JPH01306529A - Continuous refining method of metal - Google Patents
Continuous refining method of metalInfo
- Publication number
- JPH01306529A JPH01306529A JP13865388A JP13865388A JPH01306529A JP H01306529 A JPH01306529 A JP H01306529A JP 13865388 A JP13865388 A JP 13865388A JP 13865388 A JP13865388 A JP 13865388A JP H01306529 A JPH01306529 A JP H01306529A
- Authority
- JP
- Japan
- Prior art keywords
- primary crystal
- molten metal
- roll
- crystal nuclei
- metal
- 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
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 93
- 239000002184 metal Substances 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims description 20
- 238000007670 refining Methods 0.000 title claims description 9
- 239000013078 crystal Substances 0.000 claims abstract description 42
- 239000012535 impurity Substances 0.000 claims abstract description 27
- 239000000155 melt Substances 0.000 claims abstract description 19
- 238000005096 rolling process Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims description 23
- 239000007790 solid phase Substances 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 abstract description 8
- 238000002844 melting Methods 0.000 abstract description 8
- 210000001787 dendrite Anatomy 0.000 abstract description 2
- 238000000746 purification Methods 0.000 description 31
- 150000002739 metals Chemical class 0.000 description 15
- 238000011084 recovery Methods 0.000 description 6
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 238000005204 segregation Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- AMHXPZLIADYCSB-ZCFIWIBFSA-N (2R)-2-amino-2-formyl-4-methylsulfanylbutanoic acid Chemical compound CSCC[C@@](N)(C=O)C(O)=O AMHXPZLIADYCSB-ZCFIWIBFSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明は金属の連続精製法に関するものであり、不純物
を含む金属を連続的に精製して、ボンディングワイヤー
、メモリーディスク等の電子機器材料等に用いられる高
純度金属を製造する方法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for continuously refining metals, in which metals containing impurities are continuously refined to produce electronic device materials such as bonding wires and memory disks. The present invention relates to a method for producing high-purity metals used in
近年、電子機器の超小型化、精密化等に伴い、そこに使
用される金属材料には導電性、柔軟性、表面特性等の一
層の向上が求められており、高純度金属をヘースとする
材料開発が年々拡大してきている。In recent years, with the miniaturization and precision of electronic devices, the metal materials used there are required to further improve conductivity, flexibility, surface properties, etc. Material development is expanding year by year.
金属を精製する方法としては、電解法と偏析凝固法とが
あるが、微量不純物を除去するには偏析凝固法が適して
いる。この偏析凝固法は溶質の分配法則、即ち溶湯から
固相が形成される際、溶質は固相から液相側へ排出され
、初期濃度Ｃ０に対して、形成された固相濃度Ｃ１と固
相周辺の残留融液濃度Ｃ，との関係が、Ｃ，＞Ｃ，＞Ｃ
，となる法則を利用したものである。即ち不純物を含む
溶融金属を冷却凝固させると、初めに純度の高い初晶核
が晶出し、不純物は残った溶融金属中に排出されるが、
この純度の高い初晶核のみを選択的に回収する事によっ
て金属を精製する方法である。Methods for refining metals include electrolytic methods and segregation solidification methods, and segregation solidification methods are suitable for removing trace impurities. This segregation solidification method is based on the distribution law of solutes, that is, when a solid phase is formed from the molten metal, the solute is discharged from the solid phase to the liquid phase side. The relationship with the surrounding residual melt concentration C, is C,>C,>C
, which makes use of the law that . In other words, when a molten metal containing impurities is cooled and solidified, highly pure primary crystal nuclei crystallize first, and the impurities are discharged into the remaining molten metal.
This is a method of refining metals by selectively collecting only these highly pure primary crystal nuclei.
