JPH10158754A - Production of high-purity bismuth and apparatus for production - Google Patents
Production of high-purity bismuth and apparatus for productionInfo
- Publication number
- JPH10158754A JPH10158754A JP8330367A JP33036796A JPH10158754A JP H10158754 A JPH10158754 A JP H10158754A JP 8330367 A JP8330367 A JP 8330367A JP 33036796 A JP33036796 A JP 33036796A JP H10158754 A JPH10158754 A JP H10158754A
- Authority
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- Japan
- Prior art keywords
- bismuth
- purity
- raw material
- crucible
- vacuum
- Prior art date
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Classifications
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- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、純度９９．９９％
程度の市販金属ビスマス等から真空蒸留精製により、純
度９９．９９９９％以上の高純度ビスマスを製造する方
法とその装置に関する。TECHNICAL FIELD The present invention relates to a 99.99% purity.
The present invention relates to a method and apparatus for producing high-purity bismuth having a purity of 99.9999% or more by vacuum distillation purification from a commercially available metal bismuth or the like.
【０００２】[0002]
【従来の技術】一般に金属ビスマスは、自然ソウエンや
キソウエン等の鉱石を比重選鉱により濃縮して、反射炉
内で炭素、鉄、融剤を添加して粗ビスマスを得、次いで
この粗ビスマスを精製して金属ビスマスとする方法が知
られている。2. Description of the Related Art Generally, metallic bismuth is obtained by concentrating natural ore or xenium ore by specific gravity separation, adding carbon, iron and a flux in a reverberatory furnace to obtain crude bismuth, and then purifying the crude bismuth. Is known to produce metallic bismuth.
【０００３】その他の方法としては、鉛電解におけるア
ノードスライムから回収する方法も知られているが、こ
の方法は、上記アノードスライムを反射炉で溶融してス
ラグと金属分とに分離し、得られた金属分中のビスマス
をさらに反射炉中で酸化処理してスラグと金銀地金とに
分離する。さらにこのスラグを反射炉内で還元して粗ビ
スマスを得る方法である。As another method, a method of recovering from anode slime in lead electrolysis is also known. In this method, the anode slime is melted in a reverberatory furnace, separated into slag and metal, and obtained. The bismuth in the metal content is further oxidized in a reverberatory furnace to separate it into slag and gold and silver bullion. Further, this is a method in which this slag is reduced in a reverberatory furnace to obtain crude bismuth.
【０００４】こららの方法によって得られた粗ビスマス
を原料として、帯溶融法や電解精製法によって純度を上
げ、現在では９９．９９−９９．９９９％の純度を有す
る金属ビスマスが市販されている。Using the crude bismuth obtained by these methods as a raw material, the purity is increased by a zone melting method or an electrolytic refining method. At present, metal bismuth having a purity of 99.99-99.999% is commercially available. .
【０００５】[0005]
【発明が解決しようとする課題】上記の帯溶融法や電解
精製法によって得られる金属ビスマスの純度は９９．９
９〜９９．９９９％程度であり、電解法によるビスマス
中の不純物として硫黄、銀はいずれも２０ppm 以上含ま
れていた。The purity of the metal bismuth obtained by the above-mentioned band melting method and electrolytic refining method is 99.9.
It was about 9-99.999%, and both sulfur and silver were contained as impurities in bismuth by electrolysis at 20 ppm or more.
【０００６】上記の金属をさらにゾーン精製法によって
精製する手段もあるが、精製後の切断加工の必要性と汚
染の危険があることから、精製時の処理量の制約や精製
ビスマスをインゴットにする場合には鋳造時の不純物の
混入による汚染の問題があった。There is also a means for purifying the above metals by a zone refining method. However, because of the necessity of cutting after the refining and the danger of contamination, there is a restriction on a processing amount at the time of refining and a refined bismuth is made into an ingot. In such a case, there is a problem of contamination due to contamination of impurities during casting.
