる。[0010] As described above, silver itself is a useful metal, and has many uses such as decorative materials and electric materials. Therefore, it can be said that it is desirable from an economic point of view to efficiently recover even those treated as impurities.
【００１１】本発明は以上のような背景の下なされたも
のであり、銀と他の金属との混合物より銀を選択的に分
離し、かつ、この銀を効率的に回収する手法を提供する
ものである。The present invention has been made in view of the above background, and provides a method of selectively separating silver from a mixture of silver and another metal and efficiently recovering the silver. Things.
【００１２】[0012]
【課題を解決するための手段】かかる課題を解決すべ
く、本発明者らは鋭意研究を行った結果、本願請求項１
に係る発明を完成させるに至った。即ち、本願請求項１
に記載の発明は、銀を含有する溶液と、化５で示される
ヒダントイン化合物と化６で示される高級アルコールと
を混合してなる抽出溶媒とを接触させ、該抽出溶媒中に
銀を選択抽出させる銀の分離・回収方法である。Means for Solving the Problems In order to solve such problems, the inventors of the present invention have conducted intensive studies and as a result, claim 1 of the present application.
Has been completed. That is, Claim 1 of the present application
In the invention described in (1), a solution containing silver is brought into contact with an extraction solvent obtained by mixing a hydantoin compound represented by the chemical formula 5 with a higher alcohol represented by the chemical formula 6, and silver is selectively extracted in the extraction solvent. This is a method for separating and recovering silver.
【００１３】[0013]
【化５】 〔式中Ｒ１、Ｒ２はフェニル基、若しくは炭素数６以上
の直鎖又は側鎖を有するアルキル基、若しくは水素を示
す。〕Embedded image [In the formula, R1 and R2 represent a phenyl group, an alkyl group having 6 or more carbon atoms having a straight or side chain, or hydrogen. ]
【００１４】[0014]
【化６】 〔式中Ｒ３は、炭素数８から１６の直鎖又は側鎖を有す
るアルキル基を示す。〕Embedded image [In the formula, R 3 represents an alkyl group having 8 to 16 carbon atoms and having a straight or side chain. ]
【００１５】本発明で抽出剤として利用される化５で示
されるヒダントイン化合物は、溶液中の銀イオンとプロ
トン交換反応して錯形成することにより銀を抽出するも
のである。従って、本発明によれば、不純物である銀と
他の金属との混合物を分離する際に、従来のよう富化目
的である当該他の金属を抽出するものとは異なり、不純
物である銀を選択抽出することができるため富化目的の
金属のロスを低減することができる。そして、特に、本
発明の抽出剤であるヒダントイン化合物は銀に対して特
異的な選択性を有すものであることから、銀と他の金属
が存在する溶液より、銀を極めて高い抽出率で抽出し当
該他の金属の高純度化を図ることが可能となる。The hydantoin compound represented by Chemical Formula 5 used as an extractant in the present invention is a compound that extracts silver by performing a proton exchange reaction with silver ions in a solution to form a complex. Therefore, according to the present invention, when separating a mixture of silver, which is an impurity, and another metal, unlike the conventional method for extracting the other metal, which is an enrichment object, the silver, which is an impurity, is separated. Since selective extraction is possible, loss of the metal for the purpose of enrichment can be reduced. In particular, since the hydantoin compound, which is the extractant of the present invention, has specific selectivity for silver, silver can be extracted at an extremely high extraction rate from a solution in which silver and other metals are present. Extraction makes it possible to purify the other metal.
