JPH05125462A - Method for refining aluminum - Google Patents
Method for refining aluminumInfo
- Publication number
- JPH05125462A JPH05125462A JP28582091A JP28582091A JPH05125462A JP H05125462 A JPH05125462 A JP H05125462A JP 28582091 A JP28582091 A JP 28582091A JP 28582091 A JP28582091 A JP 28582091A JP H05125462 A JPH05125462 A JP H05125462A
- Authority
- JP
- Japan
- Prior art keywords
- stirrer
- container
- aluminum
- vessel
- molten aluminum
- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は不純アルミニウムの溶融
体を分別結晶化の原理を用いて凝固せしめ、原料アルミ
ニウムより純度の高いアルミニウムを分別取得するアル
ミニウムの精製法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for refining aluminum in which a molten material of impure aluminum is solidified by the principle of fractional crystallization to fractionally obtain aluminum having a higher purity than the raw material aluminum.
【０００２】[0002]
【従来の技術】不純アルミニウムを原料として、その溶
融体を保温容器中に保持し、コントロール条件下徐々に
冷却せしめて、より純度の高いアルミニウムを分離取得
する方法が種々提案されている。（例えば、特公昭 49-
5806号及び特公昭50-20536号公報等）2. Description of the Related Art Various methods have been proposed in which impure aluminum is used as a raw material, the melt is held in a heat-retaining container, and gradually cooled under controlled conditions to separate and obtain higher-purity aluminum. (For example, Japanese Patent Publication 49-
5806 and Japanese Patent Publication No. 50-20536)
【０００３】しかしながら分別結晶化の原理を用いてア
ルミニウムを精製する方法は、一般に生産効率が悪く、
設備費が嵩みコスト高となるとともに、液相のアルミニ
ウム溶融体を攪拌せず静的状態で凝固せしめた場合には
分別結晶化の効果が小さく、相対的に高純度アルミニウ
ムを分別取得することが容易ではない。However, the method for purifying aluminum using the principle of fractional crystallization generally has a low production efficiency,
The equipment cost is high and the cost is high, and the effect of fractional crystallization is small when the liquid-phase aluminum melt is solidified in a static state without stirring. Is not easy.
【０００４】この原因は、凝固過程の固液界面をミクロ
的に観察した場合に明らかとなる。すなわち、分別結晶
化に於いては冷却の過程で結晶核あるいは固相面から純
度の高い樹枝状晶が成長して凝固が進行するが樹枝状晶
の間隙には、不純物が濃縮された液相アルミニウムが残
る。この状態で静的に凝固が進行すると成長した樹枝状
晶間に不純物が濃縮された不純アルミニウム相が拘束さ
れ、残余の溶融アルミニウム相への拡散、液相不純物濃
度の均一化がはかれない状態で凝固が進行してしまう。
このため、凝固相の平均濃度は予期したほどには向上し
ないのである。This cause becomes clear when the solid-liquid interface in the solidification process is observed microscopically. That is, in fractional crystallization, high-purity dendrites grow from the crystal nuclei or solid-phase surface in the course of cooling and solidification proceeds, but in the gaps between the dendrites, liquid phase in which impurities are concentrated Aluminum remains. When the solidification proceeds statically in this state, the impure aluminum phase in which impurities are concentrated is confined between the grown dendrites, and the diffusion into the remaining molten aluminum phase and the inhomogeneity of the liquid phase impurity concentration cannot be achieved. Coagulation progresses at.
For this reason, the average concentration of the solidification phase does not improve as expected.
【０００５】そこで分別結晶化の効果を高めるために、
凝固過程下の液相部を何等かの手段で攪拌し、凝固相に
近接する不純物が濃縮されたアルミニウムを残余の遠隔
部のアルミニウム液相部に十分拡散せしめ、液相内部の
不純物濃度の偏差を可能な限り小さくする種々の試みが
なされている。Therefore, in order to enhance the effect of fractional crystallization,
The liquid phase part under the solidification process is agitated by some means so that the aluminum concentrated in the vicinity of the solid phase and having impurities concentrated is sufficiently diffused into the remaining aluminum liquid phase part of the residual part, and the deviation of the impurity concentration inside the liquid phase Various attempts have been made to make the value as small as possible.
