JPH06248370A - Method for recovering in from in-sb alloy - Google Patents
Method for recovering in from in-sb alloyInfo
- Publication number
- JPH06248370A JPH06248370A JP6138093A JP6138093A JPH06248370A JP H06248370 A JPH06248370 A JP H06248370A JP 6138093 A JP6138093 A JP 6138093A JP 6138093 A JP6138093 A JP 6138093A JP H06248370 A JPH06248370 A JP H06248370A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- dross
- metal
- recovering
- amount
- 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]
【産業上の利用分野】本発明は、Ｉｎ−Ｓｂ合金からＩ
ｎを回収する方法に関する。The present invention relates to an In--Sb alloy containing I
and a method of recovering n.
【０００２】[0002]
【従来の技術】Ｉｎ−Ｓｂ合金は、例えば、５０重量％
前後のＩｎを含有する化合物半導体としてホール素子や
赤外線デテクターに使用されている。Ｉｎ−Ｓｂ合金ス
クラップは、簡単な処理により再利用することが難しい
ため、該スクラップから高価なＩｎを回収する方法が検
討されている。2. Description of the Related Art In-Sb alloys are, for example, 50% by weight.
It is used as a front and rear compound semiconductor containing In for a Hall element and an infrared detector. Since it is difficult to reuse In—Sb alloy scrap by a simple process, a method of recovering expensive In from the scrap has been studied.
【０００３】上記方法として、（１）ＨＣｌ，Ｈ2 ＳＯ
4 などにより浸出する、（２）Ｓｂ含有率を０．５〜１
０重量％に組成を調整したものをアノードとして電解精
製する、（３）融体から塩化物として揮発させる、
（４）融体からドロス中に移行させるなどの方法が提案
されている。The above methods include (1) HCl, H 2 SO
Leach by 4 etc., (2) Sb content is 0.5 to 1
Electrolytic refining with the composition adjusted to 0% by weight as the anode, (3) volatilization from the melt as chloride,
(4) A method of moving the melt into the dross has been proposed.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、これら
の方法はいずれも、Ｉｎの回収率が悪いという問題点が
ある。本発明の目的は、上記事情に鑑み、Ｉｎ−Ｓｂ合
金スクラップからＩｎを高収率で回収する方法を提供す
ることにある。However, all of these methods have a problem that the recovery rate of In is poor. In view of the above circumstances, an object of the present invention is to provide a method for recovering In from In—Sb alloy scrap in a high yield.
【０００５】[0005]
【課題を解決するための手段】本発明は、上記目的を達
成するものとして、Ｉｎ−Ｓｂ合金と金属Ｐｂ、金属Ｓ
ｎおよび金属Ｂｉのうちの少なくとも１種とを加熱溶解
して合金融体を形成し、該合金融体の温度を３５０〜５
００℃に維持しつつ、該合金融体に塩化剤を反応させ、
生成したドロスを該合金融体から分離回収することを特
徴とするＩｎ−Ｓｂ合金からのＩｎの回収方法である。In order to achieve the above object, the present invention provides an In-Sb alloy, a metal Pb, and a metal S.
n and at least one of the metals Bi are heated and melted to form a combined financial body, and the temperature of the combined financial body is set to 350 to 5
While maintaining the temperature at 00 ° C., react a chlorinating agent with the combined financial body,
A method for recovering In from an In-Sb alloy, characterized in that the generated dross is separated and recovered from the financial instrument.
【０００６】[0006]
【作用】本発明方法において、まず、Ｉｎ−Ｓｂ合金と
金属Ｐｂ、金属Ｓｎおよび金属Ｂｉのうちの少なくとも
１種とを加熱溶解して合金融体を形成する。金属Ｐｂ、
金属Ｓｎおよび金属Ｂｉのうちの少なくとも１種を添加
するのは、後述する塩化剤を３５０〜５００℃で反応さ
せる工程でＩｎを効率よくドロス中に移行させるためで
ある。これは、金属Ｐｂ、金属Ｓｎおよび金属Ｂｉのう
ちの少なくとも１種の添加により上記反応温度で合金が
融体となるため、ＩｎのＩｎＣｌとしての揮発が無視し
得ることと、添加する上記金属のＣｌに対する親和力が
Ｉｎのそれより小さいことによると考えられる。In the method of the present invention, first, the In-Sb alloy and at least one of the metal Pb, the metal Sn and the metal Bi are heated and melted to form a financial instrument. Metal Pb,
The reason for adding at least one of the metal Sn and the metal Bi is to efficiently transfer In into dross in the step of reacting a chlorinating agent described later at 350 to 500 ° C. This is because the addition of at least one of metal Pb, metal Sn and metal Bi turns the alloy into a melt at the above reaction temperature, so that volatilization of In as InCl can be neglected and that the addition of the above-mentioned metal It is considered that the affinity for Cl is smaller than that of In.
