JPS62263938A - Separation of nickel ion from zinc ion - Google Patents
Separation of nickel ion from zinc ionInfo
- Publication number
- JPS62263938A JPS62263938A JP61105199A JP10519986A JPS62263938A JP S62263938 A JPS62263938 A JP S62263938A JP 61105199 A JP61105199 A JP 61105199A JP 10519986 A JP10519986 A JP 10519986A JP S62263938 A JPS62263938 A JP S62263938A
- Authority
- JP
- Japan
- Prior art keywords
- ions
- extractant
- contact
- hydroxyoxime
- acid
- 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.)
- Pending
Links
- 238000000926 separation method Methods 0.000 title claims abstract description 12
- 229910001453 nickel ion Inorganic materials 0.000 title claims description 14
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 title claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title description 61
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- -1 ester compounds Chemical class 0.000 claims abstract description 17
- 230000002378 acidificating effect Effects 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 11
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 25
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 13
- 229910019142 PO4 Inorganic materials 0.000 claims description 11
- 239000010452 phosphate Substances 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 235000011007 phosphoric acid Nutrition 0.000 claims description 3
- UHSURKDCQCGNGM-UHFFFAOYSA-N 5-(2-hydroxyimino-2-phenylethyl)nonan-2-ol Chemical compound CCCCC(CCC(C)O)CC(=NO)C1=CC=CC=C1 UHSURKDCQCGNGM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 40
- 239000011701 zinc Substances 0.000 description 36
- 238000000605 extraction Methods 0.000 description 15
- 229910052759 nickel Inorganic materials 0.000 description 14
- 229910052725 zinc Inorganic materials 0.000 description 13
- 238000007747 plating Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 description 3
- 239000003350 kerosene Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- APRJFNLVTJWEPP-UHFFFAOYSA-N Diethylcarbamic acid Chemical compound CCN(CC)C(O)=O APRJFNLVTJWEPP-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- LLYOXZQVOKALCD-UHFFFAOYSA-N chembl1400298 Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC1=CC=CC=N1 LLYOXZQVOKALCD-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000005246 galvanizing Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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
【発明の詳細な説明】
［産業上の利用分野］
本発明はニッケルイオンと亜鉛イオンとの分離方法に係
り、特にニッケルイオンと亜鉛イオンとを含む液から、
ニッケルイオンのみを選択的に高効率で分離回収する方
法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for separating nickel ions and zinc ions from a liquid containing nickel ions and zinc ions.
This invention relates to a method for selectively separating and recovering only nickel ions with high efficiency.
［従来の技術］
ニッケル（Ｎｉ）イオン及び亜鉛（Ｚ ｎ）イオンの混
在する液中から、Ｎｉイオンを分離する技術が、メッキ
分野、製錬分野等において必要とされている。[Prior Art] A technique for separating Ni ions from a liquid containing nickel (Ni) ions and zinc (Zn) ions is needed in the plating field, smelting field, and the like.
例えば、亜鉛メッキ工程において、メッキ浴中にはＺｎ
、正リン酸の他に金属基材から持ち込まれるＮｉが共存
しているが、このＮｉ濃度が１１００ｐｐを超えて多量
に含まれるようになると、メッキ浴として使用できなく
なり、メッキ廃液として処理しなければならなくなる。For example, in the galvanizing process, Zn is present in the plating bath.
In addition to orthophosphoric acid, Ni brought in from the metal base material coexists, but when the Ni concentration exceeds 1100 pp and it becomes contained in large quantities, it can no longer be used as a plating bath and must be treated as plating waste liquid. It will stop happening.
しかしながら、このようなＮｉ濃度の高くなったメッキ
浴を廃液として処理するには、処理コストがかかるうえ
に有価金属の廃棄につながり、経済的に不利である。こ
のため、ＮｉとＺｎの共存するメッキ浴中からＮｉのみ
を除去することにより、メッキ浴の再使用を図ることが
必要となる。However, treating such a plating bath with a high Ni concentration as a waste solution is economically disadvantageous because it not only increases processing costs but also leads to waste of valuable metals. Therefore, it is necessary to reuse the plating bath by removing only Ni from the plating bath in which Ni and Zn coexist.