【０００７】したがって本発明の目的は、従来の電解溶
融法ではビスマスとの完全分離が困難であったアルミニ
ウム、硫黄、ニッケル、銀、鉛等を分離できる新規な精
製手段を開発することによって純度９９．９９９９％以
上の高純度ビスマスを直接インゴット状で製造できる製
造方法と製造装置を提供することにある。[0007] Accordingly, an object of the present invention is to develop a new purification means capable of separating aluminum, sulfur, nickel, silver, lead, etc., which has been difficult to completely separate from bismuth by the conventional electrolytic melting method. An object of the present invention is to provide a manufacturing method and a manufacturing apparatus capable of directly manufacturing high-purity bismuth of 0.9999% or more in an ingot shape.
【０００８】[0008]
【課題を解決するための手段】本発明者らは上記目的を
達成すべく鋭意研究の結果、外筒と内筒からなる二重の
石英筒で封体した内部に原料ビスマスが装入される原料
るつぼとこれに連接して設けられる回収鋳型を配置して
真空蒸留を行い、蒸発したビスマスを石英筒面に凝縮さ
せ、これを回収鋳型に回収するようにすれば、従来より
も簡易な構造でしかも精製から鋳造までを一回の連続工
程で処理できる上、汚染が少ないので、含有する不純物
が１ppm 未満の純度９９．９９９９％以上の高純度ビス
マスが得られることを見いだし本発明に到達した。Means for Solving the Problems The inventors of the present invention have conducted intensive studies to achieve the above object, and as a result, a raw material bismuth has been charged inside a double quartz tube comprising an outer tube and an inner tube. If a raw material crucible and a recovery mold connected to the crucible are arranged and vacuum distillation is performed, the evaporated bismuth is condensed on the quartz cylinder surface and collected in the recovery mold, a simpler structure than before In addition, since the process from purification to casting can be performed in one continuous process and contamination is small, it has been found that high purity bismuth having a purity of 99.9999% or more containing less than 1 ppm of impurities can be obtained, and the present invention has been achieved. .
【０００９】すなわち本発明の第１は、ビスマス原料を
真空溶解して高純度ビスマスを製造する方法において、
原料るつぼに装入された原料ビスマスを温度６５０℃以
上、真空度１×１０-3Ｔｏｒｒ以下で真空蒸留すること
により、蒸発させたビスマスを原料るつぼに連接する回
収鋳型に回収してインゴットとし、不純物として硫黄、
カルシウム、鉛の含有量がそれぞれ０．０５ppm 以下
で、かつガス成分以外の不純物量が１ppm 未満である純
度９９．９９９９％以上の高純度ビスマスを得ることを
特徴とする高純度ビスマスの製造方法；第２に、真空精
製部と、これを加熱する電気炉を備えた加熱部とを主要
構成部とする高純度ビスマスの製造装置であって、上記
真空精製部がそれぞれ脱着可能に連接する原料るつぼと
回収鋳型、冷却トラップおよび水冷フランジとからな
り、かつ上記原料るつぼと回収鋳型が耐熱材からなる二
重の筒で封体されていることを特徴とする高純度ビスマ
スの製造装置を提供するものである。That is, a first aspect of the present invention is a method for producing high-purity bismuth by vacuum-dissolving a bismuth raw material,
The raw material bismuth charged in the raw material crucible is subjected to vacuum distillation at a temperature of 650 ° C. or more and a degree of vacuum of 1 × 10 −3 Torr or less, so that the evaporated bismuth is recovered in a recovery mold connected to the raw material crucible to form an ingot, Sulfur as an impurity,
A method for producing high-purity bismuth, characterized in that high-purity bismuth having a purity of 99.9999% or more with a content of calcium and lead of 0.05 ppm or less and an impurity amount other than gas components of less than 1 ppm, respectively; Secondly, there is provided a high-purity bismuth production apparatus mainly comprising a vacuum purifying section and a heating section provided with an electric furnace for heating the vacuum purifying section, wherein the vacuum purifying section is detachably connected to the raw material crucible. And a recovery mold, a cooling trap and a water-cooled flange, and wherein the raw material crucible and the recovery mold are sealed by a double cylinder made of a heat-resistant material. It is.