【０００７】上記添加の量は、Ｉｎ−Ｓｂ合金中に含有
されるＳｂ量の２．５〜２０重量倍とするのが好まし
い。２．５重量倍未満では、上記添加により得られる合
金の融点が上昇し、該合金を上記反応温度で融体で維持
できず、一方、２０重量倍を超えると、上記添加により
得られる合金中のＩｎ含有率が低下し、Ｉｎの回収率が
低下し易い。上記金属の中では、市販で入手し易いＰｂ
が好ましい。The amount of the above addition is preferably 2.5 to 20 times by weight the amount of Sb contained in the In-Sb alloy. If it is less than 2.5 times by weight, the melting point of the alloy obtained by the above-mentioned addition increases, and the alloy cannot be maintained as a melt at the above-mentioned reaction temperature. In content rate of In decreases, and the recovery rate of In tends to decrease. Among the above metals, Pb, which is easily available on the market
Is preferred.
【０００８】次に、得られた合金融体の温度を３５０〜
５００℃に維持しつつ、該合金融体に塩化剤を反応さ
せ、ドロスを生成させる。上記合金融体に塩化剤を反応
させると、ＩｎはＳｂや上記金属と比べてＣｌに対する
親和力が大きいために、ＩｎはＩｎＣｌとなり上記融体
上のドロスに移行する。Next, the temperature of the obtained financial institution is set to 350-
While maintaining the temperature at 500 ° C, a chlorinating agent is caused to react with the financial instrument to generate dross. When a chlorinating agent is reacted with the above-mentioned financial body, In has a greater affinity for Cl than Sb and the above metals, and thus In becomes InCl and moves to dross on the melt.
【０００９】維持する融体の温度を３５０〜５００℃と
するのは、３５０℃未満では、融体の流動性が低く、上
記反応が十分おこり難いからであり、一方、５００℃を
超えると、ドロス相と合金相との分離性が低下し、Ｉｎ
Ｃｌの揮発が大きくなるからである。The reason why the temperature of the melt to be maintained is 350 to 500 ° C. is that if the temperature is lower than 350 ° C., the fluidity of the melt is low and the above reaction is difficult to occur, while if it exceeds 500 ° C. Separation between the dross phase and the alloy phase is reduced, and In
This is because the volatilization of Cl becomes large.
【００１０】塩化剤としては、例えば、塩化アンモニウ
ム，塩素ガスが挙げられるが、その取扱上、塩化アンモ
ニウムが好ましい。この塩化剤の使用は、一度で終了す
るより、毎回ドロスを回収する操作を複数回行なって終
了する使用方式の方が好ましい。塩化アンモニウムの１
回毎の使用量は、合金融体の０．１〜１重量％とするの
が好ましい。０．１重量％未満では、ドロスの生成量が
少なく、上記反応が十分おこり難く、一方、１重量％を
超えると、生成するドロス量が増加しドロス中のＩｎ含
有率が低下し、Ｉｎの回収率が低下し易い。Examples of the chlorinating agent include ammonium chloride and chlorine gas. Ammonium chloride is preferable in terms of handling. The use of the chlorinating agent is preferably performed in a usage system in which the operation of recovering the dross each time is performed plural times and the operation is ended, rather than ending the operation once. Ammonium chloride 1
The amount used each time is preferably 0.1 to 1% by weight of the combined financial body. If it is less than 0.1% by weight, the amount of dross generated is small and the above reaction is difficult to occur. On the other hand, if it exceeds 1% by weight, the amount of dross generated increases and the In content in the dross decreases, resulting in The recovery rate tends to decrease.
