JPH0521970B2 - - Google Patents
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- Publication number
- JPH0521970B2 JPH0521970B2 JP6043685A JP6043685A JPH0521970B2 JP H0521970 B2 JPH0521970 B2 JP H0521970B2 JP 6043685 A JP6043685 A JP 6043685A JP 6043685 A JP6043685 A JP 6043685A JP H0521970 B2 JPH0521970 B2 JP H0521970B2
- Authority
- JP
- Japan
- Prior art keywords
- mgcl
- cooling
- retort
- space
- cylindrical
- 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 - Lifetime
Links
- 238000001816 cooling Methods 0.000 claims description 56
- 238000000926 separation method Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 239000003870 refractory metal Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000008023 solidification Effects 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 230000007423 decrease Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Description
【発明の詳細な説明】
本発明はクロル法によつて生成したTi、Zr等
の耐火金属から混在不純物を分離する方法、及び
そのための装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for separating mixed impurities from refractory metals such as Ti and Zr produced by the Kroll method, and an apparatus for the same.
クロル法、つまり耐火金属塩化物のMg還元に
よつて得られる反応堆積物は、スポンジ状の耐火
金属と共に未反応Mg及び副生成物のMgCl2を多
量に含んでいる。これらの不純物を除去して耐火
金属を精製するために、この反応堆積物は減圧下
にて約800℃以上の高温で処理（真空分離）され
る。 The reaction deposit obtained by the Kroll method, that is, Mg reduction of refractory metal chloride, contains a large amount of unreacted Mg and by-product MgCl 2 as well as spongy refractory metal. In order to remove these impurities and purify the refractory metal, this reaction deposit is treated (vacuum separation) at a high temperature of about 800° C. or higher under reduced pressure.
この真空分離工程を行うための装置は、例えば
特公昭55−36254、特開昭57−185940、59−
133335号等の各公報に記載されている。これらに
よるとクロル工程終了後、反応堆積物は専用の装
置に移され、或いは生成された位置で加熱され
る。発生したMg、MgCl2の蒸気は加熱部の上方
又は側方に設けた冷却部へ導かれ、冷却面上で凝
固付着させ（上方）、或は凝縮・沈降させられる
（側方）。 The apparatus for performing this vacuum separation process is, for example, Japanese Patent Publication No. 55-36254, Japanese Patent Publication No. 57-185940, 59-
It is described in various publications such as No. 133335. According to these methods, after the completion of the chloro process, the reaction deposit is transferred to a dedicated device or heated at the location where it was generated. The generated Mg and MgCl 2 vapors are led to the cooling section installed above or to the side of the heating section, and are solidified and deposited on the cooling surface (top) or condensed and precipitated (side).
冷却部を加熱部の上方に置く竪型構成では、上
記のようにMg及びMgCl2の析出、凝固は、冷却
面上により以前に形成された凝固層を介して進行
する。この際凝固層がMgのみ或はMgを大量に
含むMgCl2の場合には層全体としての熱伝導性が
高いので、発生蒸気の析出固化は速やかに進行す
るが、凝固層の主成分がMgCl2である場合には熱
伝導性が低いので、層表面での熱交換速度が小さ
くなり、これが分離工程の速度を支配することに
なる。この傾向は凝固層が厚みを増すにつれてさ
らに強くなる。このため分離装置のヒーターを
1000℃近い高温で作動させて長時間真空引操作を
続ける必要があり、この結果多大のエネルギー及
び操作時間が不可欠である。 In the vertical configuration in which the cooling section is placed above the heating section, the precipitation and solidification of Mg and MgCl 2 proceed via the solidified layer previously formed on the cooling surface, as described above. At this time, if the solidified layer is made of only Mg or MgCl 2 containing a large amount of Mg, the thermal conductivity of the layer as a whole is high, so the precipitation and solidification of the generated vapor proceeds quickly, but the main component of the solidified layer is MgCl2. If it is 2 , the thermal conductivity is low, so the heat exchange rate at the layer surface is low, and this will control the rate of the separation process. This tendency becomes even stronger as the thickness of the solidified layer increases. For this reason, the heater of the separator
It is necessary to operate at a high temperature close to 1000°C and continue vacuuming operation for a long time, and as a result, a large amount of energy and operation time are indispensable.
