JPS62290834A - Manufacturing equipment for metal rhenium - Google Patents
Manufacturing equipment for metal rheniumInfo
- Publication number
- JPS62290834A JPS62290834A JP13386686A JP13386686A JPS62290834A JP S62290834 A JPS62290834 A JP S62290834A JP 13386686 A JP13386686 A JP 13386686A JP 13386686 A JP13386686 A JP 13386686A JP S62290834 A JPS62290834 A JP S62290834A
- Authority
- JP
- Japan
- Prior art keywords
- metal
- rhenium
- temp
- subjected
- gas
- 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
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 20
- 239000002184 metal Substances 0.000 title claims abstract description 20
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 229910052702 rhenium Inorganic materials 0.000 title claims description 7
- 230000008016 vaporization Effects 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000006200 vaporizer Substances 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000009834 vaporization Methods 0.000 claims description 8
- DYIZHKNUQPHNJY-UHFFFAOYSA-N oxorhenium Chemical compound [Re]=O DYIZHKNUQPHNJY-UHFFFAOYSA-N 0.000 abstract description 12
- 229910003449 rhenium oxide Inorganic materials 0.000 abstract description 12
- QSHYGLAZPRJAEZ-UHFFFAOYSA-N 4-(chloromethyl)-2-(2-methylphenyl)-1,3-thiazole Chemical compound CC1=CC=CC=C1C1=NC(CCl)=CS1 QSHYGLAZPRJAEZ-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000843 powder Substances 0.000 abstract description 3
- 238000001291 vacuum drying Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 101100356020 Haemophilus influenzae (strain ATCC 51907 / DSM 11121 / KW20 / Rd) recA gene Proteins 0.000 description 1
- 101100042680 Mus musculus Slc7a1 gene Proteins 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
Abstract
Description
【発明の詳細な説明】 ３、発明の詳細な説明 ユ班り反亜公災 本発明は、金属レニウｔ、の製造装置に関する。[Detailed description of the invention] 3. Detailed description of the invention Yu group anti-Asia public disaster TECHNICAL FIELD The present invention relates to an apparatus for manufacturing metal resin.
発明の従来復権 金属レニウム粉の製造方法は、種々提案されている。Restoration of traditional rights to inventions Various methods for producing metal rhenium powder have been proposed.
例えば、粗製Ｒｅ金属を１０００℃で水素還元した後７
５０〜８５０’Ｃで塩素ガスを通じて塩素化し、生成し
たＲｅＣ１，は、１０℃の冷水中に入れて加水分解させ
、Ｒｅ Ｏ，を約７５％の収率で得る。このＲｅｄ、を
４００℃で１時間１次に６００℃で１時間、水素還元す
る。For example, after hydrogen reduction of crude Re metal at 1000°C,
After chlorination through chlorine gas at 50-850'C, the generated ReC1, is hydrolyzed in cold water at 10C to obtain Re2O, with a yield of about 75%. This Red was reduced with hydrogen at 400° C. for 1 hour and then at 600° C. for 1 hour.
前記で得られた焼結物は、さらに砕かれ、８００℃で２
時間水素還元して、金属Ｒｅ （９９，９５％）を得る
方法がある。The sintered product obtained above was further crushed and heated at 800°C for 2
There is a method of obtaining metal Re (99,95%) by hydrogen reduction for a period of time.
また、他の方法では、粗金属Ｒｅを酸化し、水に溶解し
、精製、晶出させ、 Ｎ Ｈ４Ｒｅ Ｏ４を得た後、乾
燥後、水素で還元（８００℃）する方法がある。一方、
これらについての特段の処理装置は、開示されていない
。Another method is to oxidize crude metal Re, dissolve it in water, purify and crystallize it to obtain N H4Re O4, and then reduce it with hydrogen (800° C.) after drying. on the other hand,
Special processing devices for these are not disclosed.