従来の偏析凝固法においては、例えばＡＮを精製しよう
とする場合、溶融Ａｌ中に冷却体を浸漬し、該冷却体の
表面に純度の高いＡｎ初晶核を晶出させるが、この際Ｓ
ｉ、Ｆ ｅ、Ｃｕ、Ｍｇ等のＡ２と共晶を生成する不
純物が溶融／ｌ中に放出されて、初晶核の樹枝状高量の
不純物４度が高くなり、純化された初晶Ａ２を再度汚染
し、精製効率を低下させる。これを防ぐ為に前記冷却体
を回転させて、溶融へ２中に放出された不純物を初晶核
との界面近傍から溶融Ａｌ中に拡散させなからＡｐ、を
晶出させて、高純度Ａ２を回収する方法が知られている
。In the conventional segregation solidification method, when purifying AN, for example, a cooling body is immersed in molten Al, and highly pure An primary crystal nuclei are crystallized on the surface of the cooling body.
Impurities that form eutectic with A2, such as i, Fe, Cu, Mg, etc., are released into the melt/l, and the dendritic high impurity 4 degree of the primary crystal nucleus becomes high, and the purified primary crystal A2 re-contaminate and reduce purification efficiency. In order to prevent this, the cooling body is rotated to prevent the impurities released into the melt from diffusing into the molten Al from near the interface with the primary crystal nucleus, and to crystallize Ap, resulting in high purity A2. There are known methods to recover.
而して冷却体表面に晶出した高純炭金属の回収方法とし
ては、溶融金属中で晶出金属を間欠的にかき落として処
理槽の底部に沈澱させ、上部の融液を排出後に前記晶出
金属を回収する方法と、冷却体を溶融金属中から取り出
して晶出金属を回収する方法とがあるが、いずれもバッ
チ処理となる為効率が悪く、又回収後に残った溶融金属
中には不純物が濃縮されており、前記高純度金属の回収
操作を繰り返し行なうと、回収される金属の純度が次第
に層下する為、純度の高い金属を連続的に得る事は不可
能であった。As a method for recovering high-purity carbon metal crystallized on the surface of the cooling body, the crystallized metal is intermittently scraped off in the molten metal and deposited at the bottom of the treatment tank, and after the upper melt is discharged, the crystallized metal is collected. There is a method of recovering the extracted metal and a method of removing the cooling body from the molten metal and recovering the crystallized metal, but both are inefficient because they are batch processes, and the molten metal remaining after recovery is Impurities are concentrated, and when the above-mentioned high-purity metal recovery operation is repeated, the purity of the recovered metal gradually decreases, making it impossible to continuously obtain high-purity metal.
本発明は上記の点に鑑み鋭意検討の結果なされたもので
あり、その目的とするところは、不純物を含む溶融金属
を連続的に精製して、高純度金属を得る方法を提供する
事である。The present invention was made as a result of intensive studies in view of the above points, and its purpose is to provide a method for continuously refining molten metal containing impurities to obtain high-purity metal. .
即ち本発明は、不純物を含む溶融金属中に、その表面温
度が溶融金属の固相線温度以上で液相線温度以下の温度
範囲内に内部冷却によりコントロールされたロールの一
部を回転させながら浸漬して、前記浸漬されたロール表
面上に溶融金属の初晶核を生成させ、該初晶核並びに初
晶核の間隙に捕捉された融液をロールの回転により、連
続的に溶融金属外に搬送し、前記冷却ロールとこれに相
対する様に配置された圧延ロールとで、初晶核からなる
固相を圧延し、咳初晶核の間隙に捕捉された融液を絞り
出して系外に排出する操作を少なく共１回行なう事を特
徴とする金属の連続精製法である６
本発明において、冷却ロールの表面温度が溶融金属の固
相線温度以下であると、初晶核から排出された不純物が
ａ縮された融液も冷却されて凝固し、固相として回収さ
れる為得られた固相の純度が低下するので、前記冷却ロ
ールの表面温度は溶融金属の固相線温度以上に保持する
必要がある。That is, the present invention provides a method for rotating a part of the roll that is controlled by internal cooling so that the surface temperature of the molten metal containing impurities is within a temperature range of not less than the solidus temperature of the molten metal and not more than the liquidus temperature of the molten metal. The primary crystal nuclei of the molten metal are generated on the surface of the immersed roll, and the primary crystal nuclei and the melt trapped in the gaps between the primary crystal nuclei are continuously removed from the molten metal by rotation of the roll. The solid phase consisting of primary crystal nuclei is rolled by the cooling roll and a rolling roll placed opposite to the cooling roll, and the melt trapped in the gaps between the primary crystal nuclei is squeezed out of the system. 6. In the present invention, when the surface temperature of the cooling roll is below the solidus temperature of the molten metal, the primary crystal nuclei are discharged. Since the melt in which the impurities are condensed is also cooled and solidified and recovered as a solid phase, the purity of the obtained solid phase decreases, so the surface temperature of the cooling roll is set to the solidus temperature of the molten metal. It is necessary to maintain more than that.