その他、ＮｉやＣＯの製錬工程等においても、Ｎｉと少
量のＺｎを含む浸出液が排出され、これらの液中からＮ
ｉイオンのみを選択的に除去することが必要とされる場
合がある。In addition, in the smelting process of Ni and CO, leachate containing Ni and a small amount of Zn is discharged, and N is extracted from these liquids.
It may be necessary to selectively remove only i-ions.
従来、Ｎｉを溶媒抽出法により分離する方法として、下
記■〜■に挙げるジメチルグリオキシム法（ＪＩＳ
Ｋ０１０２−１９７１）、ジエチルジチオカルバミン酸
法、ＰＡＮ法等が知られている。Conventionally, as a method for separating Ni by solvent extraction, the dimethylglyoxime method (JIS
K0102-1971), diethyldithiocarbamic acid method, PAN method, etc. are known.
■ ジメチルグリオキシム法二 Ｎｉを含むアルカリ性
溶液にジメチルグリオキシムを加えてＮｉ錯体とし、ク
ロロホルムで抽出したあと、逆抽出する方法。■ Dimethylglyoxime method 2 A method in which dimethylglyoxime is added to an alkaline solution containing Ni to form a Ni complex, extracted with chloroform, and then back-extracted.
■ ジエチルカルバミン酸法： 弱アンモニアアルカリ
性でＮｉのジエチルカルバミン酸の錯体を得、これをイ
ソアミルアルコールで抽出する。■ Diethylcarbamic acid method: A complex of Ni and diethylcarbamic acid is obtained under weak ammonia alkalinity, and this is extracted with isoamyl alcohol.
■ ＰＡＮ （１−（２−ピリジルアゾ）−２−ナフト
ール）法： ＰＡＮはｐＨ４〜ｌＯでＮ１（ＩＩ）と
赤色錯体を生成し、沈殿するので、この沈殿をクロロホ
ルム等の有機溶媒で抽出する。(2) PAN (1-(2-pyridylazo)-2-naphthol) method: PAN forms a red complex with N1(II) at pH 4 to 1O and precipitates, so this precipitate is extracted with an organic solvent such as chloroform.
これら■〜■の方法は、Ｎｉの分析法として従来より公
知のものである（日本化学会編＝ 「新実験化学講座分
析化学［Ｉ］Ｊ 、３４８．丸善（１９７２））。These methods (1) to (2) are conventionally known methods for analyzing Ni (edited by the Chemical Society of Japan, New Experimental Chemistry Course Analytical Chemistry [I]J, 348. Maruzen (1972)).
［発明が解決しようとする問題点］
しかしながら、ｈ記■〜■の方法に用いられる試薬は高
価である上に、水溶性のため一度しか使用することがで
きず、処理コストが高くつくという問題点がある。[Problems to be Solved by the Invention] However, the reagents used in the methods described in Sections 1 to 2 are expensive, and because they are water-soluble, they can only be used once, resulting in high processing costs. There is a point.
［問題点を解決するための手段］
本発明は、ＮｉとＺｎとを含む液からＮｉのみを低コス
トかつ高効率で分離回収する方法を提供するものであっ
て、
ニッケルイオン及び亜鉛イオンを含む液とヒドロキシオ
キシム系化合物及び／又は酸性リン酸エステル系化合物
を含む抽出剤とを接触Ｓせた後、前記抽出剤を酸と接触
させてニッケルイオンを分離することを特徴とするニッ
ケルイオンと亜鉛イオンとの分離方法、
を要旨とするものである。[Means for Solving the Problems] The present invention provides a method for separating and recovering only Ni from a liquid containing Ni and Zn at low cost and with high efficiency, and which includes Ni and Zn ions. Nickel ions and zinc, characterized in that the liquid is brought into contact with an extractant containing a hydroxyoxime compound and/or an acidic phosphate ester compound, and then the extractant is brought into contact with an acid to separate nickel ions. The gist of this paper is a method for separating ions.