本発明は竪型構成の分離装置において、効率の
低下する工程後半期に、熱導性の高い冷却面を新
たに追加し冷却面を拡張することにより、レトル
ト内に残存せる主としてMgCl2の捕捉効率を向上
せしめることを要旨とするものである。 The present invention improves the capture of mainly MgCl 2 remaining in the retort by adding a new cooling surface with high thermal conductivity and expanding the cooling surface in the second half of the process when efficiency decreases in a vertical separation device. The purpose is to improve efficiency.
本発明のこの方法は次のような構成の装置で行
なうのが適している。それゆえ本発明の第二の要
旨は、本質的に円筒状のレトルトによつて限定さ
れる空間の下方に、クル工程で得た耐火金属、
Mg、MgCl2の混在物を収容しかつ、Mg及び
MgCl2を気化しうる加熱装置を備え、一方この空
間の上方には内壁面の少くとも一部をMg、
MgCl2の凝固可能な温度に保ちうる冷却円筒面を
備えた、耐火金属からMg、MgCl2を分離するた
めの装置において、レトルト内空間の上方に、表
面の少くとも一部分をMg、MgCl2の凝固温度以
下に保ちうる冷却体を配置したことを特徴とする
装置に存する。 This method of the present invention is suitably carried out with an apparatus having the following configuration. A second aspect of the invention therefore provides that, below the space defined by the essentially cylindrical retort, the refractory metal obtained by the cru process,
Contains inclusions of Mg, MgCl 2 and
A heating device capable of vaporizing MgCl 2 is provided, while above this space at least a portion of the inner wall surface is filled with Mg,
In an apparatus for separating Mg, MgCl 2 from refractory metals, which is equipped with a cooled cylindrical surface that can be maintained at a temperature at which MgCl 2 can solidify, at least a portion of the surface is located above the interior space of the retort . The present invention resides in an apparatus characterized by disposing a cooling body capable of maintaining the temperature below the solidification temperature.
本発明において上記円筒面は、レトルト外壁面
上に設けた冷却水ジヤケツトで冷却されるレトル
ト内壁面、又はレトルト内に配置した別の筒体
（クロ工程で内筒として利用可能のもの）の内壁
面で構成する。 In the present invention, the cylindrical surface is the inner wall surface of the retort that is cooled by a cooling water jacket provided on the outer wall surface of the retort, or the inside of another cylindrical body (which can be used as an inner cylinder in the blackening process) placed inside the retort. Consists of walls.
冷却体はレトルト頂部から軸に沿つて吊下げた
中空の円筒状又はドーナツ状の環状体或は蛇管と
して構成し、内部を冷却水又は冷風が循環できる
ようにする。この冷却体には適当な間隔で数個の
水平フインを取付けておくと凝縮物の落下が防止
できて有利である。このような冷却体の代りに、
あるいはこれと共に次のような二次冷却面を用い
ることができる。即ちレトルト外壁面にジヤケツ
トを設けるに当つて、異なる高さの部位にそれぞ
れ独立して制御可能な冷却ジヤケツトを少くとも
２系統以上設け、このうち最上位置のものを主冷
却ジヤケツトとして分離工程全期を通じて作動さ
せる。一方、より下方の二次ジヤケツトは上記冷
却体同様分離工程の後半期に作動される。 The cooling body is configured as a hollow cylindrical or donut-shaped annular body or a serpentine tube suspended from the top of the retort along the axis, and allows cooling water or cold air to circulate inside. It is advantageous to attach several horizontal fins to the cooling body at appropriate intervals to prevent condensate from falling. Instead of such a cooling body,
Alternatively, a secondary cooling surface such as the following can be used in conjunction with this. In other words, when installing jackets on the outer wall of the retort, at least two systems of cooling jackets are provided at different heights, each of which can be controlled independently, and the uppermost one is used as the main cooling jacket during the entire separation process. operate through. On the other hand, the lower secondary jacket, like the cooling body described above, is operated in the latter half of the separation process.