本発明方法においては溶融金属中に浸漬した回転ロール
の表面温度を、該溶融金属の固相線温度以上で液相線温
度以下の温度範囲内にコントロールしているので、前記
浸漬された冷却ロール表面上に溶融金属の初晶核が晶出
する。この際排出される不純物がｆＡ縮された融液は、
初晶核のＰ４技状品間隙に存在するが、ロール表面温度
が固相線温度以上に保たれている為、凝固する事なく初
晶核の間隙に捕捉されたままロールの回転により溶融金
属外に搬送される。しかる後この初晶核は前記冷却ロー
ルとこれに相対する様に配置された圧延ロールとで圧延
されるので、前記初晶核の間隙に捕捉された融液は絞り
出されて連続的に系外に排出される。従って母液である
溶融金属の不純物濃度を高める事なく、高純度金属を連
続して得る事が可能である。In the method of the present invention, the surface temperature of the rotating roll immersed in the molten metal is controlled within a temperature range of above the solidus temperature of the molten metal and below the liquidus temperature of the molten metal. Primary nuclei of molten metal crystallize on the surface. The melt in which the impurities discharged at this time are reduced to fA is
They exist in the gaps between the P4 grains of primary crystal nuclei, but since the roll surface temperature is maintained above the solidus temperature, the molten metal remains trapped in the gaps of the primary crystal nuclei without solidifying as the roll rotates. transported outside. Thereafter, the primary crystal nuclei are rolled by the cooling roll and a rolling roll placed opposite to the cooling roll, so that the melt trapped in the gaps between the primary crystal nuclei is squeezed out and continuously rolled into a system. is discharged outside. Therefore, it is possible to continuously obtain high purity metal without increasing the impurity concentration of the molten metal that is the mother liquor.
〔実施例１〕 次に本発明を実施例により更に具体的に説明する。[Example 1] Next, the present invention will be explained in more detail with reference to Examples.
第１図は本発明の実施に使用した金属の連続精製装置の
一例を示す概略断面図であって、ｌは溶湯を連続的に出
湯可能な金属溶解炉、２Ａは溶湯の温度調整装置を具備
した高純化処理槽、３Ａは内部冷却された回転ロール、
４．４Ａは不純物を含む溶融金属、５Ａは精製された高
純度の初晶核、６Ａは初品の樹技状品間隙に排出された
不純物が濃縮された融液、７Ａは圧延ロール、８Ａは固
相から絞り出された不純物が濃縮された融液、９Ａは樋
、ＩＯＡは隔壁である。FIG. 1 is a schematic cross-sectional view showing an example of a continuous metal refining apparatus used in the implementation of the present invention, in which 1 is a metal melting furnace capable of continuously tapping molten metal, and 2A is equipped with a molten metal temperature adjustment device. 3A is an internally cooled rotating roll,
4.4A is a molten metal containing impurities, 5A is a refined high-purity primary crystal nucleus, 6A is a melt with concentrated impurities discharged into the gaps of the initial wood product, 7A is a rolling roll, 8A 9A is a gutter, and IOA is a partition wall.