従来、ＣＯとＮｉとの分離にリン酸エステルを使用する
方法（特公昭６Ｏ−２１２１１）、オキシムを使用する
方法（特公昭６Ｏ−２６０４９）は提案されている。し
かしながら、これらはいずれもＣｏとＮｉとの分離につ
いてであり、ＮｉとＺｎとの分離については何ら示唆さ
れていない。Conventionally, a method using a phosphoric acid ester (Japanese Patent Publication No. 6O-21211) and a method using an oxime (Japanese Patent Publication No. 6O-26049) have been proposed for separating CO and Ni. However, these are all about the separation of Co and Ni, and there is no suggestion about the separation of Ni and Zn.
これに対し、本発明者らは、ＮｉとＺｎとを含む液をヒ
ドロキシオキシム系化合物及び／又は酸性リン酸エステ
ル系化合物で抽出すると高抽出率でＮｉが若干量のＺｎ
と共に抽出され、Ｎｉ及びＺｎを含む抽出剤を酸と接触
させることにより、Ｎｉのみが選択的に逆抽出され、Ｎ
ｉの分離回収が可能となることを見出し、本発明を完成
させたものである。On the other hand, the present inventors have found that when a liquid containing Ni and Zn is extracted with a hydroxyoxime compound and/or an acidic phosphate compound, the extraction rate is high and Ni is extracted from a small amount of Zn.
By contacting an extractant containing Ni and Zn with acid, only Ni is selectively back-extracted, and N
The present invention was completed based on the discovery that it is possible to separate and recover i.
以下に本発明につき詳細に説明する。The present invention will be explained in detail below.
本発明の処理対象となるＮｉイオン及びＺｎイオンを含
む液としては、正リン酸が共存するメッキ廃液が挙げら
れ、そのＰＨは４〜５であることが好ましい。Examples of the liquid containing Ni ions and Zn ions to be treated in the present invention include plating waste liquid in which orthophosphoric acid coexists, and the pH thereof is preferably 4 to 5.
本発明においては、このようなＮｉイオンとＺｎイオン
とを含む液をヒドロキシオキシム系化合物及び／又は酸
性リン酸エステル系化合物を含む抽出剤と接触させる。In the present invention, a liquid containing such Ni ions and Zn ions is brought into contact with an extractant containing a hydroxyoxime compound and/or an acidic phosphate compound.
ヒドロキシオキシム系化合物としては、一般式で示され
る化合物が挙げられ、具体的にはＲ１＝Ｃ５）（＋９．
Ｒ２＝ＣＨ３の２−ヒドロキシ−５−ノニルアセトフェ
ノンオキシム（以下、ｒＨＮＡＦＯＩと略称することが
ある。）が好ましい。Examples of hydroxyoxime compounds include compounds represented by the general formula, specifically R1=C5)(+9.
2-hydroxy-5-nonylacetophenone oxime (hereinafter sometimes abbreviated as rHNAFOI) where R2=CH3 is preferred.
また、酸性リン酸エステル系化合物としては、リン酸ジ
−２−エチルヘキシル、リン酸ブチル等の有機リン酸エ
ステルが挙げられ、これのうち、で示されるリン酸ジ−
２−エチルヘキシル（以下、ｒ Ｄ ２ Ｅ ＨＰ Ａ
Ｊと略称することがある。）が好ましい。Examples of acidic phosphate ester compounds include organic phosphoric esters such as di-2-ethylhexyl phosphate and butyl phosphate.
2-ethylhexyl (r D 2 E HP A
It is sometimes abbreviated as J. ) is preferred.
これらヒドロキシオキシム系化合物及び／又は酸性リン
酸エステル系化合物を含む抽出剤と接触させることによ
り、被処理液中のＮｉイオンとＺｎイオンは抽出剤中に
抽出される。By contacting with an extractant containing these hydroxyoxime compounds and/or acidic phosphate ester compounds, Ni ions and Zn ions in the liquid to be treated are extracted into the extractant.
この場合、抽出剤としてヒドロキシオキシム系化合物を
用いると、Ｎｉイオンは高い抽出効率で抽出されるのに
対し、Ｚｎイオンの抽出率は３０％以下と低いことから
、Ｚｎによる抽出剤の汚染が少なく、極めて有利である
。In this case, when a hydroxyoxime compound is used as an extractant, Ni ions are extracted with high extraction efficiency, but the extraction rate of Zn ions is low at less than 30%, so the contamination of the extractant by Zn is small. , is extremely advantageous.
