JPS5924169B2 - Selective separation method for indium - Google Patents
Selective separation method for indiumInfo
- Publication number
- JPS5924169B2 JPS5924169B2 JP54057022A JP5702279A JPS5924169B2 JP S5924169 B2 JPS5924169 B2 JP S5924169B2 JP 54057022 A JP54057022 A JP 54057022A JP 5702279 A JP5702279 A JP 5702279A JP S5924169 B2 JPS5924169 B2 JP S5924169B2
- Authority
- JP
- Japan
- Prior art keywords
- indium
- extraction
- extractant
- separation method
- organic solvent
- 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
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
Description
【発明の詳細な説明】
本発明は、インジウムと各種金属を含む溶液からインジ
ウムを選択的に抽出する方法に関するものであり、特に
は亜鉛および鉛の製錬工程における煙灰、各種残滓等の
浸出液から溶媒抽出法によってインジウムを選択的に抽
出する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for selectively extracting indium from a solution containing indium and various metals, particularly from leachates such as smoke ash and various residues from the zinc and lead smelting process. The present invention relates to a method for selectively extracting indium using a solvent extraction method.
亜鉛及び鉛の製錬工程において生ずる煙灰、陽極スライ
ム等の各種残査、電解排液等には微量のインジウムが含
まれており、近年これからインジウムを回収する試みが
為されている。Trace amounts of indium are contained in various residues such as smoke ash, anode slime, and electrolytic waste generated in the zinc and lead smelting process, and attempts have been made in recent years to recover indium.
インジウムの分離方法としては、硫化物あるいは水酸化
物の形で沈殿させる方法や置換析出反応（セメンチージ
ョン）を利用する方法がある。Methods for separating indium include a method of precipitating it in the form of sulfide or hydroxide, and a method of utilizing displacement precipitation reaction (cementation).
前者は沈殿物の存在のため処理操作が複雑で面倒となり
、インジウムと他金属との分離が良好でなく、他方後者
の方法も置換用に使用される亜鉛、カドミウムおよびア
ルミニウム等より責な金属がインジウムと共に存在して
いる場合にはそれら金属との分離がなしえない。The former method requires complicated and troublesome treatment operations due to the presence of precipitates, and the separation of indium from other metals is not good.On the other hand, the latter method also has problems with metals that are more responsible than those used for replacement, such as zinc, cadmium, and aluminum. If it exists together with indium, it cannot be separated from those metals.
これら方法とは別に、溶媒抽出法として知られる方法が
ある。Apart from these methods, there is a method known as solvent extraction.
溶媒抽出法は、インジウムを選択的に抽出しうる抽出剤
を含む有機溶媒を使用してインジウム含有水溶液からイ
ンジウムを分離するものである。The solvent extraction method separates indium from an indium-containing aqueous solution using an organic solvent containing an extractant that can selectively extract indium.
抽出剤の選定に当っては、抽出剤かインジウム含有水溶
液と混らないことおよび水溶液からインジウムイオンの
みを選択的にしかも効率的に抽出しうる性能を具備して
いることが考慮されねばならない。When selecting an extractant, it must be considered that the extractant does not mix with the indium-containing aqueous solution and has the ability to selectively and efficiently extract only indium ions from the aqueous solution.
更に、抽出剤はその粘性を低下せしめ、抽出剤の分散を
良くし、そして抽出剤の接触効率を大きくするために希
釈剤で薄めて使用するのが一般的であるため、希釈剤に
よく溶けることも必要である。Furthermore, the extractant is generally diluted with a diluent to reduce its viscosity, improve the dispersion of the extractant, and increase the contact efficiency of the extractant, so it dissolves well in the diluent. It is also necessary.
加えて、抽出操作後進抽出が行われるので、逆抽出操作
を容易に行わしめることも必要である。In addition, since the extraction operation is backward extraction, it is also necessary to easily perform the reverse extraction operation.
インジウム溶媒抽出剤については、燐酸ジ２−エチルヘ
キシルエステルがインジウムの選択的抽出にきわめて秀
れていることが知られている。Regarding indium solvent extractants, it is known that di-2-ethylhexyl phosphate is extremely effective in selectively extracting indium.
上記抽出剤はインジウムに対する選択性にきわめて秀れ
、条件を適正に選ぶことによりインジウムを９８％以上
抽出しうる。The above extractant has excellent selectivity for indium, and by appropriately selecting conditions, it is possible to extract 98% or more of indium.
しかし、インジウムを抽出剤として使用した場合逆抽出
操作を効果的に行う方法が確立されておらず、それが上
記試薬を使用してのインジウム溶媒抽出法のネックとな
っていた。However, when indium is used as an extractant, no method has been established to effectively carry out the back-extraction operation, which has been a bottleneck for the indium solvent extraction method using the above-mentioned reagent.
本発明者は塩酸を使用しての逆抽出操作がきわめて有効
であることを知見した。The present inventor has found that back extraction using hydrochloric acid is extremely effective.
特に、塩酸を用いての逆抽出操作は３０〜７０℃の昇温
下において実施すると効果的であることが判明した。In particular, it has been found that the back extraction operation using hydrochloric acid is effective when carried out at an elevated temperature of 30 to 70°C.