溶融金属４としてＣｕ−８ｗｔ％Ｓｎ合金（液相線温度
： １０３２℃、固相線温度：８７５°Ｃ）を金属溶解
炉１で溶解した後、高純化処理槽２Ａに転湯し、該高純
化処理槽２Ａ内での溶融金属４Ａの温度を１０７０°Ｃ
に保持した。次に内部を空冷した外径４５０ｍｍφの回
転ロール３Ａを、その円周の約１／４が溶融金属４Ａに
つかる様にセントシた。前記回転ロール３Ａにより溶融
金属４Ａが冷却されて、ロール表面に高純度の初晶核５
Ａが晶出し、ロールの回転により溶融金属中を移動する
間に次第に成長して、帯状の初晶核（固相）５Ａが得ら
れた。この初晶核５Ａの樹枝状晶間隙には、初晶核５Ａ
から排出されたＳｎｆ：Ａ度の高い融液６Ａが含まれて
おり、ロール３Ａの回転によって初晶核５Ａと共に溶湯
外に排出される。After melting a Cu-8wt%Sn alloy (liquidus temperature: 1032°C, solidus temperature: 875°C) as the molten metal 4 in the metal melting furnace 1, it was transferred to the high purification treatment tank 2A, and the high purity The temperature of molten metal 4A in purification treatment tank 2A is set to 1070°C.
was held at Next, a rotary roll 3A having an outer diameter of 450 mm and whose inside was air-cooled was centrifuged so that about 1/4 of its circumference was covered with the molten metal 4A. The molten metal 4A is cooled by the rotating roll 3A, and highly pure primary crystal nuclei 5 are formed on the roll surface.
A crystallized and gradually grew while moving in the molten metal due to the rotation of the roll, to obtain a band-shaped primary crystal nucleus (solid phase) 5A. In the dendrite gap of this primary crystal nucleus 5A, the primary crystal nucleus 5A
The melt 6A with a high Snf:A degree discharged from the melt is contained, and is discharged out of the molten metal along with the primary crystal nuclei 5A by the rotation of the roll 3A.
次に前記冷却ロール３Ａとこれに相対する様に配置され
た圧延ロール７Ａとで、初晶核からなる固相５Ａを圧延
し、該初晶核５Ａの間隙に捕捉されたＳｎ１度の高い融
液６Ａを絞り出して、高純度Ｃｕだけを回収する。Next, the solid phase 5A consisting of primary crystal nuclei is rolled by the cooling roll 3A and a rolling roll 7A disposed opposite thereto, and the Sn1 degree high fusion captured in the gaps of the primary crystal nuclei 5A is rolled. Squeeze out liquid 6A to collect only high-purity Cu.
この際、絞り出されたＳｎ濃度の高い融液８Ａは自由落
下するので、圧延ロール７Ａの下に設けた樋９Ａに受け
て系外に排出し、母液である溶融金属４Ａの汚染を防止
した。At this time, the squeezed melt 8A with high Sn concentration fell freely, so it was received by a gutter 9A provided under the rolling roll 7A and discharged out of the system to prevent contamination of the molten metal 4A, which is the mother liquor. .
ここで高純度処理槽２Ａ内の湯面高さが一定となる様に
、金属溶解炉ｌから連続的に転湯する事によって、高純
度金属を連続的に得る事が可能となる。この転湯により
生じる高純度処理槽２Ａ内の場面の波動により、冷却ロ
ール３Ａの表面に生成した初晶核５Ａの隙間に含まれる
高濃度Ｓｎの融液６Ａが拡散して、溶融金属４Ａ中の５
ｎｆｉ度を高める事を防ぐ為、隔壁１０Ａを設けて、前
記場面の波動が冷却ロール３Ａの部分まで伝わらない様
にした。Here, by continuously turning the melt from the metal melting furnace 1 so that the height of the hot water level in the high purity treatment tank 2A is constant, it becomes possible to continuously obtain high purity metal. Due to the wave motion inside the high-purity treatment tank 2A caused by this turning, the high-concentration Sn melt 6A contained in the gaps between the primary crystal nuclei 5A generated on the surface of the cooling roll 3A is diffused into the molten metal 4A. 5
In order to prevent the degree of nfi from increasing, a partition wall 10A was provided to prevent the wave motion in the above-mentioned scene from being transmitted to the cooling roll 3A.