以上の方法は、処理工程が長く、簡易に高純度のＲｅを
得ることが難しい欠点があった。The above methods have the disadvantage that the processing steps are long and it is difficult to easily obtain high purity Re.
本発明者等は、鋭意検討した結果、より好ましい方法を
実施するための装置である以下の発明をなした。As a result of intensive studies, the present inventors have made the following invention, which is a device for carrying out a more preferable method.
発ｆｌｕ双
即ち、本発明は、外部加熱式の炉であって、上部は気化
装置であり、下部が還元装置からなることを特徴とする
金属レニウムの製造装置である。In other words, the present invention is an apparatus for manufacturing rhenium metal, which is characterized by an externally heated furnace, the upper part of which is a vaporizer, and the lower part of which is a reduction device.
また、上記発明の実施態様として、気化装置と還元装置
との間に圧力差をつけるため絞り孔を設置して還元装置
からの水素ガスの逆流を防止することを特徴とする」二
記の金属レニウムの製造装置を提供する。Further, as an embodiment of the above invention, a throttle hole is installed to create a pressure difference between the vaporization device and the reduction device to prevent backflow of hydrogen gas from the reduction device. Provides rhenium manufacturing equipment.
また、他の発明としては、外部加熱式の炉であって、上
部は気化装置であり、下部が還元装置であり、還元装置
の下部が冷却装置となっていることを特徴とする金属レ
ニウムの製造装置がある。Another invention is an externally heated furnace for producing metallic rhenium, characterized in that the upper part is a vaporizer, the lower part is a reduction device, and the lower part of the reduction device is a cooling device. There is manufacturing equipment.
分剰プ」Ｕ（ケ敬叫 本発明の装置は、外部加熱式の炉である。'U (ke exclamation) The apparatus of the present invention is an externally heated furnace.
上部は、気化装置であって、気化装置の頂部から過レニ
ウム酸、あるいは酸化レニウムを供給する。また、予め
、過レニウム酸等を所定部所に配置し、パンチ操業を行
うこともできる。The upper part is a vaporizer, and perrhenic acid or rhenium oxide is supplied from the top of the vaporizer. Alternatively, perrhenic acid or the like can be placed in a predetermined location in advance and punch operation can be performed.
過レニウム酸を供給する場合は、気化装置の高さ方向の
中心部より下方に気化用皿を設けるか、あるいは、気化
装置下部に中心部のみが上方に突出しその回りが凹状と
なった構造とし、凹状部に液を受ける構造としてもよい
、後者の装置とすれば、気化皿は不要となる。When supplying perrhenic acid, either install a vaporizing pan below the heightwise center of the vaporizer, or use a structure at the bottom of the vaporizer where only the center protrudes upward and the surrounding area is concave. Alternatively, the device may have a structure in which the liquid is received in a concave portion.If the latter device is used, a vaporization tray is not required.
また、気化用皿を用いる場合は、例えば、ロート状のも
のを先が突出した側を下方に向けて、配置することが好
ましい。In addition, when using a vaporizing dish, it is preferable to arrange a funnel-shaped dish with the protruding end facing downward, for example.
気化用皿を配置した方が、気化した酸化レニウ１１が側
壁に付着せず好ましい。ただこの場合も、気化用皿を炉
の直径に対し、直径の小さいものとして、炉断面に対し
て中心部に配置することが好ましい。It is preferable to arrange a vaporizing plate so that the vaporized Renium oxide 11 does not adhere to the side wall. However, in this case as well, it is preferable that the vaporizing dish be smaller in diameter than the diameter of the furnace and placed in the center of the furnace cross section.
気化した酸化レニウ１１が、炉内壁に接する機会を少な
くすることが好ましいからである。This is because it is preferable to reduce the chances of the vaporized Renium oxide 11 coming into contact with the inner wall of the furnace.
気化装置は、外側に加熱装置を設け、炉内が４００〜６
５０℃となるようにする。The vaporizer is equipped with a heating device on the outside, and the inside of the furnace is heated to 400 to 600℃.