【０００６】かかる目的に基づき、特公昭59-41500号、
特公平2-2935号のように溶融アルミニウム中で攪拌子を
回転させ、液相部を攪拌し、不純物濃度の均一化を計る
方法等が提案されている。Based on such a purpose, Japanese Examined Patent Publication No. 59-41500,
As disclosed in Japanese Examined Patent Publication No. 2935/1990, a method has been proposed in which a stirrer is rotated in molten aluminum to stir the liquid phase portion to make the impurity concentration uniform.
【０００７】回転攪拌子による攪拌効果を高めるには、
回転数が増加させることが必要となるが、回転数が増加
するにつれ、これにより溶融アルミニウム中の回転攪拌
子近傍に生じる渦深さが深くなり、アルミニウム酸化物
が多量に発生したり、更には回転攪拌子まで渦深さが深
くなると攪拌子の芯振れ等が生起し操作が不可能とな
る。従って回転攪拌子のみで攪拌効果を高めるには限界
がある。To enhance the stirring effect of the rotary stirrer,
It is necessary to increase the number of revolutions, but as the number of revolutions increases, the vortex depth generated in the vicinity of the rotary stirrer in the molten aluminum becomes deeper, and a large amount of aluminum oxide is generated. When the vortex depth increases to the rotary stirrer, the runout of the stirrer occurs and operation becomes impossible. Therefore, there is a limit to enhancing the stirring effect only with the rotary stirrer.
【０００８】[0008]
【発明が解決しようとする課題】かかる状況下において
本発明者らは鋭意検討を行った結果、前述の渦深さの問
題が解決でき、更により純度の高いアルミニウムを分離
取得しうるべく鋭意検討した結果、攪拌子による溶融ア
ルミニウムの攪拌と該溶融アルミニウムの保持容器を逆
回転させることにより本発明を完成するに至った。Under the circumstances, the inventors of the present invention have diligently studied, and as a result, the above-mentioned problem of the vortex depth can be solved, and further diligently studied so that a higher purity aluminum can be separated and obtained. As a result, the present invention has been completed by stirring the molten aluminum with a stirrer and rotating the holding container for the molten aluminum in the reverse direction.
【０００９】[0009]
【課題を解決するための手段】すなわち、本発明は原料
溶融アルミニウムを容器中に保持し、該容器の上部およ
び側部を制御された温度条件下に保温管理し、該容器底
部より冷却しながら、該容器をその垂直軸を中心に回転
せしめると同時に、該容器中の溶融アルミニウムを該容
器回転方向と逆方向に攪拌子により回転せしめることに
より容器底部に純度の高いアルミニウムを分別析出せし
めることを特徴とするアルミニウムの精製法を提供する
ものである。That is, according to the present invention, raw material molten aluminum is held in a container, and the upper and side portions of the container are kept warm under controlled temperature conditions, while cooling from the bottom of the container. While rotating the container about its vertical axis, the molten aluminum in the container is rotated by a stirrer in the direction opposite to the container rotation direction to separate and precipitate high-purity aluminum at the bottom of the container. The present invention provides a characteristic aluminum refining method.
【００１０】以下、本発明法を詳細に説明する。本発明
法の実施に際し、原料となるアルミニウムは周知の溶融
塩を用いる電解精錬、或いは回収による再生メタル等の
高々９９．９重量％程度の純度を有するアルミニウム、
あるいは相当する品位のアルミニウムであって、最終目
的とする純度以下の純度を有するアルミニウムである。
原料アルミニウムは、例えば別途溶解され、耐火煉瓦等
で内張りした鉄製の溶融アルミニウムの保温保持容器中
に溶融状態で供給され保持される。The method of the present invention will be described in detail below. In carrying out the method of the present invention, the raw material aluminum is aluminum having a purity of at most about 99.9% by weight, such as a reclaimed metal obtained by electrolytic refining using a known molten salt or recovery,
Alternatively, it is aluminum of a corresponding grade and having a purity equal to or lower than the final target purity.