前記連続精製装置により得られる高純度金属（Ｃｕ）中
のＳｎｌは、溶融金属４Ａの温度を一定とした場合には
、冷却ロール３Ａの表面温度及び回転速度に依存する。Snl in the high purity metal (Cu) obtained by the continuous refining device depends on the surface temperature and rotation speed of the cooling roll 3A when the temperature of the molten metal 4A is constant.
そこでこれらの量を変化させて、Ｃｕ−８ｗｔ％Ｓｎ合
金の純化実験を行い、得られた高純度金属（Ｃｕ）中の
５ｎｌｉを第１表に示した。Therefore, an experiment was conducted to purify a Cu-8wt%Sn alloy by changing these amounts, and Table 1 shows 5nli in the obtained high-purity metal (Cu).
第１表から明らかな様に、ロール表面温度が８００℃と
同相線温度よりも低い場合は、回収される金属中のＳｎ
濃度が高く、純化の効率が悪い。As is clear from Table 1, when the roll surface temperature is 800°C, which is lower than the in-phase line temperature, Sn in the recovered metal is
High concentration and poor purification efficiency.
この原因は、初晶核から排出された高４度Ｓｎ融液も冷
却されて凝固し、固相として回収される為であり、ロー
ル速度が遅い場合にはこの凝固がより進行する為、純化
の効率が一層低下する。The reason for this is that the high 4 degree Sn melt discharged from the primary crystal nucleus is also cooled and solidified, and is recovered as a solid phase.If the roll speed is slow, this solidification will progress further, resulting in purification. efficiency is further reduced.
一方ロール表面温度を１０００ ′Ｃと高くした場合に
は、ロール周速が０．２ｍ／ｍｉｎと遅い時は、初晶核
が再溶解して回収不能となる。又前記ロール周速が１．
２ｍ／ｍｉｎと速い時は、固相が連続して帯状となるま
で生成されず、やはり回収不能であった。ロール温度が
９００〜９５０°Ｃの場合も、ロール周速が速い程回収
された金属中のＳｎ濃度が低くなっており、固相が連続
して生成される範囲内で冷却ロールの回転速度をなるべ
く速くする事により、高純度金属を効率良く回収する事
が可能である。On the other hand, when the roll surface temperature is as high as 1000'C and the roll circumferential speed is as slow as 0.2 m/min, the primary crystal nuclei are redissolved and cannot be recovered. Further, the roll circumferential speed is 1.
When the speed was as fast as 2 m/min, the solid phase was not produced until it became a continuous band, and it was also impossible to recover it. Even when the roll temperature is 900 to 950°C, the faster the roll circumferential speed is, the lower the Sn concentration in the recovered metal is. By making the process as fast as possible, it is possible to efficiently recover high-purity metals.
〔実施例２〕
本実施例は前記実施例１と同じ構造の高純化処Ｆｌ！ｌ
ｒを２個連結した場合のものであり、第２図に装置の概
略断面図を示す。[Example 2] This example uses a high purification process Fl! having the same structure as the above-mentioned Example 1. l
Fig. 2 shows a schematic cross-sectional view of the device.
本実施例では、Ａ／！−５ｗＬ％Ｓｉ合金（液相線温度
： ６２８ ’Ｃ１固相線温度＝５７７°Ｃ）を金属溶
解炉ｌで溶解した後、第一高純化処理装置２０Ａの高純
化処理槽２Ａに転湯し、該高純化処理槽２Ａ内での溶融
金属４Ａの温度を６７０ ’Ｃに保持した。これに表面
温度６２０°Ｃ１周速０．７ ｍ ／ｍｉｎとした冷却
ロール３Ａをセットして、前記実施例１と同様にして高
純度金属を回収した。日記回収された高純度金属中の３
ｉ１は１．４ ｗ Ｌ％であった。In this example, A/! -5wL%Si alloy (liquidus temperature: 628' C1 solidus temperature = 577°C) was melted in metal melting furnace 1, and then transferred to high purification treatment tank 2A of first high purification treatment equipment 20A. The temperature of the molten metal 4A in the high purification treatment tank 2A was maintained at 670'C. A cooling roll 3A with a surface temperature of 620° C. and a circumferential speed of 0.7 m 2 /min was set thereon, and high-purity metal was recovered in the same manner as in Example 1. 3 of the high purity metals recovered in the diary
i1 was 1.4 wL%.