このようにして、ＮｉイオンとＺｎイオンとを抽出して
含有する抽出剤は、次いで酸水溶液と接触させることに
より、Ｎｉイオンのみを選択的に逆抽出する。逆抽出剤
として使用される酸としては、Ｈ２Ｓ ０４ 、 ＨＣ
見、ＨＮ Ｏａ等が挙げられ、そのＰＨは高過ぎるとＮ
ｉの逆抽出率が低く、低過ぎるとＺｎも逆抽出され、Ｎ
ｔの選択率が低下するこ、とから、一般にはｐＨ１〜４
とするのが好ましい。特に、抽出剤としてヒドロキシオ
キシム系化合物を用いる場合には、逆抽出剤のＰＨは２
以下、また抽出剤として酸性リン酸エステル系化合物を
用いる場合には、逆抽出剤のｐＨは１．５〜３．５とす
るのが好ましい。The extractant that extracts and contains Ni ions and Zn ions in this way is then brought into contact with an acid aqueous solution to selectively back-extract only Ni ions. Acids used as back extractants include H2S04, HC
However, if the pH is too high, N
If the back extraction rate of i is low and too low, Zn will also be back extracted and N
Generally, the pH is 1 to 4 because the selectivity of t decreases.
It is preferable that In particular, when using a hydroxyoxime compound as an extractant, the pH of the back extractant is 2.
Hereinafter, when an acidic phosphate ester compound is used as an extractant, the pH of the back extractant is preferably 1.5 to 3.5.
このようにして逆抽出剤中に選択逆抽出分離されたＮｉ
イオンは、逆抽出剤のＰＨが低いことから、逆抽出剤中
にＮｉを高濃縮して晶析回収するなどの方法により、容
易に回収することができる。In this way, Ni was selectively separated into the back extractant.
Since the pH of the back-extracting agent is low, the ions can be easily recovered by a method such as highly concentrating Ni in the back-extracting agent and recovering the ions by crystallization.
なお、本発明において、抽出剤の繰り返し使用によりＺ
ｎイオンが蓄積すると、抽出剤の抽出性能はＺｎイオン
量に比例して劣化するものと推定される。In addition, in the present invention, by repeatedly using the extractant, Z
It is estimated that when n ions accumulate, the extraction performance of the extractant deteriorates in proportion to the amount of Zn ions.
このため、必要に応じて抽出剤中のＺｎイオンを除去す
ることが好ましく、Ｚｎイオンの除去方法としては、
■ 抽出剤を濃厚な酸性溶液と接触させることにより洗
節する。For this reason, it is preferable to remove Zn ions in the extractant if necessary, and methods for removing Zn ions include: (1) Washing by bringing the extractant into contact with a concentrated acidic solution.
■ 抽出剤をＮｉを含有した濃厚な酸性溶液と接触させ
ることにより洗浄する。即ち、Ｚｎが除去しにくい場合
にはＮｉとイオン交換させることにより除去する。■ Cleaning the extractant by contacting it with a concentrated acidic solution containing Ni. That is, when Zn is difficult to remove, it is removed by ion exchange with Ni.
方法が挙げられる。There are several methods.
［作用１
本発明の分離方法においては、まず、ヒドロキシオキシ
ム系化合物及び／又は酸性リン酸エステル系化合物を含
む抽出剤中に、Ｎｉイオン及びＺｎイオンが抽出される
。しかして、これらを含む抽出剤を酸逆抽出剤と接触さ
せることにより、Ｎｉイオンのみが選択的に逆抽出され
るため。[Effect 1] In the separation method of the present invention, first, Ni ions and Zn ions are extracted into an extractant containing a hydroxyoxime compound and/or an acidic phosphate ester compound. Therefore, by bringing an extractant containing these into contact with an acid back-extracting agent, only Ni ions are selectively back-extracted.
ＮｉイオンとＺｎイオンとの分離が可能とされる。It is possible to separate Ni ions and Zn ions.