The raw material aluminum is separately melted, for example, and is supplied and held in a molten state in a heat-retaining container made of iron molten aluminum lined with refractory bricks or the like.
【００１１】該容器は、それ自体の少なくとも上部（蓋
部）、必要において側部に、容器本体を目的とする温度
に保温保持するための任意の加熱手段を付備するもので
あっても、また容器本体には加熱手段を設けず、この容
器を収容する雰囲気温度を制御し得て十分に容器本体を
目的の温度に保温保持しうる収容域、例えば雰囲気温度
制御の保持炉を保有し、該保持炉内に溶融アルミニウム
の保持容器を収容する構造のものであってもよい。The container may be provided with an arbitrary heating means for keeping the container body warm at a desired temperature, at least on its upper part (lid part), if necessary, on its side part, Further, the container body is not provided with a heating means, and the holding temperature of the container body can be controlled so that the container body can be sufficiently kept at the target temperature, for example, a holding furnace for controlling the atmosphere temperature is held. It may have a structure in which a molten aluminum holding container is housed in the holding furnace.
【００１２】本発明に於いて該容器はその底部を介して
回転可能な受け台上に固定保持され、台を回転すること
により、容器に所望の回転を付与する構造となってい
る。また該容器を回転する受け台とは別に、モーターを
設置した昇降可能な架台を設け、架台の昇降により攪拌
子を溶融アルミニウム中の所望の位置に配置し、モータ
ーにより攪拌子を該容器の回転方向とは逆方向に回転し
得るよう構成されている。該溶融アルミニウム中に於け
る攪拌子の位置は容器底部へのアルミニウムの晶出量に
合わせて容器底部の晶出アルミニウムの表面と攪拌子の
間隔が一定になるよう連動して架台を上昇せしめること
もできる。In the present invention, the container is fixedly held on a rotatable pedestal through its bottom, and by rotating the pedestal, a desired rotation is imparted to the container. In addition to the pedestal that rotates the container, a pedestal equipped with a motor that can be raised and lowered is provided, and the stirrer is placed at a desired position in the molten aluminum by raising and lowering the pedestal, and the stirrer is rotated by the motor. It is configured so that it can rotate in a direction opposite to the direction. The position of the stirrer in the molten aluminum is set in accordance with the amount of aluminum crystallized to the bottom of the container so that the pedestal can be moved up in conjunction so that the distance between the surface of the crystallized aluminum at the bottom of the container and the stirrer becomes constant. You can also
【００１３】該容器中に供給された溶融アルミニウムは
該容器の上部、側部は当該部位からの優先的な凝固が進
行しないよう管理された状態に維持され、容器底部を介
して溶融アルミニウムの有する熱を系外に導出して初晶
アルミニウムの晶出に導く。The molten aluminum supplied into the container is maintained in a state in which the upper part and the side part of the container are controlled so that preferential solidification from the relevant part does not proceed, and the molten aluminum has the property of being supplied through the bottom part of the container. Heat is led out of the system to lead to crystallization of primary aluminum.
【００１４】冷却手段としては、例えば容器底部に接す
る受け台下面に直接または間接的に空気、水などの媒体
を接触させるなど、制御された条件下の冷却が可能であ
れば任意の手段を採用しうる。As the cooling means, any means can be adopted as long as cooling under controlled conditions is possible, for example, by directly or indirectly bringing a medium such as air or water into contact with the lower surface of the pedestal which is in contact with the bottom of the container. You can.
【００１５】本発明方法に於いて、攪拌子単独で回転し
た場合、あるいは容器単独で回転した場合、回転数が増
加するにつれて渦深さが深くなる。本発明者らは、実験
により攪拌子の形状に余り関係なく、攪拌子単独の回転
による渦深さは（ｄｎ）2 に比例し、また容器単独の回
転による渦深さは（ＤＮ）2 に比例することを見出し
た。In the method of the present invention, when the stirrer is rotated alone or when the container is rotated alone, the vortex depth becomes deeper as the number of rotations increases. According to experiments, the present inventors have shown that, regardless of the shape of the stirrer, the vortex depth due to rotation of the stirrer alone is proportional to (dn) 2 and the vortex depth due to rotation of the container alone is (DN) 2 . It was found to be proportional.
