JPH0741880A - Cooling method and device for sponge titanium reducing furnace - Google Patents
Cooling method and device for sponge titanium reducing furnaceInfo
- Publication number
- JPH0741880A JPH0741880A JP5184203A JP18420393A JPH0741880A JP H0741880 A JPH0741880 A JP H0741880A JP 5184203 A JP5184203 A JP 5184203A JP 18420393 A JP18420393 A JP 18420393A JP H0741880 A JPH0741880 A JP H0741880A
- Authority
- JP
- Japan
- Prior art keywords
- titanium
- reaction vessel
- sponge
- cooling
- air
- 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】本発明は溶融金属マグネシウム浴
に四塩化チタンを滴下してスポンジチタンを製造するい
わゆるクロール法スポンジチタンの製造において、反応
容器を冷却する方法及びその装置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 and an apparatus for cooling a reaction vessel in the so-called Kroll method sponge titanium for producing titanium sponge by dropping titanium tetrachloride into a molten metal magnesium bath.
【0002】[0002]
【従来の技術】クロール法によるスポンジチタン製造法
ではステンレス鋼製の反応容器を加熱した炉内におき、
内部に溶融マグネシウムを装入し、不活性雰囲気下、静
的な状態で四塩化チタンを滴下して、マグネシウムによ
り四塩化チタンを還元してスポンジチタンを生成する。
この還元工程に続き金属マグネシウム、塩化マグネシウ
ムの分離工程、冷却工程を経てスポンジチタン塊が製造
される。2. Description of the Related Art In the titanium sponge production method by the Kroll method, a stainless steel reaction vessel is placed in a heated furnace,
Molten magnesium is charged inside, titanium tetrachloride is dropped in a static state in an inert atmosphere, and titanium tetrachloride is reduced by magnesium to produce titanium sponge.
Following this reduction step, a sponge titanium block is manufactured through a separation step of magnesium metal and magnesium chloride and a cooling step.
【0003】マグネシウムによる四塩化チタンの還元反
応は発熱を伴うため、マグネシウム浴上面に相当する反
応容器外壁の部分を空気吹き付けにより冷却して温度制
御している。しかし、空気冷却の冷却能が小さいので、
反応容器内外壁の保護のために四塩化チタンの滴下速度
を小さくせざるを得ず、還元工程の生産性が小さいとい
う問題がある。また反応容器内壁温度が高いので生成し
たスポンジチタンが容器と反応し、容器の溶損による寿
命低下、及びスポンジチタン塊表面の汚染という問題が
ある。Since the reduction reaction of titanium tetrachloride with magnesium is accompanied by heat generation, the temperature of the outer wall of the reaction vessel, which corresponds to the upper surface of the magnesium bath, is controlled by blowing air. However, since the cooling capacity of air cooling is small,
In order to protect the inner and outer walls of the reaction vessel, the dropping rate of titanium tetrachloride has to be reduced, which causes a problem of low productivity in the reduction step. Further, since the temperature of the inner wall of the reaction vessel is high, the generated titanium sponge reacts with the vessel, and there is a problem that the life of the vessel is shortened due to melting damage of the vessel and the surface of the titanium sponge mass is contaminated.
【0004】[0004]
【発明が解決しようとする課題】本発明の目的とすると
ころは、スポンジチタン製造工程のうち特に還元工程に
おいて問題となる生産性の低下を防ぎ、さらに表面の汚
染が少ないスポンジチタン塊を製造可能とするスポンジ
チタン還元炉の冷却方法及びその冷却機構を有するスポ
ンジチタン還元炉を提供するところにある。SUMMARY OF THE INVENTION The object of the present invention is to prevent a decrease in productivity, which is a problem in the reduction step of the sponge titanium production process, and to produce a sponge titanium block having less surface contamination. The present invention provides a method of cooling a titanium sponge reduction furnace and a titanium sponge reduction furnace having the cooling mechanism.