冷却体又は二次冷却面は、分離工程の前半にお
いては冷却を行なわず、むしろ熱風等を通じて加
熱し、Mg、MgCl2の析出を防止しておく。混在
Mgのほぼ全量が気化し主冷却面に付着され、発
生する蒸気相が本質的にMgCl2のみとなる分離工
程後半期―この時期は例えば、加熱入力に対する
真空度の上昇速度の低下、または所要加熱電力の
増加によつて検知される―において、二次冷却面
又は冷却体へ冷却媒の供給開始によりこれを始動
させる。この操作によつてレトルト内空間と二次
冷却面、冷却体との間で大きなMgCl2蒸気圧の差
を生じ、耐火金属とMgCl2との分離を促進するこ
とができる。 The cooling body or the secondary cooling surface is not cooled in the first half of the separation step, but rather heated with hot air or the like to prevent precipitation of Mg and MgCl 2 . mixed
In the second half of the separation process, when almost all of the Mg is vaporized and deposited on the main cooling surface, and the vapor phase generated is essentially only MgCl 2 - this is the period when, for example, the rate of increase in vacuum relative to the heating input decreases, or the required Detected by an increase in the heating power, this is triggered by the start of the supply of coolant to the secondary cooling surface or cooling body. This operation creates a large difference in MgCl 2 vapor pressure between the retort interior space, the secondary cooling surface, and the cooling body, and can promote separation of the refractory metal and MgCl 2 .
本発明においては、二次冷却面や冷却体の作動
を分離工程の初期から行なうのは次の理由により
好ましくない。つまりクロル工程から回収される
反応堆積物は耐火金属と共に、多量の金属Mgを
含有しているので、これを利用可能な状態で回収
するのが全行程コスト低減の一要因と言える。と
ころが冷却体、二次冷却面を分離工程初期から作
動させるとMgを主成分とする凝縮物中にこれら
の部材表面に強力に付着することになる。再利用
のためにはMgを多くの時間労力をかけて取りは
ずさなければならず、またこうして取りはずした
Mgは取扱い中に汚染されるので、そのまゝでは
再使用に適さなくなること、等の不利を生じる。 In the present invention, it is not preferable to operate the secondary cooling surface or the cooling body from the beginning of the separation process for the following reasons. In other words, since the reaction deposits recovered from the chlorine process contain a large amount of metal Mg as well as refractory metals, recovering this in a usable state is one of the factors that reduces the cost of the entire process. However, if the cooling body and secondary cooling surface are operated from the beginning of the separation process, the condensate containing Mg as a main component will strongly adhere to the surfaces of these members. In order to reuse the Mg, it was necessary to spend a lot of time and effort to remove it, and the Mg was removed in this way.
Since Mg becomes contaminated during handling, there are disadvantages such as making it unsuitable for reuse.
本発明において主冷却面の下方に配置せる二次
冷却面を用いるときは、レトルト下方で発生する
蒸気圧の低いMgCl2を短い移動距離で耐火金属か
ら分離することができるので、蒸発速度が低下す
る分離工程後半期において特に有効にMgCl2を捕
捉できる。 In the present invention, when a secondary cooling surface placed below the main cooling surface is used, the MgCl 2 with low vapor pressure generated below the retort can be separated from the refractory metal over a short travel distance, reducing the evaporation rate. MgCl 2 can be captured particularly effectively in the latter half of the separation process.
なお上記の説明は処理される耐火金属をレトル
ト下方へ置く構成について説明したが、耐火金属
を冷却部の上方に配置する構成に対しても本発明
は適用可能である。この場合はMg及びMgCl2の
相当部分が液状で流下して、冷却部に置いた受器
に溜るので、二次冷却面又は冷却体は、加熱部に
近い冷却部上方に設けるのが適している。 Although the above description has been made regarding a configuration in which the refractory metal to be processed is placed below the retort, the present invention is also applicable to a configuration in which the refractory metal is placed above the cooling section. In this case, a considerable portion of Mg and MgCl 2 will flow down in liquid form and collect in a receiver placed in the cooling section, so it is appropriate to install the secondary cooling surface or cooling body above the cooling section near the heating section. There is.
