JPH0754017A - Method and apparatus for producing titanium powder - Google Patents
Method and apparatus for producing titanium powderInfo
- Publication number
- JPH0754017A JPH0754017A JP20519893A JP20519893A JPH0754017A JP H0754017 A JPH0754017 A JP H0754017A JP 20519893 A JP20519893 A JP 20519893A JP 20519893 A JP20519893 A JP 20519893A JP H0754017 A JPH0754017 A JP H0754017A
- Authority
- JP
- Japan
- Prior art keywords
- container
- dehydrogenation
- hydrogenation
- titanium
- treatment
- 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.)
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Abstract
(57)【要約】
【目的】 水素化脱水素法によるチタン粉末の製造にお
いて、脱水素化処理で発生する水素ガスを有効利用する
とともに、水素化処理で発生する熱も有効利用して、消
エネ、生産性向上、設備費用の削減等を達成する。
【構成】 水素化処理容器および脱水素化処理容器を同
一の熱処理炉に装入し、脱水素化処理で発生する水素ガ
スを、水素化処理で利用するとともに、水素化処理で発
生する熱を脱水素化処理で利用することにより、両処理
を同時進行的に行う方法。また、水素化容器、脱水素化
容器、および両容器を一体的に覆う熱処理炉からなる装
置。
(57) [Summary] [Objective] In the production of titanium powder by the hydrodehydrogenation method, the hydrogen gas generated in the dehydrogenation treatment is effectively used, and the heat generated in the hydrotreatment is also effectively utilized to eliminate the hydrogen. Achieve energy saving, productivity improvement, equipment cost reduction, etc. [Structure] The hydrogenation treatment container and the dehydrogenation treatment container are charged into the same heat treatment furnace, and the hydrogen gas generated in the dehydrogenation treatment is used in the hydrogenation treatment and the heat generated in the hydrogenation treatment is used. A method in which both treatments are carried out simultaneously by being used in the dehydrogenation treatment. Also, a device comprising a hydrogenation container, a dehydrogenation container, and a heat treatment furnace that integrally covers both containers.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、粉末冶金原料としての
純チタン粉末またはチタン合金粉末（本明細書ではこれ
らを総称してチタン粉末という）を、水素化脱水素法
（以下ＨＤＨ法という）により製造する方法および装置
に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention uses a pure titanium powder or a titanium alloy powder (herein collectively referred to as titanium powder) as a powder metallurgical raw material by a hydrodehydrogenation method (hereinafter referred to as HDH method). The present invention relates to a method and an apparatus manufactured by.
【０００２】[0002]
【従来の技術】チタン合金は比強度が高く、耐熱性およ
び耐食性に優れており、航空機等の材料として極めて有
効な特性を具備しているが、溶解、鍛造や圧延等の熱間
加工性および切削加工性に難点がある。このため、加工
費低減や歩留向上の観点から、最終形状に近い半製品を
直接製造する技術として、粉末冶金法が有望になってい
る。粉末冶金によりチタン合金を製造する場合、原料と
して純チタン粉末と合金元素添加用粉末の混合粉末を用
いる方法、およびチタン合金粉末を用いる方法がある。2. Description of the Related Art Titanium alloys have high specific strength, excellent heat resistance and corrosion resistance, and have properties that are extremely effective as materials for aircraft and the like, but hot workability such as melting, forging and rolling and Difficulty in machinability. Therefore, from the viewpoint of reducing the processing cost and improving the yield, the powder metallurgy method is promising as a technique for directly manufacturing a semi-finished product having a final shape. When a titanium alloy is manufactured by powder metallurgy, there are a method of using a mixed powder of pure titanium powder and a powder for adding an alloy element as a raw material, and a method of using a titanium alloy powder.