The temperature should be 50℃.
気化装置及び還元装置を形成するものは、例えば、透明
石英等で造られる。Those forming the vaporization device and the reduction device are made of transparent quartz or the like, for example.
還元装置は、上部の気化装置から降下してくる酸化レニ
ウムを還元するため、還元ガス（水素ガス等）の導入管
が配置される。導入管は、還元装置上部に設けることが
好ましい、酸化レニウムとの接触する機会を多くするた
めである。In order to reduce the rhenium oxide falling from the upper vaporizer, the reducing device is provided with an inlet pipe for introducing reducing gas (hydrogen gas, etc.). The introduction pipe is preferably provided at the top of the reduction device, in order to increase the chances of contact with rhenium oxide.
導入管は、還元装置上部に酸化レニウムが降下する周囲
にリング状管を配置することが好ましい。It is preferable that the introduction pipe is a ring-shaped pipe arranged around the area where the rhenium oxide descends to the upper part of the reduction device.
還元ガスが、均一に分散し、かつ酸化レニウムとの接触
も良くなるからである。This is because the reducing gas is uniformly dispersed and has good contact with rhenium oxide.
還元装置の周囲には、加熱装置を設け、内部湿度が６５
０〜１０００℃となるように加熱される。A heating device is installed around the reduction device to maintain an internal humidity of 65%.
It is heated to 0 to 1000°C.
気化装置と同様、透明石英製、もしくはアルミナ製とす
ることが好ましい。Like the vaporizer, it is preferably made of transparent quartz or alumina.
気化装置直と還元装置との圧力は、気化装置がプラス圧
となるよう、圧力計を設は制御される。The pressure directly in the vaporizer and in the reduction device is controlled by designing a pressure gauge so that the vaporizer has a positive pressure.
また、還元装置の下部には、冷却装置を設けることが好
ましい、過レニウム酸を原料とする場合、さらには、還
元ガスにＮ２ガスを使用する場合に、水蒸気が発生する
ためこの蒸気を液化し処理気体量を減少させるためであ
る。In addition, it is preferable to provide a cooling device at the bottom of the reduction device.When perrhenic acid is used as a raw material, and furthermore, when N2 gas is used as the reducing gas, water vapor is generated, so it is necessary to liquefy this vapor. This is to reduce the amount of gas to be processed.
冷却装置は、冷却用パイプ等が設けられていることが好
ましい。It is preferable that the cooling device is provided with a cooling pipe or the like.
得られた金属レニウム粉は、連続、あるいは不連続に冷
却装置、あるいは還元装置下部から抜き取られる。The obtained metal rhenium powder is continuously or discontinuously extracted from the cooling device or the lower part of the reducing device.
抜き取られた金属レニウム粉は、更過等により水と分離
し、真空乾燥等を行うことにより、金属し三つム粉とす
る。The extracted metal rhenium powder is separated from water by rinsing, etc., and then vacuum-dried, etc., to obtain metal rhenium powder.
以上本発明を実施することにより、以下の効果を得る。By implementing the present invention as described above, the following effects can be obtained.
発明の蛎米
（１）本発明装置により、過レニウム酸、あるいは酸化
レニウムから連続的に金属レニウム粉を得ることができ
る。Clamp Rice of the Invention (1) With the apparatus of the present invention, metal rhenium powder can be continuously obtained from perrhenic acid or rhenium oxide.
（２）得られる粉は、９９．９９％以上の高純度であっ
て、粒度１μｍ以下である。(2) The resulting powder has a high purity of 99.99% or more and a particle size of 1 μm or less.
朱傭−例づ− 第１図、第２図をもって、本発明を具体的に説明する。Shumen - Examples - The present invention will be specifically explained with reference to FIGS. 1 and 2.