次に本発明を図によつて説明する。第１図は本
発明によつて作成された真空分離装置の構成の一
例を示す縦断面図、第２図はこのような装置の上
半分の改変例部分断面図である。図において全体
を１として示される真空分離装置の下部外方に
は、本質的に密閉構造をもち適当な減圧手段（図
示せず）に接続された電熱炉２が、炉内には縦長
円筒状レトルト３が取付けられる。この下部に
は、例えば特開昭57−192234号公報に記載のクロ
ル法還元装置で得られた、Ti、Zr等の生成金属
−Mg−MgCl2混在物が、還元反応容器４に保持
されたまゝ置かれる。炉２から突出せるレトルト
３の上部と炉内に置かれるレトルト下部とは分離
可能で、両部分の間には、下部からの輻射熱遮断
のためにステンレス鋼板製の邪魔板５が着脱可能
に配置されている。レトルト上部の下端近くには
着脱可能のコマ６が数個取付けられ、空の還元反
応容器７を支えている。レトルト上部側壁には頂
部から半分以上を覆う主ジヤケツト８と、残部を
覆う二次ジヤケツト９とが設けられている。レト
ルト頂部の蓋１０からは、下端を閉じた中空円筒
状の冷却体１１が軸に沿つて下方へ延びている。
冷却体内部は冷媒空気通路のために二重管構成と
なつている。この冷却体は第２図ａ，ｂ，に示す
ような、より短い中空の環状構成１２又は蛇管１
３とすることもできる。蓋１０にはまたレトルト
内減圧のために排気用ダクト１４が接続される。 Next, the present invention will be explained with reference to the drawings. FIG. 1 is a longitudinal cross-sectional view showing an example of the configuration of a vacuum separation device made according to the present invention, and FIG. 2 is a partial cross-sectional view of a modified example of the upper half of such a device. Outside the lower part of the vacuum separation device, which is shown as 1 in the figure, is an electric heating furnace 2 which has an essentially closed structure and is connected to a suitable pressure reducing means (not shown). Retort 3 is installed. In this lower part, a mixture of formed metals such as Ti and Zr-Mg-MgCl 2 obtained by the chloro method reduction apparatus described in JP-A-57-192234 is held in the reduction reaction vessel 4.ゝIt is placed. The upper part of the retort 3 protruding from the furnace 2 and the lower part of the retort placed in the furnace can be separated, and a baffle plate 5 made of a stainless steel plate is removably arranged between the two parts to block radiant heat from the lower part. has been done. Several removable pieces 6 are attached near the lower end of the upper part of the retort and support an empty reduction reaction vessel 7. A main jacket 8 covering more than half of the top of the retort and a secondary jacket 9 covering the remaining part are provided on the upper side wall of the retort. A hollow cylindrical cooling body 11 with a closed lower end extends downward from a lid 10 at the top of the retort along an axis.
The inside of the cooling body has a double pipe configuration for the refrigerant air passage. This cooling body can be a shorter hollow annular arrangement 12 or a serpentine tube 1 as shown in FIGS. 2a, b.
It can also be set to 3. An exhaust duct 14 is also connected to the lid 10 for reducing the pressure inside the retort.
上記のように構成された真空分離装置による操
作例を示す。内径2m、深さ4mの本質的に円筒状
の空間を持つ電熱炉に内径1.6m、肉厚32mmの
SUS316製のレトルト下部が設置されている。こ
の中に置かれた外径1.4m、肉厚16mm、全長2.4m、
SUS410製の反応容器にはスポンジチタン約４ト
ンと少量のMgCl2およびMgを含む混合物が保持
されている。反応容器上方に加熱部から冷却部へ
の輻射防止及び冷却部から反応容器内へのMgCl2
等の落下防止のための邪魔板を取付けた後、レト
ルト下部に置かれたのと同タイプの空の還元反応
容器を収容し、外周全面に一系統のみの水冷ジヤ
ケツトを設けたレトルト上部をかぶせ、一方蓋に
は冷却体として外径0.4mm、長さ2.5mの鋼管と減
圧用ダクトを取付けて、レトルト下部と接合す
る。頂部から真空引きを行ない、炉でレトルト下
部を950〜1000℃に加熱する一方、レトルト上部
のジヤケツト、次いで冷却体を作動させる。 An example of operation using the vacuum separation apparatus configured as described above will be shown. An electric furnace with an essentially cylindrical space with an inner diameter of 2 m and a depth of 4 m has an inner diameter of 1.6 m and a wall thickness of 32 mm.
The lower part of the retort is made of SUS316. The outer diameter 1.4m, wall thickness 16mm, total length 2.4m, placed inside this.