【００１０】[0010]
【発明の実施の形態】本発明の高純度ビスマスの製造装
置は、一例として図１の概略図に示す構造とすることが
できる。すなわち電気炉１内に配置された石英製外筒３
内を真空排気装置２により真空排気を行えるよう、上記
外筒３内に原料るつぼ５、回収鋳型６、鋳型中央部に設
けた吸入台９、吸入台下の冷却トラップ８、これを冷却
する水冷フランジ７を脱着可能に連接し、さらに原料る
つぼ上面に石英製内筒４を設けて外筒３と共に二重構造
となって封体されている。DESCRIPTION OF THE PREFERRED EMBODIMENTS The apparatus for producing high-purity bismuth according to the present invention can have the structure shown in the schematic diagram of FIG. 1 as an example. That is, a quartz outer cylinder 3 placed in the electric furnace 1
The raw material crucible 5, the recovery mold 6, the suction table 9 provided at the center of the mold, the cooling trap 8 below the suction table, and water cooling for cooling the crucible 5 in the outer tube 3 so that the inside can be evacuated by the vacuum evacuation device 2. A flange 7 is detachably connected, and an inner tube 4 made of quartz is provided on the upper surface of the raw material crucible.
【００１１】この場合、原料ビスマスとして市販金属ビ
スマス（純度９９．９９％程度）を原料るつぼ５に適量
入れ、電気炉で６５０℃以上、好ましくは６５０〜９０
０℃の温度範囲にすると共に、真空度を１×１０-3Ｔｏ
ｒｒ以下、好ましくは１×１０-3〜１×１０-4Ｔｏｒｒ
の範囲に制御すると原料るつぼ内の原料ビスマスが融解
・蒸発し、該るつぼ５と上部の内筒４との間に落下し
て、るつぼ底部に連接する回収鋳型６の中に回収され
る。In this case, an appropriate amount of commercially available metal bismuth (purity of about 99.99%) is charged into the raw material crucible 5 as the raw material bismuth, and is heated at 650 ° C. or higher, preferably 650 to 90 ° C. in an electric furnace.
The temperature range is 0 ° C. and the degree of vacuum is 1 × 10 −3 To.
rr or less, preferably 1 × 10 −3 to 1 × 10 −4 Torr
In this case, the raw material bismuth in the raw material crucible melts and evaporates, falls between the crucible 5 and the upper inner cylinder 4, and is recovered in the recovery mold 6 connected to the bottom of the crucible.
【００１２】原料ビスマス中に含有される不純物のう
ち、ビスマスより蒸気圧の低いアルミニウム、ケイ素、
鉄、ニッケル、銅、銀、鉛は原料るつぼ５内に残留し、
逆に蒸気圧の高い、ナトリウム、硫黄、塩素、カルシウ
ム、カリウム、亜鉛、アンチモン、テルルは凝縮するこ
となく気体状で真空排気装置２によってるつぼ底部に設
けられた吸入孔を通って冷却トラップ８内に吸収され、
水冷フランジ７の働きにより冷却されて固化する。Among the impurities contained in the raw material bismuth, aluminum, silicon, and the like having a lower vapor pressure than bismuth,
Iron, nickel, copper, silver and lead remain in the raw material crucible 5,
Conversely, sodium, sulfur, chlorine, calcium, potassium, zinc, antimony, and tellurium having a high vapor pressure are in a gaseous state without condensing and pass through a suction hole provided at the bottom of the crucible by the evacuation device 2 to form the cooling trap 8. Is absorbed by
It is cooled and solidified by the action of the water cooling flange 7.
【００１３】本発明においては、予め、回収用の鋳型の
形状を精製後の次工程で用いる鋳型の形状にしてあるた
め、従来法のように精製されたビスマスを再度鋳造する
必要はなく、このため汚染の少ない高純度ビスマス製品
を精製・鋳造の工程を区別することなく一回の処理で製
造できる。In the present invention, since the shape of the recovery mold is previously set to the shape of the mold used in the next step after purification, it is not necessary to cast the purified bismuth again as in the conventional method. Therefore, a high-purity bismuth product with little contamination can be manufactured in one process without discriminating between the steps of refining and casting.
