JPS6316337B2 - - Google Patents
Info
- Publication number
- JPS6316337B2 JPS6316337B2 JP10553984A JP10553984A JPS6316337B2 JP S6316337 B2 JPS6316337 B2 JP S6316337B2 JP 10553984 A JP10553984 A JP 10553984A JP 10553984 A JP10553984 A JP 10553984A JP S6316337 B2 JPS6316337 B2 JP S6316337B2
- Authority
- JP
- Japan
- Prior art keywords
- indium
- sulfuric acid
- acid
- mol
- extractant
- 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
- 229910052738 indium Inorganic materials 0.000 claims description 32
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- 239000002253 acid Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 9
- 239000011701 zinc Substances 0.000 description 9
- 229910052725 zinc Inorganic materials 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 7
- 239000012044 organic layer Substances 0.000 description 7
- 239000003350 kerosene Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- -1 2-ethylhexyl Chemical group 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Description
本発明はインジウムを含む硫酸溶液中からイン
ジウムを回収する方法に関するものである。
亜鉛製錬残渣を原料としてインジウムを製造す
る場合、不純物として亜鉛や鉄を含むインジウム
の硫酸溶液が得られるが、高純度のインジウムを
製造するには、インジウムを亜鉛や鉄などの不純
物から分離することが必要である。また電子材料
工業において、インジウムを含む廃液からインジ
ウムを回収することも必要である。本発明の方法
は、インジウムを含む硫酸溶液中からインジウム
を回収するにあたり抽出剤としてジアルキルジチ
オリン酸を含む溶液を用いて抽出処理し、溶液中
に含まれるインジウムを抽出剤中に移行させる方
法である。
本発明者の研究によれば、ジアルキルジチオリ
ン酸は硫酸溶液からインジウムの抽出にはすぐれ
た抽出効果を示すことが見出された。
本発明で用いる抽出剤はジアルキルジチオリン
酸を適当な溶媒に希釈することにより調製され
る。この場合ジアルキルジチオリン酸におけるア
ルキル基としては通常、炭素数６以上、好ましく
は８〜12の高級アルキル基殊に、２−エチルヘキ
シルが好適である。また溶媒としては硫酸に対し
て安定なものケロシン、ベンゼン、トルエンなど
の炭化水素溶媒が好適である。抽出剤中のジアル
キルジチオリン酸の濃度は0.01〜0.1モル／の
範囲で選定するのがよい。ジアルキルジチオリン
酸の濃度が0.01モル／以下になるとインジウム
の抽出する能力の低下を生じ好ましくなく一方、
0.1モル／を越えるようになるとインジウムの
抽出が増大すると同時に亜鉛の抽出も増大し、ジ
アルキルジチオリン酸の溶解性の限界に近い値と
なる等の弊害が生じるので好ましくない。
本発明の方法を実施するには対象溶液であるイ
ンジウム含有硫酸溶液を前記抽出剤を用いて処理
する。この場合、インジウム含有硫酸溶液中の硫
酸濃度は0.5〜４モル／の範囲にするのがよい。
この抽出処理により、硫酸溶液中に含まれるイン
ジウムは抽出剤中に移行するが、この抽出剤中の
インジウムは、次に塩酸により容易に逆抽出する
ことができる。
本発明の方法によれば、インジウムを含む各種
硫酸溶液からインジウムを効率よく分離回収する
ことが可能である。この場合、インジウム以外の
金属たとえば、亜鉛、鉄、マンガン等は抽出され
ない。本発明の方法は、インジウム含有溶液から
単にインジウムを回収する方法として使用し得る
ばかりでなく、それら金属とインジウムの混合物
からのインジウムの分離方法としても使用され
る。
次に本発明を実施例によつてさらに詳細に説明
する。
実施例 １
ジ−２−エチルヘキシルジチオリン酸をケロシ
ンに溶解して、ジ−２−エチルヘキシルジチオリ
ン酸18.6ｇ/の抽出剤と調製した。
次に、インジウムと亜鉛、鉄を含む硫酸溶液
100mlと前記抽出剤100mlを混合したのち、有機層
と水層に分離し、有機層をさらに塩酸により逆抽
出処理した。第１表に逆抽出液中に抽出された金
属の回収率を示す。
The present invention relates to a method for recovering indium from a sulfuric acid solution containing indium. When producing indium using zinc smelting residue as a raw material, a sulfuric acid solution of indium containing zinc and iron as impurities is obtained, but in order to produce high-purity indium, indium must be separated from impurities such as zinc and iron. It is necessary. In the electronic material industry, it is also necessary to recover indium from waste liquids containing indium. The method of the present invention is a method in which indium is recovered from a sulfuric acid solution containing indium by performing an extraction treatment using a solution containing dialkyldithiophosphoric acid as an extractant, and indium contained in the solution is transferred into the extractant. . According to research conducted by the present inventors, it has been found that dialkyldithiophosphoric acid exhibits an excellent extraction effect in extracting indium from a sulfuric acid solution. The extractant used in the present invention is prepared by diluting dialkyldithiophosphoric acid in a suitable solvent. In this case, the alkyl group in the dialkyldithiophosphoric acid is usually a higher alkyl group having 6 or more carbon atoms, preferably 8 to 12 carbon atoms, particularly 2-ethylhexyl. In addition, suitable solvents include hydrocarbon solvents that are stable against sulfuric acid, such as kerosene, benzene, and toluene. The concentration of dialkyldithiophosphoric acid in the extractant is preferably selected within the range of 0.01 to 0.1 mol/mol. If the concentration of dialkyldithiophosphoric acid is less than 0.01 mol/mol, the ability to extract indium will decrease, which is undesirable.