A reaction vessel made of SUS410 holds a mixture containing approximately 4 tons of titanium sponge and small amounts of MgCl 2 and Mg. Above the reaction vessel, prevent radiation from the heating section to the cooling section, and from the cooling section into the reaction vessel .
After installing a baffle plate to prevent the retort from falling, an empty reduction reaction vessel of the same type as that placed at the bottom of the retort was placed, and the top of the retort, which had only one system of water cooling jackets installed around the entire outer periphery, was placed over the top of the retort. On the other hand, a steel pipe with an outer diameter of 0.4 mm and a length of 2.5 m and a decompression duct are attached to the lid as a cooling body, and are connected to the lower part of the retort. A vacuum is drawn from the top and the lower part of the retort is heated in the furnace to 950-1000°C, while the jacket in the upper part of the retort and then the cooling body are activated.
上記要領にて操作を行つた場合、一つの典型的
な例においては上記温度範囲に約36時間保持後に
１×10-2Torrの真空度に到達した時点で冷却体
を空冷によつて冷却し、さらに48時間維持して分
離処理を完成した。得られたスポンジチタン中の
Mg及びCl含有量はそれぞれ140，300ppmであつ
た。この成果は冷却体を有しない同様設計の真空
分離装置を用いた場合の総温度維持所要時間100
時間に比べて大巾な改善を与えるものである。 When operating according to the above procedure, in one typical example, the cooling body is cooled by air cooling when a vacuum level of 1 x 10 -2 Torr is reached after maintaining the above temperature range for about 36 hours. , and maintained for an additional 48 hours to complete the separation process. In the obtained titanium sponge
The Mg and Cl contents were 140 and 300 ppm, respectively. This result shows that the total temperature maintenance time is 100% when using a similarly designed vacuum separator without a cooling body.
This is a huge improvement over time.
第１図は本発明による真空分離装置の一構成例
を示す縦断面図、第２図ａ，ｂは特にレトルト上
部の別の設計例を示す部分図である。
図において各参照番号は次の部材を示す。１…
…真空分離装置；２……電熱炉；３……レトル
ト；４……還元反応容器；５……邪魔板；６……
容器支持用コマ；７……反応容器；８……主ジヤ
ケツト；９……二次ジヤケツト；１０……蓋；１
１，１２，１３……冷却体；１４……排気用ダク
ト。
FIG. 1 is a longitudinal sectional view showing an example of the structure of a vacuum separation apparatus according to the present invention, and FIGS. 2a and 2b are partial views showing another example of the design of the upper part of the retort. In the figures, each reference number indicates the following member. 1...
...Vacuum separation device; 2...Electric furnace; 3...Retort; 4...Reduction reaction vessel; 5...Baffle plate; 6...
Container support piece; 7... Reaction vessel; 8... Main jacket; 9... Secondary jacket; 10... Lid; 1
1, 12, 13... Cooling body; 14... Exhaust duct.
Claims (1)
び耐火金属の混在物を加熱してMg及びMgCl2を
気化し、このようにして生じた蒸気を、該空間に
面しかつMg及びMgCl2の凝固温度以下に保つた
冷却面上或はこの付近で凝固析出させることによ
り、耐火金属からMg及びMgCl2を分離する方法
において、該空間内におけるMgの分圧が著しく
低下する分離工程後半期に、上記冷却面を拡張す
ることによつて、特にMgCl2の除去効率を上昇せ
しめたことを特徴とする方法。 ２ 本質的に円筒状のレトルトによつて限定され
る空間の下方に、クロル工程で得た耐火金属、
Mg、MgCl2の混在物を収容しかつ、Mg及び
MgCl2を気化しうる加熱装置を備え、一方この空
間の上方には内壁面の少くとも一部をMg、
MgCl2の凝固可能な温度に保ちうる冷却円筒面を
備えた、耐火金属からMg、MgCl2を分離するた
めの装置において、レトルト内空間の上方に、表
面の少くとも一部分をMg、MgCl2の凝固温度以
下に保ちうる冷却体を配置したことを特徴とする
装置。 ３ 上記冷却体が、レトルト頂部に冷却円筒面か
ら隔てゝ設けた環状体又は筒状体又はら旋状体で
ある、特許請求の範囲第２項記載の装置。 ４ 本質的に円筒状のレトルトによつて限定され
る空間の下方に、クロル工程で得た耐火金属、
Mg、MgCl2の混在物を収容しかつ、Mg及び
MgCl2を気化しうる加熱装置を備え、一方レトル
ト上方の外壁面の高さの異なる部位に互に独立制
御可能な冷却ジヤケツトを少くとも上下２系統備
え、こうしてレトルト上部の内壁面又はこれに隣
接して配置した別の筒体内壁面を対応部分ごと
に、Mg及びMgCl2の凝固付着可能温度に冷却で
きるようにしたことを特徴とする、耐火金属から
Mg及びMgCl2を分離するための装置。 ５ 上記レトルトの頂部にレトルト及び冷却筒体
の内壁面から隔てゝ、環状、筒状、又はら旋状に
構成した冷却体を配置し、この冷却体が上記冷却
ジヤケツトのうち少くとも最上部に位置するジヤ
ケツトに対して独立制御可能な冷却手段を有す