［実施例］
以下に実施例及び比較例を挙げて、本発明をより具体的
に説明するが、本発明はその要旨を超えない限り、以下
の実施例に限定されるものではない。[Examples] The present invention will be described in more detail with reference to Examples and Comparative Examples below, but the present invention is not limited to the following Examples unless it exceeds the gist thereof.
実施例ｌ
Ｎｉ１３０ｍｇ／ｕ、Ｚ ｎ ４６０ ｍ ｇ ／ ｎ
を含む水溶液２５０ｍ１に、抽出剤としてＤ ２ Ｅ
ＨＰ Ａ ２０％ケロシン溶液５００ｍＪ１を加え、Ｎ
ａＯＨ溶液でｐＨ＝５に調整した後、５分間振藻し、２
時間静置して、各相を分析した。Example 1 Ni 130 mg/u, Z n 460 mg/n
D 2 E as an extractant to 250 ml of an aqueous solution containing
Add 500 mJ1 of HP A 20% kerosene solution and
After adjusting the pH to 5 with aOH solution, shake the algae for 5 minutes,
Each phase was analyzed after standing for a period of time.
その結果、水相のＮｉは３．４ｍｇ／Ｍ、Ｚｎは０．４
ｍｇ／交となり、抽出剤中にはＮｉ６３ｍｇ／ｆｌ、Ｚ
ｎ２３０ｍｇ／ｉが抽出されていた。As a result, Ni in the aqueous phase was 3.4 mg/M, and Zn was 0.4 mg/M.
mg/fl, and the extractant contains 63 mg/fl of Ni and Z
n230mg/i was extracted.
次いで、Ｎｉ及びＺｎを抽出した抽出剤２５ｍμと第１
表に示す濃度のＨ２Ｓ Ｏ４逆抽出剤（Ｈ２ｓｏ、ｔを
蒸留水で希釈したもの）２５ｍＭとを第１表に示す処理
ｐＨで振薔した後、２時間静置して、逆抽出剤中のＮｉ
、Ｚｎの各濃度を測定し、逆抽出率（（逆抽出剤中のＮ
ｉ又はＺｎ濃度／抽出剤中のＮｉ又はＺｎ濃度）Ｘ１０
０）を求めた結果を第１表に示す。Next, 25 mμ of the extractant that extracted Ni and Zn and the first
After shaking 25mM of H2S O4 back extractant (H2SO, t diluted with distilled water) at the concentration shown in the table at the treatment pH shown in Table 1, it was left to stand for 2 hours. Ni
, each concentration of Zn was measured, and the back extraction rate ((N in the back extractant) was measured.
i or Zn concentration/Ni or Zn concentration in extractant)X10
0) are shown in Table 1.
第 １ 表
第１表より明らかなように、特にｐＨ１，５〜３．５の
範囲において、Ｎｉのみ逆抽出され、Ｚｎは殆ど逆抽出
されず、Ｎｉの良好な選択的逆抽出が可能である。Table 1 As is clear from Table 1, particularly in the pH range of 1.5 to 3.5, only Ni is back-extracted and almost no Zn is back-extracted, making it possible to perform good selective back-extraction of Ni. .
実施例２
抽出剤として、ＨＮＡＦＯ（ＳＭＥ５２９（シェル化学
製））２０％ケロシン溶液を用いたこと以外は実施例１
と同様にして抽出を行なった。Example 2 Example 1 except that HNAFO (SME529 (manufactured by Shell Chemical)) 20% kerosene solution was used as the extractant.
Extraction was carried out in the same manner.
その結果、水相ｃ７）Ｎｉは１８．１ｍｇ／ｉ、Ｚｎは
４０５ｍｇ／文となり、抽出剤中にはＮｉ５６、Ｏｍｇ
／ｕ、Ｚｎ２７．５ｍｇ／ｕが抽出Ｓれていた。As a result, the aqueous phase c7) Ni was 18.1 mg/i, Zn was 405 mg/i, and the extractant contained 56 and 0 mg of Ni.
/u, Zn27.5mg/u was extracted.