【0005】[0005]
【課題を解決するための手段】本発明の要旨とするとこ
ろは、加熱された反応容器内に装入された溶融金属マグ
ネシウム浴の上方から四塩化チタンを滴下してスポンジ
状の金属チタンを製造する際に、空気と霧状の水滴の混
合物を反応容器外壁上部に吹き付けて冷却することを特
徴とするスポンジチタン還元炉の冷却方法、及び反応容
器とその反応容器を加熱する加熱炉とからなるスポンジ
チタン還元炉の反応容器外壁に、冷却用空気を吹き付け
る配管によって構成されたスポンジチタン還元炉の冷却
装置において、反応容器外壁冷却用空気の吹き付け配管
に流量制御機構に接続した水噴射ノズルを取り付け、空
気と霧状の水滴の混合物を反応容器外壁に吹き付け可能
としたことを特徴とするスポンジチタン還元炉の冷却装
置である。以下に本発明の詳細を作用とともに説明す
る。The gist of the present invention is to produce sponge-like metallic titanium by dropping titanium tetrachloride from above a molten magnesium metal bath charged in a heated reaction vessel. At the time of cooling, a method of cooling the titanium sponge reduction furnace characterized by spraying a mixture of air and mist-like water droplets onto the upper portion of the outer wall of the reaction vessel to cool it, and a reaction vessel and a heating furnace for heating the reaction vessel In the cooling device of the sponge titanium reduction furnace, which is composed of piping for blowing cooling air on the outer wall of the reaction vessel of the titanium sponge reduction furnace, a water injection nozzle connected to the flow rate control mechanism was attached to the piping for blowing air for cooling the outer wall of the reaction vessel. A cooling device for a sponge titanium reduction furnace, which is capable of spraying a mixture of air and water droplets on the outer wall of a reaction vessel. The details of the present invention will be described below together with the operation.
【0006】[0006]
【作用】反応容器外壁の冷却能力を格段に増加させるた
めに、本発明では従来法において用いられている空気に
代わり、空気と霧状の水の混合物を吹き付ける。本発明
において空気と水の混合比は重量比で水/空気0.03
〜0.2が適当である。水は空気に較べて極めて大きい
冷却能をもつが、混入量が少ないと効果がない。実験の
結果、効果が認められる混合比の下限は0.03であっ
た。水の混合量が多すぎると冷却が強すぎて炉内反応が
不安定になりスポンジチタンの品質が低下する。また、
反応容器外壁に吹き付けられた水が外壁に沿って流下
し、容器下方の加熱部の温度を低下させ、スポンジチタ
ンの品質を著しく劣化させる。このとき加熱炉の燃料消
費量も増加する。水が流下しない混合比の上限は0.2
であった。In order to remarkably increase the cooling capacity of the outer wall of the reaction vessel, in the present invention, a mixture of air and atomized water is sprayed instead of the air used in the conventional method. In the present invention, the mixing ratio of air and water is 0.03 by weight.
~ 0.2 is suitable. Water has an extremely large cooling capacity compared to air, but it is ineffective if the amount of water contained is small. As a result of the experiment, the lower limit of the mixing ratio at which the effect is recognized is 0.03. If the amount of water mixed is too large, the cooling will be too strong and the reaction in the furnace will become unstable, and the quality of titanium sponge will deteriorate. Also,
The water sprayed on the outer wall of the reaction vessel flows down along the outer wall, lowers the temperature of the heating section below the vessel, and significantly deteriorates the quality of titanium sponge. At this time, the fuel consumption of the heating furnace also increases. The upper limit of the mixing ratio at which water does not flow down is 0.2
Met.
【0007】冷却後の冷却風は多量の水蒸気を含むの
で、排出経路において露点以下の温度にまで冷却すると
ドレン水を生じる。したがって、配管部等冷却風の排出
経路には水抜きドレンを設ける等の配慮を要する。反応
容器内または容器外壁の温度を測定して冷却能力を制御
する。冷却能力制御手段として空気に混合する水の流量
を制御する。即ち設定よりも温度が高いときは水量を増
加させ、温度が低いときは水量を減少させる。Since the cooling air after cooling contains a large amount of water vapor, drain water is produced when cooled to a temperature below the dew point in the discharge path. Therefore, consideration must be given to providing drainage drains in the cooling air discharge path such as the piping section. The cooling capacity is controlled by measuring the temperature in the reaction vessel or the outer wall of the vessel. As a cooling capacity control means, the flow rate of water mixed with air is controlled. That is, when the temperature is higher than the set value, the amount of water is increased, and when the temperature is lower, the amount of water is decreased.
【0008】本発明のスポンジチタン製造装置の概念図
を模式的に図1に示す。即ち、従来のクロール法スポン
ジチタン製造装置においてスポンジチタン生成反応容器
9外壁の冷却風吹き付け用空気配管5に混合器(水噴射
ノズル)7を設け、流量を制御された冷却水6を噴射し
て水空気混合気を作り、吹き付け口8を通じて容器1内
の金属マグネシウム浴2上面相当位置に吹き付ける。図
中1はスポンジチタン、3は滴下する四塩化チタン、4
は真空系、10は加熱炉である。A conceptual diagram of the titanium sponge manufacturing apparatus of the present invention is schematically shown in FIG. That is, in the conventional Kroll method titanium sponge production apparatus, a mixer (water injection nozzle) 7 is provided in the cooling air blowing air pipe 5 on the outer wall of the titanium sponge production reaction vessel 9 to inject the cooling water 6 whose flow rate is controlled. A mixture of water and air is created and sprayed onto the upper surface of the metal magnesium bath 2 in the container 1 through the spray port 8. In the figure, 1 is titanium sponge, 3 is titanium tetrachloride to be dropped, 4
Is a vacuum system and 10 is a heating furnace.