【００１６】従って攪拌子径の増大、攪拌子回転数の増
加、容器径の増大、容器回転数の増加は渦深さを大幅に
増加させ、精製効率の向上、設備の大型化を図る際、大
きな問題となる。しかるに本発明法のように溶融アルミ
ニウム中を容器の回転方向とは逆方向に攪拌子を回転せ
しむると渦深さが減少する。Therefore, when the stirrer diameter is increased, the stirrer rotation speed is increased, the vessel diameter is increased, and the container rotation speed is increased, the eddy depth is greatly increased, and purification efficiency is improved and equipment is enlarged. It becomes a big problem. However, when the stirrer is rotated in the molten aluminum in the direction opposite to the rotation direction of the container as in the method of the present invention, the vortex depth decreases.
【００１７】水による多くの詳細な実験により、（Ｄ4
Ｎ）／（ｄ4 ｎ）が２．４〜３．０の場合には、渦深さ
が零になること、更にこのことは溶融アルミニウムにお
いても同様な結果であることがわかった。Many detailed experiments with water show that (D 4
It was found that when N) / (d 4 n) is 2.4 to 3.0, the vortex depth becomes zero, and this is the same in molten aluminum.
【００１８】実際の精製操作においては、必ずしも渦深
さを零にする必要はなく（Ｄ4 Ｎ）／（ｄ4 ｎ） が１
〜４．５の条件下で操作される。（Ｄ4 Ｎ）／（ｄ
4 ｎ）が１以下或いは４．５を超える条件では渦深さを
小さくする効果が少なく、望ましくは（Ｄ4 Ｎ）／（ｄ
4 ｎ）は２．０〜３．５の条件下での操作を行なう。操
業時の渦深さの許容範囲は容器の大きさにもより一義的
ではないが操業の安定性、アルミニウム酸化物の生成防
止から、容器直径の約３０％以下、通常は約２０％以下
にするのが好ましく、（Ｄ4 Ｎ）／（ｄ4 ｎ）が１〜
４．５であれば、これを達成し得る。In the actual refining operation, it is not always necessary to make the vortex depth zero, and (D 4 N) / (d 4 n) is 1
Operated under conditions of ~ 4.5. (D 4 N) / (d
When 4 n) is 1 or less or exceeds 4.5, the effect of reducing the vortex depth is small, and it is desirable that (D 4 N) / (d
4 n) performs operations under the conditions of 2.0 to 3.5. The allowable range of the vortex depth during operation is not unique to the size of the container, but it is set to about 30% or less of the container diameter, usually about 20% or less, from the stability of operation and the prevention of aluminum oxide formation. It is preferable that (D 4 N) / (d 4 n) is 1 to
With 4.5, this can be achieved.
【００１９】[0019]
【発明の効果】以上詳述したように本発明法によれば、
実質的に溶融アルミニウムに渦を生じせしめることな
く、或いは渦の生成の少ない操業が可能となるため、攪
拌子にかかる負荷の変動が少なく芯振れ等もなく、操業
が安定するばかりか、酸化物の生成が少なく、かつ容器
回転と攪拌子の逆回転の相乗効果により攪拌子単独の回
転による攪拌よりも攪拌効果が大きくなり、より純度の
高いアルミニウムを得ることができる等、その工業的価
値は頗る大である。As described in detail above, according to the method of the present invention,
Since it is possible to operate without causing vortices in the molten aluminum or generation of vortices, the load on the stirrer does not fluctuate, there is no center runout, and the operation is stable. Is less generated, and the stirring effect is greater than the stirring by the rotation of the stirrer alone due to the synergistic effect of the container rotation and the reverse rotation of the stirrer, and it is possible to obtain higher purity aluminum, etc., and its industrial value is It is very large.