予め気化装置（１４）内を、Ｎ２ガスにより置換した後
、炉内を６００℃に昇温する。ついで過レニウム酸液（
１）を、ポンプ（２）を介して気化装置（１４）に、投
入する。After replacing the inside of the vaporizer (14) with N2 gas in advance, the inside of the furnace is heated to 600°C. Then perrhenic acid solution (
1) is introduced into the vaporizer (14) via the pump (2).
過レニウム酸は、気化用皿（３）に投入さ才ｔ。Perrhenic acid was poured into the vaporizing dish (3).
加熱装置（４）により昇温保持される。温度は、湿度計
（８）により制御される。The temperature is raised and maintained by a heating device (4). The temperature is controlled by a hygrometer (8).
気化した酸化レニウムは、ロート状（６）のものを、気
化装置下部に設け、該絞り孔（１７）より、還元装置（
１５）に入る。The vaporized rhenium oxide is funnel-shaped (6) provided at the bottom of the vaporization device, and is passed through the reduction device (17) through the aperture hole (17).
Enter 15).
気化袋！（１４）は、透明石英製で、ロート状（６）で
ある下部に設置するものとは、別に設けられる。Vaporizer bag! (14) is made of transparent quartz and is provided separately from the funnel-shaped (6) installed at the bottom.
絞り孔（１７）を出た酸化レニウムは、還元装置入口に
設けた第２図に示すガス装入孔（１２）を有するリング
状装入装置により、水素ガスが投入され還元される。水
素ガスは、バルブ（１３）で調整される。The rhenium oxide that has exited the throttle hole (17) is reduced by hydrogen gas being introduced into the ring-shaped charging device having a gas charging hole (12) shown in FIG. 2 provided at the inlet of the reducing device. Hydrogen gas is regulated with a valve (13).
還元装置（１５）は、加熱装置（７）により炉内が９０
０℃に昇温される。The reduction device (15) has a heating device (7) that reduces the temperature inside the furnace to 90%.
The temperature is raised to 0°C.
温度は、温度計（９）により温度制御される。The temperature is controlled by a thermometer (9).
還元装置（１５）も、透明石英で形成される。The reduction device (15) is also made of transparent quartz.
還元装置（１５）と気化装置（１４）の圧力のバランス
は、気化装置（１４）内が、還元装置（１５）内より１
０＋＋ａＨ，０プラスとなるよう制御される。両装置の
差圧を計測することにより行われる。The balance of pressure between the reducing device (15) and the vaporizing device (14) is such that the inside of the vaporizing device (14) is 1 lower than the inside of the reducing device (15).
It is controlled to be 0++aH, 0 plus. This is done by measuring the differential pressure between both devices.
還元装置下部には、冷却装置（１０）を設け、還元によ
り生じた水蒸気、過レニウム酸液中の水分からの水蒸気
を液化させ、処理気体量を減少させる。A cooling device (10) is provided at the bottom of the reduction device to liquefy the water vapor generated by the reduction and water vapor from the water in the perrhenic acid solution, thereby reducing the amount of gas to be treated.
冷却装置（１０）は、水冷パイプ（１１）が設けられて
いる。The cooling device (10) is provided with a water cooling pipe (11).
以上の装置により、金属レニウム粉を得るが、水も含ん
でいるため、濾過後、真空乾燥をすることにより、純度
９９．９９％以上、平均粒径０．１〜０．５μｍの金属
レニウム粉を得た。Metal rhenium powder is obtained using the above apparatus, but since it also contains water, it is filtered and vacuum dried to obtain metal rhenium powder with a purity of 99.99% or more and an average particle size of 0.1 to 0.5 μm. I got it.
尖凰員ス
実施例】−と同様であるが、第３図に示すように、気化
袋Ｈ（１４）下部に中心部が凸状（１６）とし、前記凸
部に気化した酸化レニウムの絞り孔を形成し、その外周
が凹となっており、気化用皿の役割をなしているものを
還元装置（１５）との間に設けて行った。Embodiment] Same as -, but as shown in Fig. 3, the lower part of the vaporizer bag H (14) has a convex center (16), and the convex part is filled with vaporized rhenium oxide. A hole was formed, the outer periphery of which was concave, and a device serving as a vaporizing plate was provided between the reducing device (15) and the reducing device (15).