【０００３】純チタン粉末の製造方法としては、スポン
ジチタンを機械的に直接粉砕して粉末とする方法もある
が、スポンジチタンは展延性に富むため、粉砕するのが
困難であり、また、得られたとしても塩素分が多いた
め、粉末冶金用としては低品質のものとなる。一方、チ
タン粉末の製造方法として、純チタンまたはチタン合金
（以下これらを総称してチタンという）の融液をガスで
飛散させて粉末とするアトマイズ法、あるいはチタン電
極を回転させ、プラズマ等で溶融し、遠心力で飛散させ
て粉末とする回転電極法がある。これらの方法によれ
ば、比較的純度の高いチタン粉末が得られるが、粉末個
々の形状や粒度、コスト等に難点がある。As a method of producing pure titanium powder, there is a method of directly mechanically crushing titanium sponge into powder, but since titanium sponge is rich in spreadability, it is difficult to pulverize it, and Even if it is produced, it will be of low quality for powder metallurgy due to its high chlorine content. On the other hand, as a method for producing titanium powder, an atomizing method in which a melt of pure titanium or a titanium alloy (hereinafter collectively referred to as titanium) is dispersed by a gas to form powder, or a titanium electrode is rotated and melted by plasma or the like. Then, there is a rotating electrode method in which the powder is dispersed by centrifugal force. According to these methods, a titanium powder having a relatively high purity can be obtained, but there are problems in the shape, particle size, cost, etc. of each powder.
【０００４】このため、チタンを水素化処理して脆弱な
チタン水素化物とし、これを機械的に粉砕して粉末にし
た後、真空加熱等により脱水素してチタン粉末を得るＨ
ＤＨ法による方法が一般的に採用されている。水素化処
理して常温で脆弱なチタン水素化物を得るためには、水
素を約３重量％以上吸収させる必要がある。この水素を
約３重量％以上含有する水素化物は一般にδ相といわれ
ている。そして、チタンの水素化は３００〜５００℃の
低温域が最も効率が良いとされているが、原料であるチ
タンの表層には、水素侵入のバリヤーとなる酸化層が存
在するため、５００〜６００℃以上に加熱し、この酸化
層を内部拡散させて無害化することが望ましい。そこ
で、原料チタンを６００〜７００℃に加熱した後、徐々
に冷却して水素化を行うことが効率的な操業法である。For this reason, titanium is hydrogenated to give a brittle titanium hydride, which is mechanically pulverized into powder and then dehydrogenated by vacuum heating or the like to obtain titanium powder H
The method based on the DH method is generally adopted. In order to obtain a brittle titanium hydride at room temperature by hydrotreating, it is necessary to absorb about 3% by weight or more of hydrogen. A hydride containing about 3% by weight or more of hydrogen is generally called a δ phase. And, it is said that the hydrogenation of titanium is most efficient in the low temperature range of 300 to 500 ° C., but since the surface layer of titanium as a raw material has an oxide layer which serves as a barrier for hydrogen penetration, it is 500 to 600. It is desirable to heat the material at a temperature of not less than 0 ° C. to internally diffuse the oxide layer to render it harmless. Therefore, an efficient operating method is to heat the raw material titanium to 600 to 700 ° C. and then gradually cool it to perform hydrogenation.
【０００５】従来のＨＤＨ法における水素化処理は、図
３に示すような装置により行われ、原料チタン１３の温
度推移は、例えば図５のようであった。主な工程を以下
に説明する。 （１）原料チタン１３を水素化容器１に装入し、ポンプ
１１で排気する。 （２）熱処理炉３の炉壁ヒーター５をＯＮにし、加熱を
開始する。 （３）原料チタン１３の外周部が６００〜７００℃に達
したら、炉壁ヒーター５をＯＦＦにし、熱処理炉３を取
り外し、水素化容器１を風冷開始する。 （４）ポンプ１０で水素化容器１内に水素ガスを供給開
始する。 （５）原料チタン１３の水素化が進行し、発熱反応によ
り、中心部に向かって温度が上昇する。 （６）水素化容器１内が所定の圧に保たれるよう水素ガ
スを補充する。 （７）水素化が完了したら、供給ガスを水素からアルゴ
ンに切り替え、室温まで冷却する。The hydrogenation treatment in the conventional HDH method was carried out by an apparatus as shown in FIG. 3, and the temperature transition of the raw material titanium 13 was as shown in FIG. 5, for example. The main steps will be described below. (1) The raw material titanium 13 is charged into the hydrogenation container 1 and exhausted by the pump 11. (2) Turn on the furnace wall heater 5 of the heat treatment furnace 3 to start heating. (3) When the outer peripheral portion of the raw material titanium 13 reaches 600 to 700 ° C., the furnace wall heater 5 is turned off, the heat treatment furnace 3 is removed, and the hydrogenation container 1 is started to be air-cooled. (4) The pump 10 starts supplying hydrogen gas into the hydrogenation container 1. (5) Hydrogenation of the raw material titanium 13 progresses, and the temperature rises toward the center due to the exothermic reaction. (6) Hydrogen gas is replenished so that the inside of the hydrogenation container 1 is maintained at a predetermined pressure. (7) When the hydrogenation is completed, the supply gas is switched from hydrogen to argon and cooled to room temperature.