【００１６】ここで、抽出剤であるヒダントイン化合物
と共に抽出溶媒を構成する高級アルコールは、抽出溶媒
の分散性、分相性を調整するための希釈剤としての機能
を有するものである。そして、化５において、Ｒ３を炭
素数８から１６の直鎖又は側鎖を有するアルキル基とす
るのは、このような高級アルコールのみヒダントイン化
合物を溶解させることができるからであり、通常の抽出
溶媒の希釈剤として用いられる有機溶媒、例えばケロシ
ンやベンゼンは、本発明の抽出剤であるヒダントイン化
合物を溶解させることができず、希釈剤として機能しな
いからである。また、アルコールでも置換基Ｒ３の炭素
数が低い低級アルコールはヒダントイン化合物を溶解さ
せることはできない。尚、この抽出剤と希釈剤とを混合
して抽出溶媒とする際の抽出剤の濃度は、抽出する銀含
有溶液中の銀濃度にもよるが１〜３０ｍｍｏｌ／ｄｍ３
とするのが好ましい。Here, the higher alcohol constituting the extraction solvent together with the hydantoin compound as the extractant has a function as a diluent for adjusting the dispersibility and phase separation of the extraction solvent. The reason why R 3 is an alkyl group having a straight or side chain having 8 to 16 carbon atoms in Chemical formula 5 is that only such higher alcohols can dissolve the hydantoin compound, This is because an organic solvent used as a diluent for a solvent, for example, kerosene or benzene cannot dissolve the hydantoin compound as the extractant of the present invention and does not function as a diluent. In addition, lower alcohols having a lower carbon number of the substituent R 3 cannot dissolve the hydantoin compound. The concentration of the extractant when the extractant and the diluent are mixed and used as an extraction solvent depends on the silver concentration in the silver-containing solution to be extracted, but is 1 to 30 mmol / dm 3.
It is preferred that
【００１７】また、上述のように、本発明の抽出剤であ
るヒダントイン化合物の抽出作用は、ヒダントイン化合
物と銀イオンとも錯形成によるものであり、この反応は
溶液中の銀イオンとのプロトン交換に基づくものであ
る。従って、本発明における銀の抽出率は、銀を含有す
る溶液のｐＨ値に影響を受ける。そこで、本発明におい
て銀抽出率を最適なものとするためには、ｐＨの変動を
低減するため請求項２のように、銀を含有する溶液に緩
衝剤として硝酸アンモニウムを添加するのが好ましい。Further, as described above, the extraction effect of the hydantoin compound, which is the extractant of the present invention, is due to complex formation between the hydantoin compound and silver ions, and this reaction involves proton exchange with silver ions in the solution. It is based on Therefore, the extraction rate of silver in the present invention is affected by the pH value of the solution containing silver. Therefore, in order to optimize the silver extraction rate in the present invention, it is preferable to add ammonium nitrate as a buffer to the silver-containing solution in order to reduce the fluctuation of pH.
【００１８】そして、銀を含有する溶液のｐＨ値の範囲
としては、請求項３記載のように、ｐＨ５〜７とするの
が好ましい。ｐＨが５以下であると反応が進行しがたく
なるからである。また、ｐＨが７以上となると溶液中の
アンモニアと銀イオンとがアンミン錯体を形成しやすく
なり、ヒダントイン化合物と銀イオンとの錯形成を妨げ
るためである。尚、このｐＨ値の調整は、溶液にアンモ
ニア又は硫酸のようなアルカリ溶液、酸溶液を添加する
ことで容易に行うことができる。The pH of the solution containing silver is preferably in the range of pH 5 to pH 7. This is because if the pH is 5 or less, the reaction hardly proceeds. In addition, when the pH is 7 or more, ammonia and silver ions in the solution easily form an ammine complex, which prevents complex formation between the hydantoin compound and silver ions. The pH value can be easily adjusted by adding an alkaline solution such as ammonia or sulfuric acid or an acid solution to the solution.
【００１９】尚、抽出溶媒と本発明において銀を含有す
る溶液とを接触させる際の両溶液の混合比（ｏｒｇａｎ
ｉｃ／Ａｑｕａ比：以下Ｏ／Ａ比という。）について
は、溶液中の銀の濃度、抽出溶媒中の抽出剤濃度により
異なるが、１：１０〜１０：１とするのが好ましい。When the extraction solvent is brought into contact with the solution containing silver in the present invention, the mixing ratio of both solutions (organic)
ic / Aqua ratio: hereinafter referred to as O / A ratio. ) Is different depending on the concentration of silver in the solution and the concentration of the extractant in the extraction solvent, but is preferably 1:10 to 10: 1.