【００１１】生成し、合金融体から分離回収されたドロ
スは、必要により別の合金融体に同様に反応させてＩｎ
品位のより高いドロスとした後、例えば、次の方法によ
り高純度Ｉｎを得ることができる。即ち、ドロスを過剰
の塩酸に溶解し、アルカリ水溶液によりｐＨを１程度に
調整し、主としてＰｂとＳｂとを沈殿させ、分離して得
た溶液にＺｎ粉末等の還元剤を添加しセメントＩｎを析
出させる。析出したＩｎをカセイソーダを添加し溶解し
て、粗Ｉｎとする。このようにして得た粗Ｉｎは、アノ
ードに鋳造し電解精製して、高純度Ｉｎとする。The dross produced and separated and collected from the financial institution is reacted with another financial institution in the same manner, if necessary.
After making the dross of higher quality, for example, high-purity In can be obtained by the following method. That is, the dross is dissolved in excess hydrochloric acid, the pH is adjusted to about 1 with an alkaline aqueous solution, Pb and Sb are mainly precipitated, and a reducing agent such as Zn powder is added to the solution obtained by separation to add cement In. Precipitate. The precipitated In is dissolved by adding caustic soda to obtain crude In. The crude In thus obtained is cast into an anode and electrolytically refined to obtain high-purity In.
【００１２】[0012]
【実施例】次に、本発明の実施例について説明する。 実施例 Ｉｎ４８．５重量％（以下、重量％を％と記す）、残部
が実質的にＳｂからなる合金スクラップ６７．１ｋｇと
金属Ｐｂ３００ｋｇを黒鉛るつぼに装入し、４００℃で
加熱溶解した。次に、塩化アンモニウム１．５ｋｇを添
加し、約１時間かけて充分に攪拌後、融体上に形成され
たドロスを柄杓ですくい回収した。このような操作を２
４回行なった。EXAMPLES Next, examples of the present invention will be described. Example In 48.5 wt% In (hereinafter, wt% is referred to as%), 67.1 kg of alloy scrap consisting essentially of Sb and 300 kg of metal Pb were charged into a graphite crucible and melted by heating at 400 ° C. Next, 1.5 kg of ammonium chloride was added, and after sufficiently stirring for about 1 hour, the dross formed on the melt was collected by scooping with a ladle. 2 such operations
It was performed 4 times.
【００１３】この結果は、次の通りであった。即ち、１
回目のドロスの品位は、Ｉｎ５０．３％、Ｐｂ２４．６
％、Ｓｂ０．０２％、そして２４回目は、ドロスの品位
が、Ｉｎ１２．７％、Ｐｂ６１．３％、Ｓｂ０．２８％
で、合金の品位が、Ｉｎ０．９４％、Ｐｂ８８．０％、
Ｓｂ１１．１％であった。また、得られたドロスの合計
量は、８２．６ｋｇ、その平均品位は、Ｉｎ３５．８
％、Ｐｂ４９．９％、Ｓｂ０．０４％であった。そし
て、２４回目にドロスを分離した合金は、２９４ｋｇで
あった。The results are as follows. That is, 1
The dross quality of the second time is In50.3%, Pb24.6.
%, Sb 0.02%, and the 24th time, dross quality is In12.7%, Pb61.3%, Sb0.28%
And, the grade of the alloy is In0.94%, Pb88.0%,
The Sb was 11.1%. The total amount of dross obtained was 82.6 kg, and the average quality was In35.8.
%, Pb 49.9%, and Sb 0.04%. The alloy from which the dross was separated at the 24th time was 294 kg.
【００１４】このような処理によって、ＩｎＣｌの揮発
等によるＩｎ損失がほとんどなく、高収率でＩｎをドロ
ス中に回収できることが判る。It can be seen that, by such a treatment, there is almost no loss of In due to volatilization of InCl, and In can be recovered in the dross in a high yield.
【００１５】回収したドロスは全量、３６％の塩酸１１
０ｋｇに常温で攪拌しながら溶解し、２５０ｇ／リット
ルのカセイソーダ溶液によりｐＨを１．５に調整した。
生成した沈殿を濾過により分離除去し、２６０リットル
の濾液を得た。この濾液を攪拌しつつＺｎ粉末２９．７
ｋｇを添加し、Ｉｎを析出させた。得られたセメントＩ
ｎと２．０ｋｇのカセイソーダをステンレス製るつぼに
装入し２５０℃で溶解した後、表面のスラグを除いて２
７．８ｋｇの粗Ｉｎを得た。この粗Ｉｎの品位は、Ｉｎ
９９．４％、Ｐｂ０．４４％、Ｓｂ０．０１％ であっ
た。The total amount of dross collected is 36% hydrochloric acid 11
It was dissolved in 0 kg with stirring at room temperature, and the pH was adjusted to 1.5 with a 250 g / liter caustic soda solution.