逆抽出温度は逆抽出効率に大きな影警を与え、昇温下で
は低濃度の塩酸を使用した場合でもきわめて高い逆抽出
効率を実現しうる。The back extraction temperature has a great influence on the back extraction efficiency, and at elevated temperatures, extremely high back extraction efficiency can be achieved even when using low concentration hydrochloric acid.
本発明は、硫酸酸性のインジウムおよびその他の金属を
含む溶液を燐酸ジ２−エチルヘキシルエステルを抽出剤
として含む有機溶媒とｐＨ１，０以下で接触しそしてイ
ンジウムを含有する抽出後溶媒を塩酸で３０〜７０℃の
温度において逆抽出することから成るインジウムの選択
分離方法を提供する。The present invention involves contacting a solution containing indium and other metals acidified with sulfuric acid with an organic solvent containing di-2-ethylhexyl phosphate as an extractant at a pH of 1.0 or less, and then extracting the indium-containing solvent with hydrochloric acid for 30 to 30 mL. A method for the selective separation of indium is provided, comprising back extraction at a temperature of 70°C.
以下、本発明について具体的に説明する。The present invention will be explained in detail below.
前述した亜鉛および鉛の各種製錬副産物の浸出液は、１
．０ｊｉ７１１以下のインジウムの他にクリラム、カド
ミウム、亜鉛、砒素、鉄、マンガン等の各種金属イオン
を含んでいる。The leachate of various zinc and lead smelting by-products mentioned above is 1
．． In addition to indium of 0ji711 or less, it contains various metal ions such as chlorine, cadmium, zinc, arsenic, iron, and manganese.
これら多数の金属イオン含有溶液からインジウムの選択
的抽出には、ｐ Ｈ１，０以下の硫酸酸性下において、
燐酸ジ２−エチルヘキシルエステルを抽出剤として含む
有機溶媒がきわめて秀れた効果を発揮する。To selectively extract indium from these solutions containing a large number of metal ions, under acidic sulfuric acid with a pH of 1.0 or less,
An organic solvent containing di-2-ethylhexyl phosphoric acid ester as an extractant exhibits excellent effects.
燐酸ジ２−エチルヘキシルエステルは下記の構造式を持
つ：
前述した理由により上記抽出剤は鉱油、鉱油にアルコー
ルを加えたもの、トルエン等のような希釈剤で希釈して
使用するのが通例である。Phosphoric acid di-2-ethylhexyl ester has the following structural formula: For the reasons mentioned above, the above extractant is usually used by diluting it with a diluent such as mineral oil, a mixture of mineral oil and alcohol, or toluene. .
希釈度は３〜５０容量％程度である。The degree of dilution is about 3 to 50% by volume.
本発明の対象とするインジウムおよびその他の金属を含
む硫酸酸性溶液からインジウムを選択分離するためには
ｐＨが１．０以下であることが重要である。In order to selectively separate indium from an acidic sulfuric acid solution containing indium and other metals, which is the object of the present invention, it is important that the pH is 1.0 or less.
インジウム含有量は１９／ｌ以下の低い値から３０９７
１前後の高い値まで処理可能である。Indium content ranges from as low as 19/l to 3097
It is possible to process up to a high value around 1.
インジウム含有硫酸酸性溶液と抽出剤を含む有機溶媒と
の接触は、周知のミキサーセトラー設備、抽出塔、遠心
抽出機等を使用してバッチ式でも連続式でも行いうる。The contact between the indium-containing sulfuric acid acidic solution and the organic solvent containing the extractant can be carried out either batchwise or continuously using well-known mixer-settler equipment, extraction towers, centrifugal extractors, and the like.
混合温度は使用される希釈剤に依存して０〜７０°Ｃ１
好ましくは１０〜４０’Ｃに選定される。Mixing temperature varies from 0 to 70°C depending on the diluent used
Preferably, the temperature is selected to be 10 to 40'C.
有機相（有機溶媒）対水相（被処理液）の接触時の容積
比（０／Ａ比）は１／１５〜５／１程度好ましくは１／
２〜２／１であり、使用する設備および操業条件に応じ
て適宜選択されうる。The volume ratio (0/A ratio) of the organic phase (organic solvent) to the aqueous phase (liquid to be treated) during contact is about 1/15 to 5/1, preferably 1/
The ratio is 2 to 2/1, and can be selected as appropriate depending on the equipment used and operating conditions.
接触時間は、接触効率に依存するが、５〜６０分、普通
は１０〜３０分程度で充分である。The contact time depends on the contact efficiency, but 5 to 60 minutes, usually about 10 to 30 minutes, is sufficient.
抽出後の有機溶媒は塩酸により逆抽出される。The organic solvent after extraction is back-extracted with hydrochloric acid.
塩酸としては０．１〜７規定の濃度が選択される。As hydrochloric acid, a concentration of 0.1 to 7 normal is selected.
０／Ａ比は１１５〜１０／１好ましくは２／１〜５／１
とされ、そして温度は３０〜７０℃と抽出温度よりやや
高目とされる。0/A ratio is 115 to 10/1, preferably 2/1 to 5/1
The temperature is 30 to 70°C, which is slightly higher than the extraction temperature.