ここで回収された直後の固相の温度は、約５６０°Ｃと
高温であり、少ないエネルギーで再溶解可能な事に注目
して、第二高純化処理装置２０）３の設置を行なった。The temperature of the solid phase immediately after recovery is as high as about 560° C., and the second high purification treatment device 20) 3 was installed, noting that it can be remelted with little energy.
即ち第一高純化処理装置２ＯＡから連続的に製出される
高純度金属をそのまま第二高純化処理装置２０Ｂに入れ
て再溶解させ、高純化処理槽２Ｂ内の溶湯４Ｂの温度を
６８０°Ｃにコントロールした。これに表、頂温度６４
０ ”Ｃ２周速０．６ｍ／ｍ：ｎとした冷却ロール３Ｂ
をセットして、［１１１記と同様の高純化処理を行ない
、Ｓｉ星が０．４ ｗ ｔ％と高純度化されたＡ２を回
収出来た。That is, the high-purity metal continuously produced from the first high-purification treatment apparatus 2OA is directly put into the second high-purification treatment apparatus 20B and remelted, and the temperature of the molten metal 4B in the high-purification treatment tank 2B is raised to 680°C. I controlled it. On this table, the top temperature is 64
0”C2 peripheral speed 0.6m/m:n cooling roll 3B
was set, and the same purification treatment as in Section 111 was performed, and A2 with a highly purified Si star content of 0.4 wt% was recovered.
ここで冷却ロール３Ｂの表面に生成した初晶核５Ｂの間
隙に含まれる不純物が濃縮された融液６Ｂは圧延ロール
３Ｂにより絞り出したが、前記絞り出された融ｆｉ８Ｂ
はＳｉを２．２ｗ ｔ％含んでいるｌｒから樋９Ｂに受
けて第一高純化処理装置２０Ａに戻し、回収効率の向上
をはかった。Here, the melt 6B in which the impurities contained in the gaps of the primary crystal nuclei 5B generated on the surface of the cooling roll 3B are concentrated is squeezed out by the rolling roll 3B.
was received from lr containing 2.2 wt % Si in the gutter 9B and returned to the first high purification treatment device 20A, in order to improve the recovery efficiency.
又第一高純化処理装置２０Ａと第二高純化処理装置２０
Ｂとでは製出量が必ずしも一敗しない事から、第二高純
化処理装置２０Ｂにオーバーフロー樋ｌｌを設け、オー
バーフローした溶湯を第一１高純化処理装置２０Ａに戻
した。Also, the first high purification treatment device 20A and the second high purification treatment device 20
Since the production volume is not necessarily the same with B, an overflow gutter was provided in the second high purification treatment apparatus 20B, and the overflowing molten metal was returned to the first high purification treatment apparatus 20A.
以上に述べた様に、本実施例ではＡＮ−５ｗＬ％Ｓｉ合
金から第一高純化処理装置２ＯＡによって１．４ ｗ
ｔ％Ｓｉに、第二高純化処理装置２０Ｂによって０．４
ｗ ｔ％Ｓｉに高純度化されたＡ２を回収する事が出
来た。As mentioned above, in this example, 1.4w
t%Si to 0.4% by the second high purification processing device 20B.
A2 highly purified to wt% Si could be recovered.
即ち本実施例から明らかな様に、複数個の高純化処理装
置を連続して設置する事により、各処理装置で回収され
る高純度金属中の不純物間を漸減させる事が出来、多量
の不純物を含む金属から高純度金属を連続して回収する
事が可能である。In other words, as is clear from this example, by installing a plurality of high-purification treatment devices in succession, it is possible to gradually reduce the amount of impurities in the high-purity metal recovered by each treatment device. It is possible to continuously recover high-purity metals from metals containing
この場合、高温状態で回収された固相を、次の高純化処
理槽で再溶解するので、従来のハツチ処理による高純化
処理を繰り返していた場合に比べて、エネルギーコスト
が大幅に低減する。In this case, the solid phase recovered at high temperature is redissolved in the next high-purification treatment tank, so energy costs are significantly reduced compared to the case where high-purification treatment using conventional hatch processing is repeated.