第１図に示す気化用皿（３）を用いず実施例１と同様な
金属レニウム粉を得ることができた。A metal rhenium powder similar to that in Example 1 could be obtained without using the vaporizing dish (3) shown in FIG.
第１図は、本発明の一態様である製造装置を示す。第２
図は、水素ガス投入リングである。第３図は、気化装置
と還元装置の中間に設けた絞り孔と同時に気化用皿を兼
ねたものである。
１４は、気化装置、１５は、還元装置を示す。FIG. 1 shows a manufacturing apparatus that is one embodiment of the present invention. Second
The figure shows the hydrogen gas injection ring. FIG. 3 shows an aperture hole provided between the vaporization device and the reduction device, which also serves as a vaporization plate. 14 is a vaporization device, and 15 is a reduction device.
Claims (3)
、下部が還元装置からなることを特徴とする金属レニウ
ムの製造装置。(1) An apparatus for manufacturing rhenium metal, which is an external heating type furnace, and is characterized by having a vaporizer in the upper part and a reduction apparatus in the lower part.
絞り孔を設置して還元装置からの水素ガスの逆流を防止
することを特徴とする特許請求の範囲第１項記載の金属
レニウムの製造装置。(2) Metal rhenium according to claim 1, characterized in that a throttle hole is installed to create a pressure difference between the vaporization device and the reduction device to prevent hydrogen gas from flowing back from the reduction device. manufacturing equipment.
、下部が還元装置であり、還元装置の下部が冷却装置と
なっていることを特徴とする金属レニウムの製造装置。(3) An apparatus for manufacturing rhenium metal, which is an externally heated furnace, comprising a vaporizer in the upper part, a reduction apparatus in the lower part, and a cooling apparatus in the lower part of the reduction apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13386686A JPS62290834A (en) | 1986-06-11 | 1986-06-11 | Manufacturing equipment for metal rhenium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13386686A JPS62290834A (en) | 1986-06-11 | 1986-06-11 | Manufacturing equipment for metal rhenium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62290834A true JPS62290834A (en) | 1987-12-17 |
| JPH029095B2 JPH029095B2 (en) | 1990-02-28 |
Family
ID=15114883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13386686A Granted JPS62290834A (en) | 1986-06-11 | 1986-06-11 | Manufacturing equipment for metal rhenium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62290834A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01303942A (en) * | 1988-06-01 | 1989-12-07 | Hitachi Ltd | Communication control system |
| JP2010168629A (en) * | 2009-01-23 | 2010-08-05 | Dowa Metals & Mining Co Ltd | Method for recovering rhenium |
| CN114561543A (en) * | 2022-03-01 | 2022-05-31 | 合肥工业大学 | Device and method for recovering rhenium powder from tungsten-rhenium alloy scrap |
-
1986
- 1986-06-11 JP JP13386686A patent/JPS62290834A/en active Granted
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01303942A (en) * | 1988-06-01 | 1989-12-07 | Hitachi Ltd | Communication control system |
| JP2528938B2 (en) * | 1988-06-01 | 1996-08-28 | 株式会社日立製作所 | Communication control system |
| JP2010168629A (en) * | 2009-01-23 | 2010-08-05 | Dowa Metals & Mining Co Ltd | Method for recovering rhenium |
| CN114561543A (en) * | 2022-03-01 | 2022-05-31 | 合肥工业大学 | Device and method for recovering rhenium powder from tungsten-rhenium alloy scrap |
| CN114561543B (en) * | 2022-03-01 | 2023-09-29 | 合肥工业大学 | Device and method for recycling rhenium powder from tungsten-rhenium alloy waste |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH029095B2 (en) | 1990-02-28 |
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