【００１４】このようにして得られた高純度ビスマスを
グロー放電質量分析装置で分析したところ、硫黄、カル
シウム、鉛が共に０．０５ppm 以下であり、ナトリウ
ム、アルミニウム、ケイ素、塩素、カリウム、鉄、ニッ
ケル、銅、銀、亜鉛、アンチモン、テルルがそれぞれ
０．０１ppm 以下で、かつガス成分以外の不純物の合計
が１ppm 未満の値を示していた。When the thus obtained high purity bismuth was analyzed by a glow discharge mass spectrometer, the content of sulfur, calcium and lead was 0.05 ppm or less, and sodium, aluminum, silicon, chlorine, potassium, iron, Nickel, copper, silver, zinc, antimony, and tellurium were each 0.01 ppm or less, and the total amount of impurities other than gas components was less than 1 ppm.
【００１５】したがって、本発明においては測定対象元
素をＮａ、Ａｌ、Ｓｉ、Ｓ、Ｃｌ、Ｋ、Ｃａ、Ｆｅ、Ｎ
ｉ、Ｃｕ、Ａｇ、Ｚｎ、Ｓｂ、Ｐｂ、Ｔｅとし、グロー
放電質量分析装置により定量分析を行い、得られた不純
物含有量の総和を１００％から差し引いて得られた数値
が９９．９９９９％以上の場合をもって純度９９．９９
９９％以上の高純度ビスマスと定義した。Therefore, in the present invention, the elements to be measured are Na, Al, Si, S, Cl, K, Ca, Fe, N
i, Cu, Ag, Zn, Sb, Pb, and Te were used for quantitative analysis by a glow discharge mass spectrometer, and a value obtained by subtracting the total of the obtained impurity contents from 100% was 99.9999% or more. 99.99 purity
It was defined as high purity bismuth of 99% or more.
【００１６】以下、実施例により本発明をさらに説明す
るが、本発明の範囲はこれらに限定されるものではな
い。Hereinafter, the present invention will be further described with reference to examples, but the scope of the present invention is not limited thereto.
【００１７】[0017]
【実施例１】図１の高純度ビスマス製造装置を参照して
以下説明する。先ず、純度９９．９９％の市販金属ビス
マス１００ｇを原料るつぼ５に入れ、回収鋳型６中央部
に設置した吸入台９上に固定した後、図１に示すように
電気炉１内に装入した。Embodiment 1 A description will be given below with reference to a high-purity bismuth manufacturing apparatus shown in FIG. First, 100 g of commercially available bismuth metal having a purity of 99.99% was placed in a raw material crucible 5, fixed on a suction table 9 provided at the center of the recovery mold 6, and then charged into the electric furnace 1 as shown in FIG. 1. .
【００１８】この場合、原料るつぼ５と回収鋳型６の上
面には、石英製の外筒３と内筒４とが設けられ、真空排
気装置２によって内筒４内部が真空状態となる構造であ
る。In this case, an outer cylinder 3 and an inner cylinder 4 made of quartz are provided on the upper surfaces of the raw material crucible 5 and the recovery mold 6, and the inside of the inner cylinder 4 is evacuated by the vacuum exhaust device 2. .
【００１９】真空排気装置２で排気して内筒４の真空度
を１×１０-3Ｔｏｒｒとすると共に炉温を６５０℃一定
で１時間精製したところ、原料中のビスマスはいったん
蒸発した後、原料るつぼ５上の内筒４の面に接触して次
第に凝縮し始め、粒状になって原料るつぼ５の底部に設
けた回収鋳型６の中に落下した。この粒状ビスマス９０
ｇを回収し、その品位を表１に示した。When the interior of the inner cylinder 4 was evacuated to 1 × 10 −3 Torr and the furnace temperature was kept constant at 650 ° C. for one hour, the bismuth in the raw material was evaporated. The powder gradually came into contact with the surface of the inner cylinder 4 on the raw material crucible 5, began to condense, and fell into granular form into the collecting mold 6 provided at the bottom of the raw material crucible 5. This granular bismuth 90
g were collected and the grade is shown in Table 1.