る、特許請求の範囲第４項記載の装置。[Claims] 1. A mixture of Mg, MgCl 2 and refractory metal is heated in a space kept under reduced pressure to vaporize Mg and MgCl 2 , and the vapor thus generated is introduced into the space. In a method for separating Mg and MgCl 2 from refractory metals by solidifying and precipitating on or near a cooling surface that faces the cooling surface and is kept below the solidification temperature of Mg and MgCl 2 , the partial pressure of Mg in the space is A method characterized in that the removal efficiency of MgCl 2 is particularly increased by expanding the cooling surface in the latter half of the separation process, when the efficiency decreases significantly. 2. Below the space defined by the essentially cylindrical retort, refractory metal obtained from the Kroll process,
Contains inclusions of Mg, MgCl 2 and
A heating device capable of vaporizing MgCl 2 is provided, while above this space at least a portion of the inner wall surface is filled with Mg,
In an apparatus for separating Mg, MgCl 2 from refractory metals, which is equipped with a cooled cylindrical surface that can be maintained at a temperature at which MgCl 2 can solidify, at least a portion of the surface is located above the interior space of the retort . A device characterized by being equipped with a cooling body that can maintain the temperature below the solidification temperature. 3. The apparatus according to claim 2, wherein the cooling body is an annular body, a cylindrical body, or a helical body provided at the top of the retort and spaced apart from the cooling cylindrical surface. 4. Below the space defined by the essentially cylindrical retort, refractory metal obtained from the Kroll process,
Contains inclusions of Mg, MgCl 2 and
It is equipped with a heating device capable of vaporizing MgCl 2 , and is equipped with at least two systems, upper and lower, of cooling jackets that can be independently controlled at different heights on the outer wall surface above the retort, and are arranged on or adjacent to the inner wall surface above the retort. made of refractory metal, characterized in that the wall surface of a separate cylinder arranged in the same manner can be cooled to a temperature at which Mg and MgCl 2 can solidify and adhere to each corresponding part.
Equipment for separating Mg and MgCl2 . 5. A cooling body configured in an annular, cylindrical, or spiral shape is disposed at the top of the retort, separated from the inner wall surfaces of the retort and the cooling cylinder, and this cooling body is located at least at the top of the cooling jacket. 5. Apparatus according to claim 4, having independently controllable cooling means for the jacket located thereon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6043685A JPS61217539A (en) | 1985-03-25 | 1985-03-25 | Method and apparatus for separating mg and mgcl2 from refractory metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6043685A JPS61217539A (en) | 1985-03-25 | 1985-03-25 | Method and apparatus for separating mg and mgcl2 from refractory metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61217539A JPS61217539A (en) | 1986-09-27 |
| JPH0521970B2 true JPH0521970B2 (en) | 1993-03-26 |
Family
ID=13142208
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6043685A Granted JPS61217539A (en) | 1985-03-25 | 1985-03-25 | Method and apparatus for separating mg and mgcl2 from refractory metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61217539A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101153357B1 (en) * | 2009-12-29 | 2012-06-05 | 재단법인 포항산업과학연구원 | Metal manufacturing device |
-
1985
- 1985-03-25 JP JP6043685A patent/JPS61217539A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61217539A (en) | 1986-09-27 |
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