又第二高純化処理装置以降においては、高純度金属を回
収する際に生じる不純物が濃縮した融液を一つ前の高純
化処理装置に戻して、再度高純度金属の回収を行なう事
が出来るので、高純度金属の回収効率が大幅に向上する
。In addition, after the second high-purification processing equipment, the melt containing concentrated impurities generated when recovering high-purity metals can be returned to the previous high-purification processing equipment to recover high-purity metals again. Therefore, the recovery efficiency of high-purity metals is greatly improved.
本発明の方法によれば、不純物を含む溶融金属を連続的
に精製して、高純度金属を得る事が可能である。しかも
高純化処理装置を複数個連続させる事により多量の不純
物を含む金属から高純度金属を連続して回収する事が出
来ると共に、エネルギーコストの大幅な低減と、高純度
金属の回収効・卜の大幅な向−ヒを図れる等工業上顕著
な効果を奏するものである。According to the method of the present invention, it is possible to continuously refine molten metal containing impurities to obtain high purity metal. Furthermore, by connecting multiple high-purification treatment devices in series, high-purity metals can be continuously recovered from metals containing a large amount of impurities, and energy costs can be significantly reduced and the recovery efficiency and performance of high-purity metals can be increased. This has significant industrial effects, such as the ability to significantly improve energy efficiency.
第１図及び第２図は、本発明の実施に使用する高純化処
理装置の一例を示す概略断面図である。
ｌ−金属溶解炉、２Ａ、２Ｂ−高純化処理槽、３Ａ、３
Ｂ−内部冷却ロール、４．４ Ａ、 ４ Ｂ−溶融金属
、５Ａ、５Ｂ〜高純度の初晶核、６Ａ、６Ｂ−不純物が
濃縮された融液、７Ａ、７Ｂ−圧延ロール、８Ａ、８Ｂ
−固相から絞り出された不純物が濃縮された融液、９Ａ
、９Ｂ−樋、ＩＯＡ、１０ Ｂ−ｍ−隔壁、ｌｌ−オー
バーフロー樋、２０高純化処理装置、２０Ａ〜第一高純
化処理装置、２０Ｂ 第二高純化処理装置。
特許出願人 古河電気工業株式会社
手続補正書（自発）
平成 元年１月１９日
１、事件の表示 特願昭６３−１３８６５３号２、発
明の名称 金属の連続精製法
３、補正をする者
事件との関係 特許出願人
住 所 〒１００東京都千代田区丸の内２丁目６番１
号４、補正の対象 明細書の「発明の詳細な説明」の
欄。
−）、
′ｔ・て・゛
ｊ、−−”、、 。（，
５、補正の内容
（１）明細書の第９頁第１表を別紙のとおり訂正する。
（２）明細書の第１２頁第６行にｒ圧延ロール３ＢＪと
あるをｒ圧延ロール７ＢＪと訂正する。FIG. 1 and FIG. 2 are schematic cross-sectional views showing an example of a high purification processing apparatus used in carrying out the present invention. l-Metal melting furnace, 2A, 2B-High purification treatment tank, 3A, 3
B- Internal cooling roll, 4.4 A, 4 B- Molten metal, 5A, 5B ~ High purity primary crystal nucleus, 6A, 6B- Melt with concentrated impurities, 7A, 7B- Rolling roll, 8A, 8B
- Melt liquid with concentrated impurities squeezed out from the solid phase, 9A
, 9B-gutter, IOA, 10 B-m-partition, ll-overflow gutter, 20 high-purification processing device, 20A-first high-purification processing device, 20B second high-purification processing device. Patent applicant: Furukawa Electric Co., Ltd. Procedural amendment (voluntary) January 19, 1989 1. Case description: Japanese Patent Application No. 63-138653 2. Title of invention: Continuous metal refining method 3. Case made by the person making the amendment Relationship with Patent applicant address 2-6-1 Marunouchi, Chiyoda-ku, Tokyo 100
Item 4: Subject of amendment: “Detailed Description of the Invention” column of the specification. -), 't・te・゛j,--'',, (, 5. Contents of amendment (1) Table 1 on page 9 of the specification is corrected as shown in the attached sheet. (2) Section 1 of the specification In the 6th line of page 12, "r rolling roll 3BJ" is corrected to "r rolling roll 7BJ."