【００２０】以上の本発明に係る方法によれば、銀と他
の金属とを含有する溶液から銀のみを選択的に抽出溶媒
相に抽出して銀を分離することができる。この本発明に
よる銀の選択的抽出作用は溶液中に含まれる他の金属が
上記従来技術で例として揚げたパラジウムである場合の
他、銅、ニッケル、タリウム等多くの金属であっても本
発明の効果を得ることができる。According to the above-described method of the present invention, silver can be separated from a solution containing silver and another metal by selectively extracting only silver into an extraction solvent phase. The selective extraction effect of silver according to the present invention is not limited to the case where the other metal contained in the solution is palladium fried as an example in the above-mentioned prior art, and even when many metals such as copper, nickel and thallium are used. The effect of can be obtained.
【００２１】そして、本発明においては、この抽出溶媒
中に分離した銀を如何に効率よく逆抽出して回収するか
も重要である。この抽出溶媒からの銀の回収方法として
は請求項４記載のように、請求項１〜請求項３記載の方
法により銀を選択抽出した抽出溶媒と、硝酸水溶液とを
接触させ銀を逆抽出するのが好ましい。In the present invention, it is also important how efficiently the back-extracted silver is recovered in the extraction solvent. As a method for recovering silver from the extraction solvent, as described in claim 4, silver is back-extracted by contacting an extraction solvent in which silver is selectively extracted by the method according to claim 1 with an aqueous nitric acid solution. Is preferred.
【００２２】この硝酸水溶液を用いることで、抽出溶媒
中の銀はほぼ１００％の収率で回収することができる。
また、硝酸水溶液は有機溶媒である抽出溶媒と容易に分
離できることからその作業も簡易である。従って、請求
項４記載の発明によれば、請求項１〜請求項３記載の発
明により高い抽出率で分離した銀をそのまま回収するこ
とができる。そしてその結果、本発明に係る銀の分離回
収方法は経済的にみても有利な方法であることいえる。By using this aqueous nitric acid solution, silver in the extraction solvent can be recovered with a yield of almost 100%.
Further, since the aqueous nitric acid solution can be easily separated from the extraction solvent which is an organic solvent, the operation is simple. Therefore, according to the invention of claim 4, silver separated at a high extraction rate by the invention of claims 1 to 3 can be recovered as it is. As a result, it can be said that the method for separating and recovering silver according to the present invention is economically advantageous.
【００２３】[0023]
【発明の実施の形態】以下、本発明の好適と思われる実
施形態について説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The preferred embodiments of the present invention will be described below.
【００２４】第１実施形態：本実施形態では、抽出剤と
して５，５−ジフェニルヒダントインとオクチルアルコ
−ルとを混合し、５，５−ジフェニルヒダントイン濃度
が１０ｍｍｏｌ／ｄｍ３である抽出溶媒を製造した。次
にこの抽出溶媒と、銀とパラジウムとをそれぞれ５０ｐ
ｐｍ含む１００ｍｍｏｌ／ｄｍ３の硝酸アンモニウム溶
液とを、Ｏ／Ａ比＝１：１の比率で接触、両者を３時間
振り混ぜ抽出溶媒液中に銀を選択抽出させた。この際、
銀とパラジウムとを含む硝酸アンモニウム溶液のｐＨは
アンモニア及び硫酸水溶液により適宜変更させ、ｐＨと
抽出率との関係も検討している。 First Embodiment : In this embodiment, 5,5-diphenylhydantoin is mixed with octyl alcohol as an extractant to produce an extraction solvent having a 5,5-diphenylhydantoin concentration of 10 mmol / dm 3. did. Next, this extraction solvent, silver and palladium were each added 50 p.