【０００６】つぎに従来のＨＤＨ法における脱水素処理
は、図４に示すような装置により行われ、水素化チタン
粉末１４の温度推移は、例えば図６のようであった。主
な工程を以下に説明する。 （１）水素化チタン粉末１４を皿状容器１５に３０〜５
０mm程度の層厚にし、脱水素化容器２内に多段に積み、
ポンプ１２で排気する。 （２）熱処理炉３の炉壁ヒーター５をＯＮにし、排気し
つつ６００〜７００℃に加熱する。 （３）脱水素化が完了したら、炉壁ヒーター５をＯＦＦ
にし、熱処理炉３を取り外す。 （４）脱水素化容器２内にアルゴンガスを導入し、内圧
を大気圧に保持しながら容器２を室温まで風冷する。Next, the dehydrogenation treatment in the conventional HDH method was performed by the apparatus shown in FIG. 4, and the temperature transition of the titanium hydride powder 14 was as shown in FIG. 6, for example. The main steps will be described below. (1) Titanium hydride powder 14 is placed in a dish-shaped container 15 in an amount of 30 to 5
A layer thickness of about 0 mm and stacked in multiple stages in the dehydrogenation container 2,
Exhaust with the pump 12. (2) The furnace wall heater 5 of the heat treatment furnace 3 is turned on and heated to 600 to 700 ° C. while exhausting. (3) When the dehydrogenation is completed, turn off the furnace wall heater 5
Then, the heat treatment furnace 3 is removed. (4) Argon gas is introduced into the dehydrogenation container 2, and the container 2 is air-cooled to room temperature while maintaining the internal pressure at atmospheric pressure.
【０００７】[0007]
【発明が解決しようとする課題】このように従来のＨＤ
Ｈ法においては、水素化処理と脱水素化処理は、別々の
炉を用いるか、あるいは同一の炉を使用する場合でも各
処理が別々に行われており、次のような問題点を有して
いた。 （１）水素化処理は発熱反応であるため、ヒーターをＯ
ＦＦにした後も、原料チタンの自己燃焼により、１００
０℃近くまで過熱され、冷却に時間がかかり、無駄なエ
ネルギーを消費する。 （２）脱水素化処理は吸熱反応であるため、容器中心部
の水素化チタン粉末の温度上昇に時間がかかる。 （３）脱水素化処理の温度を高めにすると、脱水素粉が
凝結するおそれがある。 （４）脱水素化処理で発生する水素ガスは、高純度であ
るにもかかわらず、廃棄されていた。As described above, the conventional HD
In the H method, the hydrogenation treatment and the dehydrogenation treatment are performed in different furnaces, or even when the same furnace is used, the respective treatments are performed separately, which causes the following problems. Was there. (1) Since the hydrogenation treatment is an exothermic reaction, the heater is turned off.
Even after FF, 100% is obtained due to self-combustion of raw material titanium.
It is overheated to near 0 ° C, it takes time to cool, and wastes energy. (2) Since the dehydrogenation treatment is an endothermic reaction, it takes time to raise the temperature of the titanium hydride powder in the center of the container. (3) If the temperature of the dehydrogenation treatment is raised, the dehydrogenated powder may condense. (4) The hydrogen gas generated by the dehydrogenation treatment was discarded despite its high purity.
【０００８】本発明は、ＨＤＨ法によるチタン粉末の製
造において、脱水素化処理で発生する高純度の水素ガス
を水素化処理に有効利用するとともに、水素化処理で発
生する熱を脱水素化処理に有効利用することにより、設
備費用の削減、生産性向上等を達成することを目的とす
る。According to the present invention, in the production of titanium powder by the HDH method, the high-purity hydrogen gas generated in the dehydrogenation treatment is effectively used in the hydrogenation treatment, and the heat generated in the hydrogenation treatment is dehydrogenation treated. The objective is to achieve equipment cost reduction, productivity improvement, etc.