【００２０】一方、ビスマスより蒸気圧の高いものはガ
ス状のまま排気装置で吸引され、吸入台９の上部に設け
られた吸入孔を通過して冷却トラップ８上で固化した。
この固化物を分析したところ、その主成分はビスマス
で、ナトリウム、硫黄、塩素、カリウム、カルシウム、
亜鉛、アンチモン、テルルなどいずれも蒸気圧の高い物
質が多く含まれていることがわかった。併せて原料るつ
ぼ内に残っている金属を分析したところ、その主成分は
ビスマスで、アルミニウム、ケイ素、鉄、ニッケル、
銅、銀、鉛などの蒸気圧の低い物質が原料より多く含ま
れていることがわかった。On the other hand, the gas having a higher vapor pressure than bismuth is sucked by the exhaust device in a gaseous state, and solidified on the cooling trap 8 through a suction hole provided at an upper portion of the suction table 9.
When this solid was analyzed, its main component was bismuth, and sodium, sulfur, chlorine, potassium, calcium,
It was found that zinc, antimony, tellurium, etc. all contained a lot of substances having high vapor pressure. At the same time, when the metal remaining in the raw material crucible was analyzed, its main component was bismuth, and aluminum, silicon, iron, nickel,
It was found that low vapor pressure substances such as copper, silver, and lead were contained more than the raw materials.
【００２１】[0021]
【表１】 [Table 1]
【００２２】[0022]
【実施例２】純度９９．９４％の市販金属ビスマス１０
０ｇを原料るつぼ５に入れて、真空度を１×１０-4Ｔｏ
ｒｒ、加熱温度を８５０℃として実施例１と同様に精製
を行い、精製ビスマス９２ｇを得た。この品位を表１に
併せて示した。Example 2 Commercially available metal bismuth 10 having a purity of 99.94%
0 g is placed in the crucible 5 and the degree of vacuum is 1 × 10 −4 To.
Purification was performed in the same manner as in Example 1 except that rr and the heating temperature were set to 850 ° C., to obtain 92 g of purified bismuth. The quality is also shown in Table 1.
【００２３】[0023]
【比較例１】比較のため、純度９９．９４％の市販金属
ビスマスの品位を表１に併せて示した。Comparative Example 1 For the purpose of comparison, Table 1 also shows the grades of commercially available bismuth metal having a purity of 99.94%.
【００２４】[0024]
【発明の効果】上述のように、本発明の方法に基づく製
造装置によれば、原料るつぼに溶解したビスマスは蒸発
して内筒表面に凝縮し、鋳型に回収されてインゴットを
形成するので、従来必要とされていた鋳造や後処理等の
複雑な工程に代わって、本発明の簡易な構造の製造装置
を用いることにより、精製から鋳造までの一連の工程を
汚染の危険が少ない一回の工程で行なえるようになり、
従来よりも分離精度が高くしかもコスト低減可能な精製
手段を提供できる。As described above, according to the manufacturing apparatus based on the method of the present invention, bismuth dissolved in the raw material crucible evaporates and condenses on the surface of the inner cylinder and is collected in the mold to form an ingot. Instead of the complicated processes such as casting and post-processing that were conventionally required, by using the manufacturing apparatus having the simple structure of the present invention, a series of processes from refining to casting can be performed once with less risk of contamination. It can be done in the process,
It is possible to provide a purification means having a higher separation accuracy than the conventional one and capable of reducing the cost.
【図１】本発明に係る高純度ビスマスの製造装置の概要
を示す概略断面図である。FIG. 1 is a schematic cross-sectional view showing an outline of an apparatus for producing high-purity bismuth according to the present invention.