【0009】[0009]
【実施例】内径800mmのステンレス鋼製反応容器に
1.2トンの溶融マグネシウムを装入した後、温度を8
00℃に保持しながら上蓋の中心部に設けた滴下管から
四塩化チタンを毎分2.6kgの割合で滴下した。加熱炉
上部に内向きに吹き出しノズルを24個等間隔に配置し
た円環状配管を高さ方向に3段設置し、操業中の金属マ
グネシウム浴上面高さの変化に応じた高さのノズルから
水/空気混合気を反応容器外壁に吹き付けた。EXAMPLE A 1.2 ton molten magnesium was charged into a stainless steel reactor having an inner diameter of 800 mm, and the temperature was raised to 8
Titanium tetrachloride was dripped at a rate of 2.6 kg per minute from a dropping tube provided at the center of the upper lid while maintaining the temperature at 00 ° C. In the upper part of the heating furnace, inwardly-discharging nozzles with 24 nozzles arranged at equal intervals are installed in three stages in the height direction, and water is supplied from the nozzles whose height corresponds to the change in height of the upper surface of the metal magnesium bath during operation. A / air mixture was sprayed onto the outer wall of the reaction vessel.
【0010】制御用温度は容器外壁に高さ方向150mm
間隔で埋設した熱電対により測定した。熱電対の指示が
660℃となるよう空気/水混合比を調整した。操業中
の空気/水混合比は0.06〜0.14の範囲であっ
た。25時間後、四塩化チタンの供給を停止し、温度を
1020℃に昇温して真空分離工程に入った。真空分離
工程36時間の後、アルゴンガス雰囲気として、炉の加
熱を停止し、冷却工程に入った。32時間後には十分冷
却したので、スポンジチタンの塊1012kgを反応容器
から取り出して破砕工程に供給した。The control temperature is 150 mm in the height direction on the outer wall of the container.
It was measured by a thermocouple embedded at intervals. The air / water mixture ratio was adjusted so that the thermocouple indicated 660 ° C. The air / water mixture ratio during operation was in the range of 0.06 to 0.14. After 25 hours, the supply of titanium tetrachloride was stopped, the temperature was raised to 1020 ° C., and the vacuum separation process was started. After 36 hours from the vacuum separation step, the heating of the furnace was stopped under an argon gas atmosphere, and the cooling step was started. After 32 hours, since it was sufficiently cooled, 1012 kg of a mass of titanium sponge was taken out from the reaction vessel and supplied to the crushing step.
【0011】比較として冷却風に水を混合しない標準方
法では同一温度、圧力条件で1トンのスポンジチタン塊
を得るのに還元工程40時間(四塩化チタン平均滴下速
度毎分1.7kg)、真空分離工程36時間、冷却工程3
2時間を要していた。したがって、本発明は還元工程で
は1.6倍、全工程を通じては1.16倍の生産性増加
になった。破砕工程でのスポンジチタン塊の表面皮剥き
厚さは平均0.8mmと標準方法によるスポンジチタン塊
の平均値1.5mmから半減した。破砕後のスポンジチタ
ン品質は密度、不純物量とも標準方法によるスポンジチ
タンと同等の良好な品質であった。使用後の反応容器肉
厚減少は0.12mmであり、標準方法の60%に低下し
た。As a comparison, in the standard method in which water is not mixed with cooling air, a reduction step of 40 hours (titanium tetrachloride average dropping rate of 1.7 kg / min) and a vacuum are performed in order to obtain 1 ton of titanium sponge mass under the same temperature and pressure conditions. Separation process 36 hours, cooling process 3
It took 2 hours. Therefore, the present invention increased the productivity by 1.6 times in the reduction process and 1.16 times in the whole process. The surface peeling thickness of the titanium sponge lump in the crushing step was 0.8 mm on average, which was halved from the average value of 1.5 mm of the titanium sponge lump by the standard method. The quality of sponge titanium after crushing was as good as that of titanium sponge prepared by the standard method in terms of density and amount of impurities. The reduction in the reaction vessel wall thickness after use was 0.12 mm, which was 60% of the standard method.
【0012】[0012]
【発明の効果】本発明により、スポンジチタンの生産性
が特に還元工程において増加し、スポンジチタンインゴ
ットの歩留り向上、反応容器寿命延長の効果がある。According to the present invention, the productivity of titanium sponge is increased especially in the reduction step, the yield of titanium sponge ingot is improved, and the life of the reaction vessel is extended.
【図1】本発明法を実施する装置の概略を模式的に示す
説明図である。FIG. 1 is an explanatory view schematically showing the outline of an apparatus for carrying out the method of the present invention.