A 100 mmol / dm 3 ammonium nitrate solution containing pm was contacted at an O / A ratio of 1: 1, and both were shaken for 3 hours to selectively extract silver in the extraction solvent. On this occasion,
The pH of the ammonium nitrate solution containing silver and palladium is appropriately changed with an aqueous solution of ammonia and sulfuric acid, and the relationship between the pH and the extraction rate is also studied.
【００２５】第１実施形態における硝酸アンモニウム溶
液のｐＨと、抽出溶媒への銀及びパラジウムの抽出率と
の関係を図１に示す。図１では、縦軸に抽出率を、横軸
に硝酸アンモニウム溶液のｐＨをとり、各ｐＨの溶液か
ら抽出した銀及びパラジウムの抽出率をプロットしてい
る。尚、このときの銀の抽出率は、溶媒中の銀濃度をＩ
ＣＰ原子発光分光光度計で測定することにより求めてい
る。FIG. 1 shows the relationship between the pH of the ammonium nitrate solution and the extraction ratio of silver and palladium into the extraction solvent in the first embodiment. In FIG. 1, the extraction rate is plotted on the vertical axis and the pH of the ammonium nitrate solution is plotted on the horizontal axis, and the extraction rates of silver and palladium extracted from the solutions at each pH are plotted. The silver extraction rate at this time is determined by setting the silver concentration in the solvent to I
It is determined by measuring with a CP atomic emission spectrophotometer.
【００２６】図１から、本実施形態に係る抽出液は、パ
ラジウムよりも銀に対して高い選択性があることが確認
された。そして、この銀の抽出率はｐＨが５以上となっ
たときに上昇し、ｐＨ＝７近傍において最大となること
が判明した。From FIG. 1, it was confirmed that the extract of the present embodiment had higher selectivity for silver than for palladium. Then, it was found that the extraction ratio of silver increased when the pH became 5 or more, and became maximum near pH = 7.
【００２７】次に、溶媒相を混合相から分離し、この溶
媒相と１００ｍｍｏｌ／ｄｍ３の硝酸水溶液とをＯ／Ａ
比＝１：１の比率で接触させ、両者を２時間振り混ぜ、
水溶液中に銀を逆抽出させた。Next, the solvent phase was separated from the mixed phase, and this solvent phase and a 100 mmol / dm 3 nitric acid aqueous solution were mixed with O / A
Contact at a ratio of 1: 1 and shake both for 2 hours,
The silver was back-extracted into the aqueous solution.
【００２８】この際、抽出溶媒中の銀は、逆抽出前後の
溶媒中の銀濃度測定結果から１００％の収率で逆抽出で
きたことが確認された。At this time, it was confirmed from the measurement results of the silver concentration in the solvent before and after the back extraction that the silver in the extraction solvent could be back extracted with a yield of 100%.
【００２９】第２実施形態：本実施形態では、オクチル
アルコ−ルを希釈剤として、抽出剤である５，５−ジフ
ェニルヒダントイン濃度が５〜３０ｍｍｏｌ／ｄｍ３の
範囲内にある複数の抽出溶媒を調整し、これらの抽出溶
媒と、ｐＨ＝７に調整した銀とパラジウムとをそれぞれ
５０ｐｐｍ含む１００ｍｍｏｌ／ｄｍ３の硝酸アンモニ
ウム溶液とを、Ｏ／Ａ比＝１：１の比率で接触、両者を
３時間振り混ぜ抽出溶媒液中に銀を選択抽出させた。 Second Embodiment In this embodiment, octyl alcohol is used as a diluent, and a plurality of extraction solvents having an extractant concentration of 5,5-diphenylhydantoin in the range of 5 to 30 mmol / dm 3 are used. The extraction solvent was contacted with a 100 mmol / dm 3 ammonium nitrate solution containing 50 ppm each of silver and palladium adjusted to pH = 7 at an O / A ratio of 1: 1. Silver was selectively extracted into the extraction solvent by shaking.
【００３０】この際の、５，５−ジフェニルヒダントイ
ンの濃度による抽出率の変化を表１に示す。Table 1 shows the change in the extraction rate depending on the concentration of 5,5-diphenylhydantoin.