次いで、このＮｉ及びＺｎを抽出した抽出剤２５ｍＭと
第２表に示すＨ２ＳＯ４濃度の逆抽出剤（Ｈ２ＳＯ４を
蒸留水で希釈したもの）２５ｍＭとを第２表に示す処理
ｐＨで、振蓋し、実施例１と同様にしてＮｉ及びＺｎの
逆抽出量及び逆抽出率を求めた。Next, 25mM of the extractant used to extract Ni and Zn and 25mM of the back extractant (H2SO4 diluted with distilled water) with the H2SO4 concentration shown in Table 2 were shaken at the treatment pH shown in Table 2, The back extraction amount and back extraction rate of Ni and Zn were determined in the same manner as in Example 1.
結果を第２表に示す。The results are shown in Table 2.
第２表より明らかなように、特にｐＨ２以下において、
Ｎｉの良好な選択的逆抽出が可能である。As is clear from Table 2, especially at pH 2 or below,
Good selective back extraction of Ni is possible.
第 ２ 表
比較例１
抽出剤として第３表に示す化合物の２０％濃度ケロシン
溶液を用いたこと以外は、実施例１と同様にして抽出を
行ない、水相を分析した。Table 2 Comparative Example 1 Extraction was carried out in the same manner as in Example 1, except that a 20% concentration kerosene solution of the compounds shown in Table 3 was used as the extractant, and the aqueous phase was analyzed.
結果を第３表に示す。The results are shown in Table 3.
第３表より、比較例で用いた化合物はいずれもＮｉの抽
出率が低く、一方Ｚｎの抽出率が高く、Ｎｉの分離除去
には不適であることが明らかである。From Table 3, it is clear that all the compounds used in the comparative examples have a low extraction rate of Ni, while a high extraction rate of Zn, and are therefore unsuitable for separating and removing Ni.
第３表
才ｌ ： トリーＮ−オクチルアミン
ｔ２ニジエル化学製
（Ｒ’ 、Ｒ“は合計の炭素数が７であるようなアルキ
ル基を示す。）
求３： リン酸トリブチル
＊４：イソプロピルエーテル
［発明の効果］
以上詳述した通り、本発明のＮｉイオンとＺｎイオンと
の分離方法は、Ｎｉイオン及びＺｎイオンを含む液をヒ
ドロキシオキシム系化合物及び／又は酸性リン酸エステ
ル系化合物を含む抽出剤で抽出した後、Ｎｉイオンのみ
を選択的に酸で逆抽出するものであって、
■ 使用する試薬は工業的に市販されている安価なもの
である。3rd expression: Tri-N-octylamine t2 manufactured by Nisiel Chemical (R', R'' represents an alkyl group having a total number of carbon atoms of 7.) Request 3: Tributyl phosphate*4: Isopropyl ether [ [Effects of the Invention] As detailed above, the method for separating Ni ions and Zn ions of the present invention is such that a liquid containing Ni ions and Zn ions is treated with an extractant containing a hydroxyoxime compound and/or an acidic phosphate ester compound. After extraction, only Ni ions are selectively back-extracted with acid. (2) The reagents used are commercially available and inexpensive ones.
■ しかも、抽出剤、逆抽出剤は繰り返し使用すること
が可能である。■ Furthermore, the extractant and back-extractant can be used repeatedly.
■ 処理操作は極めて容易である。■ Processing operations are extremely easy.
■ 逆抽出剤からのＮｉの回収も容易である。■ Recovery of Ni from the back-extracting agent is also easy.
等の利点を有する。It has the following advantages.
従って、本発明によれば、Ｎｉイオン及びＺｎイオンを
含む液から、Ｎｉイオンのみを低コストで効率的に分離
除去することができ、工業的、経済的に極めて有利であ
る。Therefore, according to the present invention, only Ni ions can be efficiently separated and removed from a liquid containing Ni ions and Zn ions at low cost, which is extremely advantageous industrially and economically.
Claims (7)
キシオキシム系化合物及び／又は酸性リン酸エステル系
化合物を含む抽出剤とを接触させた後、前記抽出剤を酸
と接触させてニッケルイオンを分離することを特徴とす
るニッケルイオンと亜鉛イオンとの分離方法。(1) After bringing a liquid containing nickel ions and zinc ions into contact with an extractant containing a hydroxyoxime compound and/or an acidic phosphate ester compound, the extractant is brought into contact with an acid to separate the nickel ions. A method for separating nickel ions and zinc ions, characterized by the following.