接触時間は、使用装置の型式に依存するが、５〜３０分
で充分である。The contact time depends on the type of equipment used, but 5 to 30 minutes is sufficient.
抽出剤は循環使用中鉄等の蓄積が起り、抽出能力が低下
した場合、鉱酸等で洗浄してやることにより抽出能力は
回復する。When the extractant accumulates iron and other substances during cyclical use and its extraction ability decreases, the extraction ability can be recovered by washing it with mineral acid or the like.
実施例
燐酸ジ２−エチルヘキシルエステルをティスパーゾル（
シェル化学の商品名）で１０容量％に希釈した有機溶媒
によって抽出（抽出条件：温度２０℃、時間１５分、撹
拌羽根回転数７５ Ｏｒｐｍ、０／Ａ−９０７７１１／
９０ｍ１゜）後の、インジウムｏ、６５２ｇ／Ａを含む
有機溶媒を塩酸溶液を用いて逆抽出した。Example Phosphoric acid di2-ethylhexyl ester was dissolved in Tispersol (
Extraction with an organic solvent diluted to 10% by volume with Shell Chemical (trade name) (extraction conditions: temperature 20°C, time 15 minutes, stirring blade rotation speed 75 Orpm, 0/A-907711/
After 90ml (1°), the organic solvent containing 652g/A of indium O was back-extracted using a hydrochloric acid solution.
塩酸溶液としては３５ ｇ／ｌ、１０５ ｇ／ｌおよび
１７５ｇ／１１の濃度のものを用いた。Hydrochloric acid solutions with concentrations of 35 g/l, 105 g/l and 175 g/11 were used.
逆抽出条件は以下の通りとした：０／Ａ−６０ｍｌ／
６０ ｒｕｌ！、撹拌回転数７５ Ｏｒｐｍ％ 温度
５０℃、時間１５分。The back extraction conditions were as follows: 0/A-60ml/
60 rules! , stirring rotation speed 75 Orpm%, temperature 50°C, time 15 minutes.
逆抽出後の抜液（水相）のインジウム濃度を表Ｉに示す
。Table I shows the indium concentration of the drained liquid (aqueous phase) after back extraction.
比較目的の為硫酸１００．３００及び５ｏ ０９／１３
溶液により逆抽出を行った結果をも示す。For comparison purposes, sulfuric acid 100.300 and 5o 09/13
The results of back extraction using the solution are also shown.
表１かられかるように、塩酸の使用により非常に良好な
逆抽出性能が得られる。As can be seen from Table 1, the use of hydrochloric acid provides very good back extraction performance.
本発明は、インジウムに対してきわめて選択性のよい有
機溶媒を使用してのインジウム溶媒抽出分離方法におい
てきわめて容易に且つ効果的に実施しうる逆抽出法を確
立したものであり、鉛滓等の製錬工程の各種副産物から
のインジウムの回収にきわめて効果的である。The present invention establishes a back extraction method that can be carried out extremely easily and effectively in the indium solvent extraction separation method using an organic solvent with extremely high selectivity for indium. It is extremely effective in recovering indium from various by-products of the smelting process.
Claims (1)
液を燐酸ジ２−エチルヘキシルエステルを抽出剤として
含む有機溶媒とｐＨ１，ｏ以下で接触しそしてインジウ
ムを含有する抽出後溶媒を塩酸で３０〜７０℃の温度に
おいて逆抽出することから成るインジウムの選択分離方
法。1. A sulfuric acid acidic solution containing indium and other metals is brought into contact with an organic solvent containing phosphoric acid di-2-ethylhexyl ester as an extractant at pH 1.0 or below, and the indium-containing extraction solvent is heated at 30 to 70°C with hydrochloric acid. A selective separation method for indium consisting of back extraction at temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP54057022A JPS5924169B2 (en) | 1979-05-11 | 1979-05-11 | Selective separation method for indium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP54057022A JPS5924169B2 (en) | 1979-05-11 | 1979-05-11 | Selective separation method for indium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS55148736A JPS55148736A (en) | 1980-11-19 |
| JPS5924169B2 true JPS5924169B2 (en) | 1984-06-07 |
Family
ID=13043797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP54057022A Expired JPS5924169B2 (en) | 1979-05-11 | 1979-05-11 | Selective separation method for indium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5924169B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT1185549B (en) * | 1985-04-12 | 1987-11-12 | Samim Soc Azionaria Minero Met | PROCEDURE FOR THE SEPARATION OF INDIO FROM ACID SOLUTIONS THAT CONTAIN IT |
| BRPI0701919B1 (en) * | 2007-05-23 | 2016-10-11 | Votorantim Metais Zinco S A | pure metal indium production process from zinc oxide and / or metal-containing solution |
| CN106756060B (en) * | 2017-03-24 | 2018-10-09 | 河北长力环保科技有限公司 | A kind of recovery method of indium metal |
-
1979
- 1979-05-11 JP JP54057022A patent/JPS5924169B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS55148736A (en) | 1980-11-19 |
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