【００３１】[0031]
【表１】 [Table 1]
【００３２】表１より、銀の抽出率は、抽出溶媒中の
５，５−ジフェニルヒダントインの濃度の増加に伴い上
昇する傾向にあり、特に、５，５−ジフェニルヒダント
インの濃度が３０ｍｍｏｌ／ｄｍ３の場合、９９％にも
上ることがわかった。From Table 1, it can be seen that the extraction rate of silver tends to increase with an increase in the concentration of 5,5-diphenylhydantoin in the extraction solvent. In particular, the concentration of 5,5-diphenylhydantoin is 30 mmol / dm 3. In the case of, it was found that it was as high as 99%.
【００３３】この、第１及び第２実施形態の結果から、
水溶液中の銀濃度が５０ｐｐｍの場合において銀の抽出
率を１００％に極力近づける為には、抽出溶媒中の５，
５−ジフェニルヒダントインの濃度を３０ｍｍｏｌ／ｄ
ｍ３前後とすると共に、銀含有水溶液のｐＨを５〜７に
調整するのが適当であることが確認された。From the results of the first and second embodiments,
In the case where the silver concentration in the aqueous solution is 50 ppm, in order to bring the silver extraction rate as close to 100% as possible,
The concentration of 5-diphenylhydantoin is 30 mmol / d
m 3 with a longitudinal, it was confirmed that adjusting the pH of the silver-containing aqueous solution 5-7 is appropriate.
【００３４】比較例：トリオクチルアミンと燐酸トリブ
チルとをトルエンに溶解させ、トリオクチルアミンが
６．６７ｖｏｌ％、燐酸トリブチルが３．３３ｖｏｌ％
となるようにしたものを抽出溶媒として、パラジウムと
銀とをそれぞれ１００ｐｐｍ含む硝酸水溶液に接触させ
た。この際の、Ｏ／Ａ比は１：１としている。また、こ
の比較例では、硝酸濃度を変化させて複数のパラジウム
−銀含有硝酸溶液を準備し、硝酸濃度と抽出率との関係
を検討している。 Comparative Example : Trioctylamine and tributyl phosphate were dissolved in toluene, and 6.67% by volume of trioctylamine and 3.33% by volume of tributyl phosphate.
Was brought into contact with an aqueous nitric acid solution containing 100 ppm of palladium and 100 ppm of silver, respectively, as an extraction solvent. At this time, the O / A ratio is 1: 1. Further, in this comparative example, a plurality of palladium-silver-containing nitric acid solutions were prepared by changing the nitric acid concentration, and the relationship between the nitric acid concentration and the extraction rate was examined.
【００３５】図２は、各種硝酸濃度のパラジウム−銀含
有硝酸溶液と比較例の抽出溶媒とを接触させたときの、
抽出溶媒へのパラジウム及び銀の抽出率の変化を示した
ものである。この図２から、比較例の抽出溶媒において
は銀ではなくパラジウムに対して選択性を有するもので
あり、パラジウムの抽出率は硝酸濃度が１ｍｏｌ／ｄｍ
３以下において９０％以上と最大となっている。従っ
て、この比較例においてもパラジウムと銀との分離は可
能であるが、１％でも抽出率が異なれば溶液中にパラジ
ウムが多量含まれている場合、採取されるパラジウム量
にロスが生じるものと考えられる。FIG. 2 shows the results when the palladium-silver-containing nitric acid solutions having various nitric acid concentrations were brought into contact with the extraction solvent of the comparative example.
It is a figure which shows the change of the extraction rate of palladium and silver to an extraction solvent. From FIG. 2, the extraction solvent of the comparative example has selectivity for palladium instead of silver, and the extraction rate of palladium is 1 mol / dm3 of nitric acid concentration.
At 3 or less, the maximum is 90% or more. Therefore, even in this comparative example, palladium and silver can be separated, but if the extraction rate is different even at 1%, if the solution contains a large amount of palladium, the amount of palladium to be collected will be lost. Conceivable.