化学式、表等があります▼ ［ただし、式中、Ｒ＿１は炭素数１〜１２のアルキル基
、Ｒ＿２は炭素数１〜１０のアルキル基を示す。］ で示される化合物であることを特徴とする特許請求の範
囲第１項に記載の分離方法。(2) The hydroxyoxime compound has the general formula ▲ mathematical formula,
Chemical formulas, tables, etc. are available▼ [However, in the formula, R_1 represents an alkyl group having 1 to 12 carbon atoms, and R_2 represents an alkyl group having 1 to 10 carbon atoms. ] The separation method according to claim 1, which is a compound represented by the following.
−５−ノニルアセトフェノンオキシムであることを特徴
とする特許請求の範囲第２項に記載の分離方法。(3) The separation method according to claim 2, wherein the hydroxyoxime compound is 2-hydroxy-5-nonylacetophenone oxime.
エチルヘキシルであることを特徴とする特許請求の範囲
第１項ないし第３項に記載の分離方法。(4) Acidic phosphate ester compound is di-2-phosphoric acid
The separation method according to any one of claims 1 to 3, characterized in that ethylhexyl is used.
ン酸が共存する液であることを特徴とする特許請求の範
囲第１項ないし第４項のいずれか１項に記載の分離方法
。(5) The separation method according to any one of claims 1 to 4, wherein the liquid containing nickel ions and zinc ions is a liquid in which orthophosphoric acid coexists.
キシオキシム系化合物を含む抽出剤とを接触させた後、
前記抽出剤をｐＨ２以下の酸と接触させてニッケルイオ
ンを分離することを特徴とする特許請求の範囲第１項に
記載の分離方法。(6) After bringing the liquid containing nickel ions and zinc ions into contact with the extractant containing a hydroxyoxime compound,
2. The separation method according to claim 1, wherein nickel ions are separated by bringing the extractant into contact with an acid having a pH of 2 or less.
ン酸エステル系化合物を含む抽出剤とを接触させた後、
前記抽出剤をｐＨ１〜４の酸と接触させてニッケルイオ
ンを分離することを特徴とする特許請求の範囲第１項に
記載の分離方法。(7) After bringing the liquid containing nickel ions and zinc ions into contact with the extractant containing an acidic phosphate ester compound,
2. The separation method according to claim 1, wherein nickel ions are separated by bringing the extractant into contact with an acid having a pH of 1 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61105199A JPS62263938A (en) | 1986-05-08 | 1986-05-08 | Separation of nickel ion from zinc ion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61105199A JPS62263938A (en) | 1986-05-08 | 1986-05-08 | Separation of nickel ion from zinc ion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62263938A true JPS62263938A (en) | 1987-11-16 |
Family
ID=14400995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61105199A Pending JPS62263938A (en) | 1986-05-08 | 1986-05-08 | Separation of nickel ion from zinc ion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62263938A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005256170A (en) * | 2004-02-12 | 2005-09-22 | National Institute Of Advanced Industrial & Technology | Electroless nickel plating method and plated product thereby |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5438970A (en) * | 1977-08-31 | 1979-03-24 | Toray Industries | Operating of weaving machine without weft yarn wound tube |
| JPS6021211A (en) * | 1983-07-16 | 1985-02-02 | Shozo Miura | Manufacture of hanger having hook part |
| JPS6133046A (en) * | 1984-07-25 | 1986-02-15 | コ−デツクス・コ−ポレ−シヨン | Network forming circuit |
-
1986
- 1986-05-08 JP JP61105199A patent/JPS62263938A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5438970A (en) * | 1977-08-31 | 1979-03-24 | Toray Industries | Operating of weaving machine without weft yarn wound tube |
| JPS6021211A (en) * | 1983-07-16 | 1985-02-02 | Shozo Miura | Manufacture of hanger having hook part |
| JPS6133046A (en) * | 1984-07-25 | 1986-02-15 | コ−デツクス・コ−ポレ−シヨン | Network forming circuit |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005256170A (en) * | 2004-02-12 | 2005-09-22 | National Institute Of Advanced Industrial & Technology | Electroless nickel plating method and plated product thereby |
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