１ 電気炉 ２ 真空排気装置 ３ 石英製外筒 ４ 石英製内筒 ５ 原料るつぼ ６ 回収鋳型 ７ 水冷フランジ ８ 冷却トラップ ９ 吸入台 DESCRIPTION OF SYMBOLS 1 Electric furnace 2 Vacuum exhaust device 3 Quartz outer cylinder 4 Quartz inner cylinder 5 Raw material crucible 6 Collection mold 7 Water-cooled flange 8 Cooling trap 9 Suction stand
Claims (2)
マスを製造する方法において、原料るつぼに装入された
原料ビスマスを温度６５０℃以上、真空度１×１０-3Ｔ
ｏｒｒ以下で真空蒸留することにより、蒸発させたビス
マスを原料るつぼに連接する回収鋳型に回収してインゴ
ットとし、不純物として硫黄、カルシウム、鉛の含有量
がそれぞれ０．０５ppm 以下で、かつガス成分以外の不
純物量が１ppm 未満である純度９９．９９９９％以上の
高純度ビスマスを得ることを特徴とする高純度ビスマス
の製造方法。1. A method for producing high-purity bismuth by dissolving a bismuth raw material in vacuum, wherein the raw material bismuth charged in the raw material crucible is heated to a temperature of 650 ° C. or higher and a degree of vacuum of 1 × 10 −3 T.
Vacuum distillation at orr or lower recovers the evaporated bismuth in a recovery mold connected to the raw material crucible to form an ingot. The content of sulfur, calcium, and lead as impurities is 0.05 ppm or less, respectively, and other than gas components. A method for producing high-purity bismuth, characterized in that high-purity bismuth having a purity of 99.9999% or more and an impurity amount of less than 1 ppm is obtained.
備えた加熱部とを主要構成部とする高純度ビスマスの製
造装置であって、上記真空精製部がそれぞれ脱着可能に
連接する原料るつぼ、回収鋳型、冷却トラップおよび水
冷フランジからなり、かつ上記原料るつぼと回収鋳型が
耐熱材からなる二重の筒で封体されていることを特徴と
する高純度ビスマスの製造装置。2. A high-purity bismuth production apparatus mainly comprising a vacuum purification unit and a heating unit provided with an electric furnace for heating the vacuum purification unit, wherein the vacuum purification unit is detachably connected to each other. An apparatus for producing high-purity bismuth, comprising a crucible, a recovery mold, a cooling trap, and a water-cooled flange, wherein the raw material crucible and the recovery mold are sealed by a double cylinder made of a heat-resistant material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33036796A JP3838716B2 (en) | 1996-11-26 | 1996-11-26 | Purification method of bismuth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33036796A JP3838716B2 (en) | 1996-11-26 | 1996-11-26 | Purification method of bismuth |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10158754A true JPH10158754A (en) | 1998-06-16 |
| JP3838716B2 JP3838716B2 (en) | 2006-10-25 |
Family
ID=18231819
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33036796A Expired - Fee Related JP3838716B2 (en) | 1996-11-26 | 1996-11-26 | Purification method of bismuth |
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| Country | Link |
|---|---|
| JP (1) | JP3838716B2 (en) |
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|---|---|---|---|---|
| US6444164B2 (en) * | 1996-06-21 | 2002-09-03 | Dowa Mining Co., Ltd. | Apparatus for producing high-purity silver materials |
| US6627149B1 (en) | 1996-06-21 | 2003-09-30 | Dowa Mining Co., Ltd. | High-purity silver wires for use in recording, acoustic or image transmission applications |
| CN103184355A (en) * | 2011-12-31 | 2013-07-03 | 广东先导稀材股份有限公司 | Preparation method of high purity bismuth |
| JP2013185214A (en) * | 2012-03-08 | 2013-09-19 | Jx Nippon Mining & Metals Corp | BISMUTH OR BISMUTH ALLOY HAVING SMALL AMOUNT OF α-RAY, AND METHOD FOR PRODUCING THE SAME |