【００３６】[0036]
【発明の効果】以上説明したように本発明の銀の分離回
収方法は、銀に対する選択性の高い抽出剤を用いるもの
であり、銀と他の金属との混合物より銀を選択的に抽出
し、当該他の金属のロスなく高純度化を図ることができ
る。また、本発明によれば、上記手法により抽出した銀
も高い収率で回収することができる。As described above, the method for separating and recovering silver of the present invention uses an extractant having high selectivity for silver, and selectively extracts silver from a mixture of silver and another metal. Thus, high purity can be achieved without loss of the other metal. Further, according to the present invention, silver extracted by the above method can be recovered in a high yield.
【図１】第１実施形態における銀含有アンモニウム溶液
のｐＨと、抽出溶媒への銀及びパラジウムの抽出率との
関係を示す図。FIG. 1 is a diagram showing the relationship between the pH of a silver-containing ammonium solution and the extraction ratio of silver and palladium into an extraction solvent in a first embodiment.
【図２】比較例における各種硝酸濃度のパラジウム−銀
含有硝酸溶液と抽出溶媒とを接触させたときの、抽出溶
媒へのパラジウム及び銀の抽出率の変化を示す図。FIG. 2 is a graph showing changes in the extraction rates of palladium and silver into an extraction solvent when a palladium-silver-containing nitric acid solution having various nitric acid concentrations is brought into contact with an extraction solvent in a comparative example.
Claims (4)
ントイン化合物と化２で示される高級アルコールとを混
合してなる抽出溶媒とを接触させ、該抽出溶媒中に銀を
選択抽出させる銀の分離・回収方法。 【化１】 〔式中Ｒ１、Ｒ２はフェニル基、若しくは炭素数６以上
の直鎖又は側鎖を有するアルキル基、若しくは水素を示
す。〕 【化２】 〔式中Ｒ３は、炭素数８から１６の直鎖又は側鎖を有す
るアルキル基を示す。〕1. A silver-containing solution is brought into contact with an extraction solvent obtained by mixing a hydantoin compound represented by the chemical formula 1 with a higher alcohol represented by the chemical formula 2, and silver is selectively extracted into the extraction solvent. How to separate and collect silver. Embedded image [In the formula, R1 and R2 represent a phenyl group, an alkyl group having 6 or more carbon atoms having a straight or side chain, or hydrogen. [Chemical formula 2] [In the formula, R 3 represents an alkyl group having 8 to 16 carbon atoms and having a straight or side chain. ]
モニウムを添加する請求項１記載の銀の分離・回収方
法。2. The method for separating and recovering silver according to claim 1, wherein ammonium nitrate is added as a buffer to the solution containing silver.
として銀を抽出する請求項１又は請求項２記載の銀の分
離・回収方法。3. The pH value of the solution containing silver is 5-7.
3. The method for separating and recovering silver according to claim 1 or 2, wherein silver is extracted as the material.
選択抽出した抽出溶媒と、硝酸水溶液とを接触させ銀を
逆抽出する銀の分離・回収方法。4. A method for separating and recovering silver, wherein an extraction solvent in which silver is selectively extracted by the method according to claim 1 is brought into contact with an aqueous nitric acid solution to reversely extract silver.
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|---|---|---|---|
| JP33361999A JP4321929B2 (en) | 1999-11-25 | 1999-11-25 | Silver separation and recovery methods |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33361999A JP4321929B2 (en) | 1999-11-25 | 1999-11-25 | Silver separation and recovery methods |
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| Publication Number | Publication Date |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100713662B1 (en) * | 2005-10-20 | 2007-05-02 | 한국지질자원연구원 | Manufacturing Process of Sphere Shape Silver Powder from Silver Scrap |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100713662B1 (en) * | 2005-10-20 | 2007-05-02 | 한국지질자원연구원 | Manufacturing Process of Sphere Shape Silver Powder from Silver Scrap |
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