Claims (1)
固相線温度以上で液相線温度以下の温度範囲内に内部冷
却によりコントロールされたロールの一部を回転させな
がら浸漬して、前記浸漬されたロール表面上に溶融金属
の初晶核を生成させ、該初晶核並びに初晶核の間隙に捕
捉された融液をロールの回転により、連続的に溶融金属
外に搬送し、前記冷却ロールとこれに相対する様に配置
された圧延ロールとで、初晶核からなる固相を圧延し、
該初晶核の間隙に捕捉された融液を絞り出して系外に排
出する操作を少なく共１回行なう事を特徴とする金属の
連続精製法。A part of the roll whose surface temperature is controlled by internal cooling within a temperature range of above the solidus temperature of the molten metal and below the liquidus temperature of the molten metal is immersed in the molten metal containing impurities while rotating. Primary crystal nuclei of the molten metal are generated on the surface of the immersed roll, and the primary crystal nuclei and the melt trapped in the gaps between the primary crystal nuclei are continuously conveyed out of the molten metal by the rotation of the roll. A solid phase consisting of primary crystal nuclei is rolled by a cooling roll and a rolling roll placed opposite to the cooling roll,
A continuous metal refining method characterized in that an operation of squeezing out the melt trapped in the gaps between the primary crystal nuclei and discharging it out of the system is performed at least once.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13865388A JPH01306529A (en) | 1988-06-06 | 1988-06-06 | Continuous refining method of metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13865388A JPH01306529A (en) | 1988-06-06 | 1988-06-06 | Continuous refining method of metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01306529A true JPH01306529A (en) | 1989-12-11 |
Family
ID=15227012
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13865388A Pending JPH01306529A (en) | 1988-06-06 | 1988-06-06 | Continuous refining method of metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01306529A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH062054A (en) * | 1992-06-24 | 1994-01-11 | Showa Alum Corp | Production of high purity aluminum |
| JP2008163418A (en) * | 2006-12-28 | 2008-07-17 | Showa Denko Kk | Metal-refining method and apparatus, refined metal, casting, metal product and electrolytic capacitor |
| JP2009167526A (en) * | 2007-12-20 | 2009-07-30 | Showa Denko Kk | Method of purifying substance and apparatus for purifying substance |
| ES2736727A1 (en) * | 2018-06-28 | 2020-01-07 | Cobre Las Cruces S A U | Metal cementing apparatus and continuous cementing process by means of it (Machine-translation by Google Translate, not legally binding) |
| US11603577B2 (en) | 2019-07-08 | 2023-03-14 | Cobre Las Cruces, S.A.U. | Metal cementing apparatus and continuous cementation method by means of same |
-
1988
- 1988-06-06 JP JP13865388A patent/JPH01306529A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH062054A (en) * | 1992-06-24 | 1994-01-11 | Showa Alum Corp | Production of high purity aluminum |
| JP2008163418A (en) * | 2006-12-28 | 2008-07-17 | Showa Denko Kk | Metal-refining method and apparatus, refined metal, casting, metal product and electrolytic capacitor |
| JP2009167526A (en) * | 2007-12-20 | 2009-07-30 | Showa Denko Kk | Method of purifying substance and apparatus for purifying substance |
| ES2736727A1 (en) * | 2018-06-28 | 2020-01-07 | Cobre Las Cruces S A U | Metal cementing apparatus and continuous cementing process by means of it (Machine-translation by Google Translate, not legally binding) |
| US11603577B2 (en) | 2019-07-08 | 2023-03-14 | Cobre Las Cruces, S.A.U. | Metal cementing apparatus and continuous cementation method by means of same |
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