【０００９】[0009]
【課題を解決するための手段】上記目的を達成するため
に、本発明は以下の構成を要旨とする。すなわち、本発
明法は、ＨＤＨ法において、水素化処理を行う容器およ
び脱水素化処理を行う容器を同一の熱処理炉に装入し、
水素化チタン粉末の脱水素化処理で発生する水素ガス
を、原料チタンの水素化処理で利用するとともに、水素
化処理で発生する熱を脱水素化処理で利用することによ
り、水素化処理および脱水素化処理を同時進行的に行う
ことを特徴とするチタン粉末の製造方法である。In order to achieve the above object, the present invention has the following structures. That is, in the method of the present invention, in the HDH method, a vessel for performing a hydrogenation treatment and a vessel for performing a dehydrogenation treatment are charged in the same heat treatment furnace,
By using the hydrogen gas generated by the dehydrogenation treatment of titanium hydride powder in the hydrogenation treatment of the titanium raw material and the heat generated in the hydrogenation treatment in the dehydrogenation treatment, It is a method for producing titanium powder, which is characterized by simultaneously performing the oxidization treatment.
【００１０】また本発明装置は、水素化容器、脱水素化
容器、および両容器を一体的に覆う熱処理炉からなり、
水素化容器には水素ガス導入管および排気ポンプが接続
され、脱水素化容器には内部ヒーターが配設され、かつ
水素ガス排出管が接続され、水素ガス排出管は逆止弁を
経て水素ガス導入管に連結されていることを特徴とする
チタン粉末の製造装置である。The apparatus of the present invention comprises a hydrogenation vessel, a dehydrogenation vessel, and a heat treatment furnace that integrally covers both vessels.
A hydrogen gas introduction pipe and an exhaust pump are connected to the hydrogenation container, an internal heater is arranged in the dehydrogenation container, and a hydrogen gas discharge pipe is connected, and the hydrogen gas discharge pipe is connected to the hydrogen gas through a check valve. The titanium powder manufacturing apparatus is characterized in that it is connected to an introduction pipe.
【００１１】なお、本発明において「チタン」は純チタ
ンまたはチタン合金を総称したものである。すなわち、
原料チタンは純チタンでもチタン合金でもよく、純チタ
ンの原料からは純チタン粉末が得られ、チタン合金の原
料からはチタン合金粉末が得られる。In the present invention, "titanium" is a general term for pure titanium or titanium alloy. That is,
The raw material titanium may be pure titanium or a titanium alloy, pure titanium powder is obtained from the pure titanium raw material, and titanium alloy powder is obtained from the titanium alloy raw material.
【００１２】[0012]
【作用】以下、図面により本発明を詳細に説明する。図
１は本発明装置の断面図であり、水素化容器１、脱水素
化容器２、および両容器を一体的に覆う熱処理炉３から
なり、水素化容器１には水素ガス導入管６および排気管
８が接続され、脱水素化容器２には内部ヒーター４が配
設され、かつ水素ガス排出管７が接続され、水素ガス排
出管７は逆止弁９を経て水素ガス導入管６に連結されて
いる。The present invention will be described in detail below with reference to the drawings. FIG. 1 is a cross-sectional view of the apparatus of the present invention, which comprises a hydrogenation container 1, a dehydrogenation container 2, and a heat treatment furnace 3 that integrally covers both containers. The hydrogenation container 1 includes a hydrogen gas introduction pipe 6 and an exhaust gas. A pipe 8 is connected, an internal heater 4 is provided in the dehydrogenation container 2, and a hydrogen gas discharge pipe 7 is connected. The hydrogen gas discharge pipe 7 is connected to a hydrogen gas introduction pipe 6 via a check valve 9. Has been done.