The generated precipitate was separated and removed by filtration to obtain 260 liters of filtrate. Zn powder 29.7 while stirring this filtrate
In was deposited by adding kg. The obtained cement I
n and 2.0 kg caustic soda were charged into a stainless crucible and melted at 250 ° C., and then the surface slag was removed to remove it.
7.8 kg of crude In was obtained. The quality of this coarse In is In
It was 99.4%, Pb 0.44%, and Sb 0.01%.
【００１６】[0016]
【発明の効果】本発明の方法によれば、Ｉｎ−Ｓｂ合金
スクラップからＩｎを高収率で、かつ簡便にドロス中に
回収することができる。According to the method of the present invention, In can be easily recovered from the In-Sb alloy scrap in the dross in a high yield.
Claims (4)
よび金属Ｂｉのうちの少なくとも１種とを加熱溶解して
合金融体を形成し、該合金融体の温度を３５０〜５００
℃に維持しつつ、該合金融体に塩化剤を反応させ、生成
したドロスを該合金融体から分離回収することを特徴と
するＩｎ−Ｓｂ合金からのＩｎの回収方法。1. An In—Sb alloy and at least one of metal Pb, metal Sn and metal Bi are heated and melted to form a financial unit, and the temperature of the unit is 350 to 500.
A method for recovering In from an In-Sb alloy, which comprises reacting a chlorinating agent with the financial instrument while maintaining the temperature at 0 ° C to separate and recover the produced dross from the financial instrument.
項１記載のＩｎ−Ｓｂ合金からのＩｎの回収方法。2. The method for recovering In from the In—Sb alloy according to claim 1, wherein the chlorinating agent is ammonium chloride.
ちの少なくとも１種の使用量は、Ｉｎ−Ｓｂ合金中に含
有されるＳｂ量の２．５〜２０重量倍である請求項１ま
たは２記載のＩｎ−Ｓｂ合金からのＩｎの回収方法。3. The use amount of at least one of metal Pb, metal Sn and metal Bi is 2.5 to 20 times by weight the amount of Sb contained in the In—Sb alloy. A method for recovering In from the described In-Sb alloy.
き合金融体の０．１〜１重量％である請求項２記載のＩ
ｎ−Ｓｂ合金からのＩｎの回収方法。4. The method according to claim 2, wherein the amount of ammonium chloride used is 0.1 to 1% by weight of the combined financial body per time.
A method for recovering In from an n-Sb alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6138093A JP2958504B2 (en) | 1993-02-26 | 1993-02-26 | Method for recovering In from In-Sb alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6138093A JP2958504B2 (en) | 1993-02-26 | 1993-02-26 | Method for recovering In from In-Sb alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06248370A true JPH06248370A (en) | 1994-09-06 |
| JP2958504B2 JP2958504B2 (en) | 1999-10-06 |
Family
ID=13169518
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6138093A Expired - Lifetime JP2958504B2 (en) | 1993-02-26 | 1993-02-26 | Method for recovering In from In-Sb alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2958504B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7611631B2 (en) | 2004-07-09 | 2009-11-03 | Aquatech Corporation | Indium adsorbent and indium fractioning method |
| JP2016107329A (en) * | 2014-12-10 | 2016-06-20 | 住友金属鉱山株式会社 | Anode regeneration process |
| JP2016194120A (en) * | 2015-04-01 | 2016-11-17 | 住友金属鉱山株式会社 | Method for producing indium metal |
-
1993
- 1993-02-26 JP JP6138093A patent/JP2958504B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7611631B2 (en) | 2004-07-09 | 2009-11-03 | Aquatech Corporation | Indium adsorbent and indium fractioning method |
| JP2016107329A (en) * | 2014-12-10 | 2016-06-20 | 住友金属鉱山株式会社 | Anode regeneration process |
| JP2016194120A (en) * | 2015-04-01 | 2016-11-17 | 住友金属鉱山株式会社 | Method for producing indium metal |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2958504B2 (en) | 1999-10-06 |
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