【００２０】[0020]
【実施例】以下本発明方法を実施例により更に詳細に説
明するが、該実施例は本発明方法の一実施態様を示すも
のであって、本発明はこの実施例に限定されるものでは
ない。EXAMPLES The method of the present invention will be described in more detail with reference to the following examples, which show one embodiment of the method of the present invention, and the present invention is not limited to these examples. ..
【００２１】（実施例１）図１は本発明の一実施態様よ
りなる試験装置を例示するものである。容器側壁および
蓋部に保温用加熱ヒーター１を有する容器径（Ｄ）６０
０ｍｍ，容量５００kgの耐火煉瓦２を内張りした鉄製容
器３をターンテーブル５上に容器底部が空気冷却可能な
ごとく空間部を持って構成された架台４上にしっかり固
定して組立てた。またターンテーブルとは別に昇降可能
な架台６を立て、その架台上にモーター７を設置し、上
部から攪拌子径（ｄ）２７０ｍｍの攪拌子７を吊るし
た。このように形成した容器中に、不純物としてＦｅ
０．０５wt% 、Ｓｉ０．０３wt% を含有する原料溶融ア
ルミニウム５００ｋｇを投入し、６７０℃に保持し、タ
ーンテーブル回転数２５rpm 、攪拌子回転数２００rpm
で双方を逆に回転させ、凝固進行とともに容器底部の晶
出アルミニウムの表面と攪拌子の間隔を約１００ｍｍと
なる如く昇降可能な架台を上昇させ、１０時間かけて投
入原料アルミニウムの５０重量％が凝固析出するごとく
分別結晶化を行った。なおｄ／Ｄは０．４５であり、こ
の時の溶融アルミニウムの渦深さはほぼ零であり、溶融
アルミニウム表面状態は穏やかであった。実験終了後、
攪拌子の回転を停止し、攪拌子を溶融アルミニウムから
引き上げると共に、ターンテーブルを停止し、直ちに該
容器を傾転して、容器上部に存在する溶融アルミニウム
を流出せしめた。次いで、容器内に凝固析出したアルミ
ニウムを再溶解して精製アルミニウムとして分離取得し
た。このようにして得た精製アルミニウムを分析したと
ころ、不純物としてのＦｅは０．００５重量％、Ｓｉは
０．００６重量％であり、アルミニウム換算で２重量％
のドロス（アルミニウム酸化物）が生成していた。(Embodiment 1) FIG. 1 illustrates a test apparatus according to an embodiment of the present invention. Container diameter (D) 60 having heater 1 for heat retention on the container side wall and lid
An iron container 3 lined with a refractory brick 2 having a capacity of 0 mm and a capacity of 500 kg was firmly fixed and assembled on a turntable 5 on a pedestal 4 having a space so that the bottom of the container could be air-cooled. Separately from the turntable, a stand 6 that can be raised and lowered was set up, a motor 7 was installed on the stand, and a stirrer 7 having a stirrer diameter (d) of 270 mm was hung from above. In the container thus formed, Fe as an impurity
500 kg of molten aluminum containing 0.05 wt% and 0.03 wt% of Si was charged and kept at 670 ° C., turntable rotation speed 25 rpm, stirrer rotation speed 200 rpm.
Rotate both sides in reverse so that as the solidification progresses, the pedestal that can be moved up and down so that the distance between the surface of the crystallized aluminum at the bottom of the container and the stirrer is about 100 mm is raised. Fractional crystallization was performed so that solidification and precipitation occurred. The d / D was 0.45, the eddy depth of the molten aluminum at this time was almost zero, and the surface state of the molten aluminum was mild. After the experiment,
The rotation of the stirrer was stopped, the stirrer was pulled up from the molten aluminum, the turntable was stopped, the container was immediately tilted, and the molten aluminum existing in the upper part of the container was allowed to flow out. Then, the aluminum solidified and precipitated in the container was redissolved and separated and obtained as purified aluminum. When the purified aluminum thus obtained was analyzed, Fe as impurities was 0.005% by weight, Si was 0.006% by weight, and 2% by weight in terms of aluminum.