【００１３】本発明法は、このような装置を用い、つぎ
のような手順で行うことができる。 （１）水素化容器１に原料チタン１３を、脱水素化容器
２に水素化チタン粉末１４をそれぞれ装入する。原料チ
タン１３としては、スポンジチタン、チタン製品あるい
は中間製品の切削屑、端切れ材等のスクラップが適用で
きる。水素化チタン粉末１４は、上記原料チタンを水素
化し粉砕し篩別したものであり、粉末を皿状容器１５に
入れたものを多段に積んで装入する。皿状容器１５は中
央部が空胴になったドーナツ状で、内周および外周の縁
に切欠１６が設けてあり、空胴部に内部ヒーター４が通
してある。The method of the present invention can be carried out in the following procedure using such a device. (1) A raw material titanium 13 is charged in the hydrogenation container 1, and a titanium hydride powder 14 is charged in the dehydrogenation container 2. As the raw material titanium 13, sponge titanium, scraps of titanium products or intermediate products, scraps such as scraps, etc. can be applied. The titanium hydride powder 14 is obtained by hydrogenating and sieving the raw material titanium, and the powder is placed in a dish-shaped container 15 and loaded in multiple stages. The dish-shaped container 15 is in the shape of a doughnut having a hollow central portion, is provided with notches 16 at the inner and outer peripheral edges, and the internal heater 4 is passed through the hollow portion.
【００１４】（２）ポンプ１１および１２で水素化容器
１および脱水素化容器２内を排気する。容器１および２
内の真空度は１０-3torr以下とするのが好ましい。 （３）ポンプ１２を停止し、内部ヒーター４をＯＮにし
て、脱水素化容器２内の水素化チタン粉末１４を加熱す
る。 （４）脱水素化容器２内が４００℃に達したら、炉壁ヒ
ーター５をＯＮにし、熱処理炉３内全体を加熱する。(2) The pumps 11 and 12 exhaust the inside of the hydrogenation container 1 and the dehydrogenation container 2. Containers 1 and 2
The internal vacuum degree is preferably 10 -3 torr or less. (3) The pump 12 is stopped and the internal heater 4 is turned on to heat the titanium hydride powder 14 in the dehydrogenation container 2. (4) When the temperature inside the dehydrogenation vessel 2 reaches 400 ° C., the furnace wall heater 5 is turned on to heat the entire inside of the heat treatment furnace 3.
【００１５】（５）脱水素化容器２内にて脱水素化の進
行に伴い発生する水素ガスを、水素ガス排出管７を経
て、ポンプ１０により水素ガス導入管６から、水素化容
器１内に導入する。 （６）水素化容器１の内圧を所定圧に保つように、水素
ガスの過不足は、ポンプ１１による排気と、ポンプ１０
による外部からの水素ガス供給により調節する。 （７）水素化処理の発熱反応により、原料チタン１３が
自己燃焼を開始した後は、炉壁ヒーター５をＯＦＦにす
る。(5) The hydrogen gas generated along with the progress of dehydrogenation in the dehydrogenation container 2 is passed through the hydrogen gas discharge pipe 7 and the pump 10 from the hydrogen gas introduction pipe 6 into the hydrogenation container 1. To introduce. (6) Excess and shortage of hydrogen gas is exhausted by the pump 11 and the pump 10 so that the internal pressure of the hydrogenation container 1 is maintained at a predetermined pressure.
It is adjusted by supplying hydrogen gas from the outside. (7) After the raw material titanium 13 starts self-combustion due to the exothermic reaction of the hydrogenation treatment, the furnace wall heater 5 is turned off.
【００１６】（８）脱水素化処理が完了したら、内部ヒ
ーター４をＯＦＦにし、熱処理炉３を取り外し、水素化
容器１および脱水素化容器２を風冷する。脱水素化処理
完了後の水素化処理は、（６）のとおり、外部からの水
素ガス供給により行う。 （９）水素化された原料チタン１３、あるいは脱水素化
されたチタン粉末１４は、それぞれ水素化容器１、ある
いは脱水素化容器２が室温まで冷却された後、取り出
す。 （１０）脱水素化完了後の脱水素化容器２内の冷却に際
し、容器２内にアルゴンガスを導入した方が、冷却が促
進され好ましい。 （１１）水素化容器１内の冷却に際しては、容器１内の
導入ガスを、水素化が殆ど生じなくなる３００℃以下
で、水素からアルゴンに切替えた方が冷却が促進されて
好ましい。(8) When the dehydrogenation process is completed, the internal heater 4 is turned off, the heat treatment furnace 3 is removed, and the hydrogenation container 1 and the dehydrogenation container 2 are air-cooled. The hydrogenation process after completion of the dehydrogenation process is performed by supplying hydrogen gas from the outside, as described in (6). (9) The hydrogenated raw material titanium 13 or the dehydrogenated titanium powder 14 is taken out after the hydrogenation container 1 or the dehydrogenation container 2 is cooled to room temperature, respectively. (10) When cooling the inside of the dehydrogenation container 2 after completion of dehydrogenation, it is preferable to introduce an argon gas into the container 2 because cooling is promoted. (11) When cooling the hydrogenation container 1, it is preferable to switch the introduced gas into the container 1 from hydrogen to argon at 300 ° C. or less at which hydrogenation hardly occurs, because the cooling is promoted.
【００１７】このような本発明において、上記（５）の
脱水素化処理で発生する水素ガスは高純度のものであ
り、従来法において、水素化処理に使用されていた酸化
防止のための高純度水素ガスに十分代替可能な純度を有
している。したがって、本発明により、従来廃棄されて
いた高純水素ガスが有効利用される。さらに、上記
（７）において、水素化容器１で発生した熱が、同一炉
内にある脱水素化容器２内に伝熱され、水素化処理の発
熱反応および脱水素化処理の吸熱反応が効果的に促進さ
れる。In the present invention as described above, the hydrogen gas generated in the dehydrogenation treatment of the above (5) is of high purity, and has a high content for preventing oxidation, which was used in the hydrogenation treatment in the conventional method. Purity It has a purity sufficient to replace hydrogen gas. Therefore, according to the present invention, the highly pure hydrogen gas which has been conventionally discarded can be effectively used. Further, in (7) above, the heat generated in the hydrogenation container 1 is transferred to the dehydrogenation container 2 in the same furnace, and the exothermic reaction of the hydrogenation process and the endothermic reaction of the dehydrogenation process are effective. Be promoted.
【００１８】[0018]
（本発明例） 図１に示す本発明装置により、種々の形
態の商用純チタンスクラップからなる原料チタン１３を
２００ｋｇ水素化容器１に装入し、商用純チタンからな
る水素化チタン粉末１４を合計２００ｋｇ皿状容器１５
に入れ、脱水素化容器２内に積重ねて装入し、図２に示
す温度推移で処理した。水素化処理は水素含有量４％、
脱水素化処理は水素含有量２００ppm までとした。加熱
開始から冷却終了までの合計処理時間は、図２のとお
り、２５時間であった。また消費電力は１６０kwh 、高
純度水素ガス使用量は３５Ｎｍ3 であった。(Example of the present invention) With the apparatus of the present invention shown in FIG. 1, 200 kg of raw material titanium 13 made of commercial pure titanium scrap in various forms was charged into the hydrogenation vessel 1, and the total amount of titanium hydride powder 14 made of commercial pure titanium was added. 200kg dish-shaped container 15
And placed in the dehydrogenation vessel 2 in a stacked manner and treated at the temperature transition shown in FIG. Hydrogen content is 4% hydrogen content,
The dehydrogenation treatment was performed up to a hydrogen content of 200 ppm. The total processing time from the start of heating to the end of cooling was 25 hours as shown in FIG. The power consumption was 160 kwh and the amount of high-purity hydrogen gas used was 35 Nm 3 .
【００１９】（従来例１） 図３に示す従来装置によ
り、本発明例と同様の原料チタンを２００ｋｇ、図５に
示す温度推移で水素化処理した。本発明例と同様、処理
後の水素含有量４％とした。加熱開始から冷却終了まで
の合計処理時間は、図５のとおり、２５時間であった。
また消費電力は１５kwh 、高純度水素ガス使用量は９５
Ｎｍ3 であった。(Conventional Example 1) Using the conventional apparatus shown in FIG. 3, 200 kg of the same raw material titanium as in the present invention was hydrotreated at the temperature transition shown in FIG. The hydrogen content after treatment was set to 4% as in the case of the present invention. The total processing time from the start of heating to the end of cooling was 25 hours as shown in FIG.
Power consumption is 15kWh and high-purity hydrogen gas consumption is 95
It was Nm 3 .
【００２０】（従来例２） 図４に示す従来装置によ
り、本発明例と同様の水素化チタン粉末を２００ｋｇ、
図６に示す温度推移で脱水素化処理した。本発明例と同
様、処理後の水素含有量２００ppm とした。加熱開始か
ら冷却終了までの合計処理時間は、図６のとおり、７５
時間であった。また消費電力は３００kwh であった。(Prior Art Example 2) Using the conventional apparatus shown in FIG. 4, 200 kg of the same titanium hydride powder as in the invention example was
The dehydrogenation treatment was performed at the temperature transition shown in FIG. The hydrogen content after treatment was set to 200 ppm as in the case of the present invention. The total processing time from the start of heating to the end of cooling is 75
It was time. The power consumption was 300 kwh.
【００２１】上記のように、本発明により、水素ガスお
よび反応熱が有効に利用され、処理時間短縮および省電
力に顕著な効果が認められた。また、種々の形態のチタ
ン合金（Ｔｉ−６Ａｌ−４Ｖ）スクラップを原料チタン
とした場合も、上記と同様の効果が得られた。As described above, according to the present invention, the hydrogen gas and the heat of reaction are effectively used, and the remarkable effects in shortening the processing time and power saving are recognized. Also, when titanium alloy (Ti-6Al-4V) scraps of various forms were used as raw material titanium, the same effect as above was obtained.
【００２２】[0022]
【発明の効果】本発明によれば、水素化脱水素法による
チタン粉末の製造において、チタンの水素化および脱水
素化が、一体化された炉内で同時進行的に行われ、脱水
素化処理で発生する水素ガスが水素化処理に有効利用さ
れるとともに、水素化処理で発生する熱が脱水素化処理
に有効利用される。このため、水素使用量の大幅な削
減、脱水素化処理時間の大幅な短縮に伴う真空ポンプ運
転時間短縮による消電力、水素化処理反応熱の有効利用
によるエネルギー使用の削減、処理時間短縮に伴う生産
性の著しい向上、さらに、装置の簡易化による設備費用
および保守費用の削減等の効果が得られる。According to the present invention, in the production of titanium powder by the hydrodehydrogenation method, the hydrogenation and dehydrogenation of titanium are carried out simultaneously in an integrated furnace to carry out dehydrogenation. The hydrogen gas generated by the treatment is effectively used for the hydrogenation treatment, and the heat generated by the hydrogenation treatment is effectively used for the dehydrogenation treatment. Therefore, the amount of hydrogen used is greatly reduced, the power consumption is reduced by shortening the vacuum pump operating time with the drastic reduction of the dehydrogenation treatment time, the energy use is reduced by the effective use of the heat of the hydrogenation treatment reaction, and the treatment time is shortened. The productivity can be remarkably improved, and the facility cost and maintenance cost can be reduced by simplifying the device.
【図１】本発明装置の例を示す中央部断面図である。FIG. 1 is a central sectional view showing an example of a device of the present invention.
【図２】本発明法における温度推移を示すグラフであ
る。FIG. 2 is a graph showing a temperature transition in the method of the present invention.
【図３】従来の水素化処理装置の例を示す中央部断面図
である。FIG. 3 is a central sectional view showing an example of a conventional hydrotreating apparatus.
【図４】従来の脱水素化処理装置の例を示す中央部断面
図である。FIG. 4 is a central sectional view showing an example of a conventional dehydrogenation treatment apparatus.
【図５】従来の水素化処理における温度推移を示すグラ
フである。FIG. 5 is a graph showing a temperature transition in a conventional hydrotreatment.
【図６】従来の脱水素化処理における温度推移を示すグ
ラフである。FIG. 6 is a graph showing a temperature transition in the conventional dehydrogenation treatment.