| WO2014069357A1 (en) * | 2012-11-02 | 2014-05-08 | Jx日鉱日石金属株式会社 | Method for producing low α-emitting bismuth, low α-emitting bismuth, and bismuth alloy |
| CN104018009A (en) * | 2014-06-19 | 2014-09-03 | 湖南华信有色金属有限公司 | Separating and purifying technology for bismuth metal |
| WO2015083405A1 (en) * | 2013-12-03 | 2015-06-11 | Jx日鉱日石金属株式会社 | Method for manufacturing low-alpha-radiation bismuth and low-alpha-radiation bismuth |
| WO2015098191A1 (en) * | 2013-12-24 | 2015-07-02 | Jx日鉱日石金属株式会社 | Low-α-emission bismuth and process for producing low-α-emission bismuth |
| WO2015102062A1 (en) * | 2014-01-06 | 2015-07-09 | Jx日鉱日石金属株式会社 | Process for producing low-α-emission bismuth, and low-α-emission bismuth |
| WO2015125331A1 (en) * | 2014-02-20 | 2015-08-27 | Jx日鉱日石金属株式会社 | Method for producing low α-emitting bismuth and low α-emitting bismuth |
| JP2016191083A (en) * | 2015-03-30 | 2016-11-10 | Ｊｘ金属株式会社 | BISMUTH WITH A REDUCED AMOUNT OF α RAYS AND METHOD FOR PRODUCING THE SAME |
| CN106191449A (en) * | 2016-08-15 | 2016-12-07 | 永兴县億翔环保科技有限公司 | Bismuth anode mud treatment method |
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-
1996
- 1996-11-26 JP JP33036796A patent/JP3838716B2/en not_active Expired - Fee Related
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|---|---|---|---|---|
| US6627149B1 (en) | 1996-06-21 | 2003-09-30 | Dowa Mining Co., Ltd. | High-purity silver wires for use in recording, acoustic or image transmission applications |
| US6444164B2 (en) * | 1996-06-21 | 2002-09-03 | Dowa Mining Co., Ltd. | Apparatus for producing high-purity silver materials |
| CN103184355A (en) * | 2011-12-31 | 2013-07-03 | 广东先导稀材股份有限公司 | Preparation method of high purity bismuth |
| JP2013185214A (en) * | 2012-03-08 | 2013-09-19 | Jx Nippon Mining & Metals Corp | BISMUTH OR BISMUTH ALLOY HAVING SMALL AMOUNT OF α-RAY, AND METHOD FOR PRODUCING THE SAME |
| WO2014069357A1 (en) * | 2012-11-02 | 2014-05-08 | Jx日鉱日石金属株式会社 | Method for producing low α-emitting bismuth, low α-emitting bismuth, and bismuth alloy |
| JP5903497B2 (en) * | 2012-11-02 | 2016-04-13 | Ｊｘ金属株式会社 | Method for producing low α-ray bismuth, low α-ray bismuth and bismuth alloy |
| WO2015083405A1 (en) * | 2013-12-03 | 2015-06-11 | Jx日鉱日石金属株式会社 | Method for manufacturing low-alpha-radiation bismuth and low-alpha-radiation bismuth |
| JP6067855B2 (en) * | 2013-12-24 | 2017-01-25 | Ｊｘ金属株式会社 | Low α-ray bismuth and method for producing low α-ray bismuth |
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| JP5960341B2 (en) * | 2014-01-06 | 2016-08-02 | Ｊｘ金属株式会社 | Method for producing low α-ray bismuth |
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| CN104018009A (en) * | 2014-06-19 | 2014-09-03 | 湖南华信有色金属有限公司 | Separating and purifying technology for bismuth metal |
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| CN106191449A (en) * | 2016-08-15 | 2016-12-07 | 永兴县億翔环保科技有限公司 | Bismuth anode mud treatment method |
| CN112063854A (en) * | 2020-09-02 | 2020-12-11 | 河南豫光金铅股份有限公司 | Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material |
| CN115491509A (en) * | 2022-08-31 | 2022-12-20 | 永兴县鸿福金属有限公司 | Vacuum purification method for multi-stage extraction of refined bismuth |
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