Dross (aluminum oxide) was produced.
【００２２】（比較例１）尚、比較のためターンテーブ
ルの回転操作を行なわないほかは上記と同一装置、同一
方法により分別結晶を行ない、精製アルミニウムを得
た。得られた精製アルミニウムを分析したところ、不純
物としてのＦｅは０．００８重量％、Ｓｉは０．００８
重量％であり、アルミニウム換算で５重量％のドロスが
生成していた。(Comparative Example 1) For comparison, except that the turntable was not rotated, fractional crystallization was carried out using the same apparatus and method as above to obtain purified aluminum. Analysis of the obtained purified aluminum revealed that Fe as an impurity was 0.008% by weight and Si was 0.008%.
% By weight, and dross of 5% by weight in terms of aluminum was produced.
【図１】は本発明の実施例において使用した試験装置の
断面図を示すものである。FIG. 1 is a sectional view of a test apparatus used in an embodiment of the present invention.
図中１は保温用加熱ヒーター、２は耐火煉瓦、３は鉄製
容器、４は架台、５はターンテーブル、６は昇降可能な
架台、７はモーター、８は攪拌子である。In the figure, 1 is a heating heater for heat retention, 2 is a refractory brick, 3 is an iron container, 4 is a stand, 5 is a turntable, 6 is a stand that can be raised and lowered, 7 is a motor, and 8 is a stirrer.
Claims (2)
し、該容器の上部および側部を制御された温度条件下に
保温管理し、該容器底部より冷却しながら、該容器をそ
の垂直軸を中心に回転せしめると同時に、該容器中の溶
融アルミニウムを該容器回転方向と逆方向に攪拌子によ
り回転せしめることにより容器底部に純度の高いアルミ
ニウムを分別析出せしめることを特徴とするアルミニウ
ムの精製法。1. A molten aluminum source material is held in a container, the upper and side parts of the container are kept warm under controlled temperature conditions, and the container is centered on its vertical axis while being cooled from the bottom of the container. A method for purifying aluminum, characterized in that the molten aluminum in the container is rotated by a stirrer in the direction opposite to the direction of rotation of the container at the same time as the aluminum is rotated to separate the highly pure aluminum at the bottom of the container.
容器径、ｄ：攪拌子径、Ｎ：容器回転数、ｎ：攪拌子回
転数を示す。）が１〜４．５であることを特徴とする請
求項１記載のアルミニウムの精製法。2. (D 4 N) / (d 4 n) (wherein D:
Container diameter, d: stirrer diameter, N: container rotation speed, n: stirrer rotation speed. ) Is 1 to 4.5. The method for purifying aluminum according to claim 1, wherein.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28582091A JP3370689B2 (en) | 1991-10-31 | 1991-10-31 | Aluminum purification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28582091A JP3370689B2 (en) | 1991-10-31 | 1991-10-31 | Aluminum purification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05125462A true JPH05125462A (en) | 1993-05-21 |
| JP3370689B2 JP3370689B2 (en) | 2003-01-27 |
Family
ID=17696513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28582091A Expired - Lifetime JP3370689B2 (en) | 1991-10-31 | 1991-10-31 | Aluminum purification method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3370689B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6398845B1 (en) | 2000-02-10 | 2002-06-04 | Sumitomo Chemical Company, Limited | Method for purifying aluminum |
| CN106480323A (en) * | 2016-11-02 | 2017-03-08 | 昆明冶金研究院 | A kind of continuous segregation of up-drawing method purifies device and its method for purification of refined aluminium |
-
1991
- 1991-10-31 JP JP28582091A patent/JP3370689B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6398845B1 (en) | 2000-02-10 | 2002-06-04 | Sumitomo Chemical Company, Limited | Method for purifying aluminum |
| CN106480323A (en) * | 2016-11-02 | 2017-03-08 | 昆明冶金研究院 | A kind of continuous segregation of up-drawing method purifies device and its method for purification of refined aluminium |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3370689B2 (en) | 2003-01-27 |
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