１：水素化容器 ２：脱水素化容器 ３：熱処理炉 ４：内部ヒーター ５：炉壁ヒーター ６：水素ガス導入管 ７：水素ガス排気管 ８：排気管 ９：逆止弁 １０，１１，１２：ポンプ １３：原料チタン １４：水素化チタン粉末 １５：皿状容器 １６：切欠 1: Hydrogenation container 2: Dehydrogenation container 3: Heat treatment furnace 4: Internal heater 5: Furnace wall heater 6: Hydrogen gas introduction pipe 7: Hydrogen gas exhaust pipe 8: Exhaust pipe 9: Check valve 10, 11, 12 : Pump 13: Titanium raw material 14: Titanium hydride powder 15: Dish-shaped container 16: Notch
───────────────────────────────────────────────────── フロントページの続き (72)発明者 山宮 昌夫 東京都千代田区大手町２−６−３ 新日本 製鐵株式会社内 (72)発明者 田村 道夫 兵庫県姫路市広畑区富士町１番地 新日本 製鐵株式会社広畑製鐵所内 (72)発明者 籠橋 亘 神奈川県茅ヶ崎市茅ヶ崎３−３−５ 東邦 チタニウム株式会社内 (72)発明者 深澤 英一 神奈川県茅ヶ崎市茅ヶ崎３−３−５ 東邦 チタニウム株式会社内 (72)発明者 村山 良治 神奈川県茅ヶ崎市茅ヶ崎３−３−５ 東邦 チタニウム株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Masao Yamamiya 2-6-3 Otemachi, Chiyoda-ku, Tokyo Within Nippon Steel Corporation (72) Inventor Michio Tamura 1 Fuji-machi, Hirohata-ku, Himeji-shi, Hyogo New Nippon Steel Co., Ltd., Hirohata Works (72) Inventor Wataru Kagohashi 3-3-5 Chigasaki, Chigasaki City, Kanagawa Prefecture Toho Titanium Co., Ltd. (72) Eiichi Fukazawa 3-3-5 Chigasaki, Chigasaki City, Kanagawa Prefecture Toho Titanium Co., Ltd. (72) Inventor Ryoji Murayama 3-3-5 Chigasaki, Chigasaki City, Kanagawa Toho Titanium Co., Ltd.
Claims (2)
する方法において、水素化処理を行う容器および脱水素
化処理を行う容器を同一の熱処理炉に装入し、水素化チ
タン粉末の脱水素化処理で発生する水素ガスを、原料チ
タンの水素化処理で利用するとともに、水素化処理で発
生する熱を脱水素化処理で利用することにより、水素化
処理および脱水素化処理を同時進行的に行うことを特徴
とするチタン粉末の製造方法。1. A method for producing titanium powder by a hydrodehydrogenation method, wherein a container for hydrotreating and a container for dehydrogenating are charged in the same heat treatment furnace to dehydrogenate titanium hydride powder. The hydrogen gas generated in the hydrogenation process is used in the hydrogenation process of the raw material titanium, and the heat generated in the hydrogenation process is used in the dehydrogenation process, so that the hydrogenation process and the dehydrogenation process can be performed simultaneously. A method for producing titanium powder, characterized in that
器を一体的に覆う熱処理炉からなり、水素化容器には水
素ガス導入管および排気ポンプが接続され、脱水素化容
器には内部ヒーターが配設され、かつ水素ガス排出管が
接続され、水素ガス排出管は逆止弁を経て水素ガス導入
管に連結されていることを特徴とするチタン粉末の製造
装置。2. A hydrogenation container, a dehydrogenation container, and a heat treatment furnace that integrally covers both containers. A hydrogen gas introduction pipe and an exhaust pump are connected to the hydrogenation container, and the dehydrogenation container has an internal structure. An apparatus for producing titanium powder, characterized in that a heater is provided and a hydrogen gas discharge pipe is connected, and the hydrogen gas discharge pipe is connected to a hydrogen gas introduction pipe through a check valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20519893A JPH0754017A (en) | 1993-08-19 | 1993-08-19 | Method and apparatus for producing titanium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20519893A JPH0754017A (en) | 1993-08-19 | 1993-08-19 | Method and apparatus for producing titanium powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0754017A true JPH0754017A (en) | 1995-02-28 |
Family
ID=16503034
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20519893A Withdrawn JPH0754017A (en) | 1993-08-19 | 1993-08-19 | Method and apparatus for producing titanium powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0754017A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009057634A (en) * | 2000-11-09 | 2009-03-19 | Nikko Kinzoku Kk | Manufacturing method for high-purity zirconium or hafnium powder |
| CN103418798A (en) * | 2012-05-22 | 2013-12-04 | 宁波江丰电子材料有限公司 | Method for preparing high-purity titanium powder by residual titanium targets |
-
1993
- 1993-08-19 JP JP20519893A patent/JPH0754017A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009057634A (en) * | 2000-11-09 | 2009-03-19 | Nikko Kinzoku Kk | Manufacturing method for high-purity zirconium or hafnium powder |
| CN103418798A (en) * | 2012-05-22 | 2013-12-04 | 宁波江丰电子材料有限公司 | Method for preparing high-purity titanium powder by residual titanium targets |
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