1 スポンジチタン 2 溶融マグネシウム 3 四塩化チタン 4 真空系 5 冷却空気 6 冷却水流量制御機構 7 混合器 8 冷却用流体吹き付け口 9 反応容器 10 加熱炉 1 Titanium Sponge 2 Molten Magnesium 3 Titanium Tetrachloride 4 Vacuum System 5 Cooling Air 6 Cooling Water Flow Control Mechanism 7 Mixer 8 Cooling Fluid Spray Port 9 Reaction Vessel 10 Heating Furnace
Claims (2)
金属マグネシウム浴の上方から四塩化チタンを滴下して
スポンジ状の金属チタンを製造する際に、空気と霧状の
水滴の混合物を反応容器外壁上部に吹き付けて冷却する
ことを特徴とするスポンジチタン還元炉の冷却方法。1. When producing titanium metal sponge by dropping titanium tetrachloride from above a molten metal magnesium bath charged in a heated reaction vessel, a mixture of air and mist-like water droplets is added. A method for cooling a titanium sponge reduction furnace, characterized by spraying onto the outer wall of the reaction vessel to cool.
炉とからなり、反応容器の外壁に、冷却用空気を吹き付
ける配管を有する構成のスポンジチタン還元炉におい
て、反応容器外壁冷却用空気の吹き付け配管に、流量制
御機構に接続した水噴射ノズルを取り付けたことを特徴
とするスポンジチタン還元炉の冷却装置。2. A sponge titanium reduction furnace having a reaction vessel and a heating furnace for heating the reaction vessel and having a pipe for blowing cooling air to the outer wall of the reaction vessel. A cooling device for a titanium sponge reduction furnace, wherein a water injection nozzle connected to a flow rate control mechanism is attached to the pipe.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP18420393A JP3567209B2 (en) | 1993-07-26 | 1993-07-26 | Cooling method of titanium sponge reduction furnace |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP18420393A JP3567209B2 (en) | 1993-07-26 | 1993-07-26 | Cooling method of titanium sponge reduction furnace |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH0741880A true JPH0741880A (en) | 1995-02-10 |
JP3567209B2 JP3567209B2 (en) | 2004-09-22 |
Family
ID=16149168
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP18420393A Expired - Lifetime JP3567209B2 (en) | 1993-07-26 | 1993-07-26 | Cooling method of titanium sponge reduction furnace |
Country Status (1)
Country | Link |
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JP (1) | JP3567209B2 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005232500A (en) * | 2004-02-17 | 2005-09-02 | Toho Titanium Co Ltd | Method and apparatus for producing sponge titanium |
CN100370042C (en) * | 2005-05-26 | 2008-02-20 | 唐山市天赫钛业有限公司 | Open direct-cooling condensation technology for vacuum distillation of reduction distillation furnace |
US7813862B2 (en) | 2004-09-21 | 2010-10-12 | Toyota Jidosha Kabushiki Kaisha | Hybrid vehicle |
KR101219181B1 (en) * | 2012-01-06 | 2013-01-09 | 한국기계연구원 | Device for producing sponge titanium and method in using same |
CN104776722A (en) * | 2015-03-20 | 2015-07-15 | 江苏新辉钛锆装备有限公司 | Variable-frequency ventilation cooling system for titanium sponge and zirconium sponge |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0210092A (en) * | 1988-03-08 | 1990-01-12 | Union Carbide Corp | Vessel treating heated substance and cooling method thereof |
JPH031099B2 (en) * | 1985-05-15 | 1991-01-09 | Nippon Kokan Kk |
-
1993
- 1993-07-26 JP JP18420393A patent/JP3567209B2/en not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH031099B2 (en) * | 1985-05-15 | 1991-01-09 | Nippon Kokan Kk | |
JPH0210092A (en) * | 1988-03-08 | 1990-01-12 | Union Carbide Corp | Vessel treating heated substance and cooling method thereof |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005232500A (en) * | 2004-02-17 | 2005-09-02 | Toho Titanium Co Ltd | Method and apparatus for producing sponge titanium |
US7813862B2 (en) | 2004-09-21 | 2010-10-12 | Toyota Jidosha Kabushiki Kaisha | Hybrid vehicle |
CN100370042C (en) * | 2005-05-26 | 2008-02-20 | 唐山市天赫钛业有限公司 | Open direct-cooling condensation technology for vacuum distillation of reduction distillation furnace |
KR101219181B1 (en) * | 2012-01-06 | 2013-01-09 | 한국기계연구원 | Device for producing sponge titanium and method in using same |
CN104776722A (en) * | 2015-03-20 | 2015-07-15 | 江苏新辉钛锆装备有限公司 | Variable-frequency ventilation cooling system for titanium sponge and zirconium sponge |
Also Published As
Publication number | Publication date |
---|---|
JP3567209B2 (en) | 2004-09-22 |
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