If the amount exceeds 0.1 mol/mol, the extraction of indium increases and at the same time the extraction of zinc also increases, resulting in problems such as a value close to the solubility limit of dialkyldithiophosphoric acid, which is not preferable. To carry out the method of the present invention, an indium-containing sulfuric acid solution, which is a target solution, is treated with the extractant. In this case, the sulfuric acid concentration in the indium-containing sulfuric acid solution is preferably in the range of 0.5 to 4 mol/mol.
Through this extraction process, the indium contained in the sulfuric acid solution is transferred into the extractant, but the indium in this extractant can then be easily back-extracted with hydrochloric acid. According to the method of the present invention, it is possible to efficiently separate and recover indium from various sulfuric acid solutions containing indium. In this case, metals other than indium, such as zinc, iron, manganese, etc., are not extracted. The method of the present invention can be used not only as a method for recovering indium from indium-containing solutions, but also as a method for separating indium from mixtures of these metals and indium. Next, the present invention will be explained in more detail with reference to Examples. Example 1 Di-2-ethylhexyldithiophosphoric acid was dissolved in kerosene to prepare an extractant of 18.6 g/di-2-ethylhexyldithiophosphoric acid. Next, a sulfuric acid solution containing indium, zinc and iron
After mixing 100 ml and 100 ml of the above extractant, the mixture was separated into an organic layer and an aqueous layer, and the organic layer was further subjected to back extraction treatment using hydrochloric acid. Table 1 shows the recovery rate of metals extracted into the back extraction solution.
【表】
なお、前記ジ−２−エチルヘキシルジチオリン
酸は次の構造式で示される。[Table] Note that the di-2-ethylhexyldithiophosphoric acid is represented by the following structural formula.
【式】（式中Ｒは２−エチルヘキシル
基である）
実施例 ２
インジウムと亜鉛、鉄を含む１モル／硫酸溶
液100mlと18.6ｇ/のジ−２−エチルヘキシルジ
チオリン酸のケロシン溶液100mlと混合したのち、
有機層と水層に分離した、塩酸を用いて有機層を
逆抽出した。その結果を第２表に示す。[Formula] (In the formula, R is a 2-ethylhexyl group) Example 2 100 ml of a 1 mol/sulfuric acid solution containing indium, zinc, and iron was mixed with 100 ml of a kerosene solution of 18.6 g/di-2-ethylhexyldithiophosphoric acid. after,
The organic layer was separated into an organic layer and an aqueous layer, and the organic layer was back-extracted using hydrochloric acid. The results are shown in Table 2.
【表】
実施例 ３
インジウムと亜鉛、鉄を含む0.5モル／硫酸
溶液100mlと18.6ｇ/ジ−２−エチルヘキシルジ
チオリン酸のケロシン溶液100mlと混合したのち、
有機層と水層に分離した。塩酸を用いて有機層を
逆抽出処理した。その結果を第３表に示す。[Table] Example 3 After mixing 100 ml of a 0.5 mol/sulfuric acid solution containing indium, zinc, and iron with 100 ml of a kerosene solution containing 18.6 g/di-2-ethylhexyldithiophosphoric acid,
Separated into organic and aqueous layers. The organic layer was back-extracted using hydrochloric acid. The results are shown in Table 3.
【表】
実施例 ４
インジウムと亜鉛、鉄、マンガン、鉛を含む１
モル／硫酸溶液100mlと18.6ｇ/のジ−２−エ
チルヘキシルジチオリン酸100mlと混合したのち、
有機層と水層に分離した。塩酸を用いて有機層を
逆抽出処理した。その結果を第４表に示す。[Table] Example 4 1 containing indium, zinc, iron, manganese, and lead
After mixing 100 ml of mol/sulfuric acid solution with 100 ml of 18.6 g/di-2-ethylhexyldithiophosphoric acid,
Separated into organic and aqueous layers. The organic layer was back-extracted using hydrochloric acid. The results are shown in Table 4.
Claims (1)
を回収するにあたり、抽出剤としてジアルキルジ
チオリン酸を含む溶液を用いて抽出処理すること
を特徴とするインジウムの回収方法。1. A method for recovering indium, which comprises performing an extraction process using a solution containing dialkyldithiophosphoric acid as an extractant when recovering indium from a sulfuric acid solution containing indium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10553984A JPS60251128A (en) | 1984-05-24 | 1984-05-24 | Method for recovering indium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10553984A JPS60251128A (en) | 1984-05-24 | 1984-05-24 | Method for recovering indium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60251128A JPS60251128A (en) | 1985-12-11 |
| JPS6316337B2 true JPS6316337B2 (en) | 1988-04-08 |
Family
ID=14410390
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10553984A Granted JPS60251128A (en) | 1984-05-24 | 1984-05-24 | Method for recovering indium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60251128A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2077601A1 (en) * | 1992-09-04 | 1994-03-05 | William Andrew Rickelton | Recovery of indium by solvent extraction using trialkyl-phosphine oxides |
-
1984
- 1984-05-24 JP JP10553984A patent/JPS60251128A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60251128A (en) | 1985-12-11 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |