JP2007291591A5 - Gas phase reactor - Google Patents
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- JP2007291591A5 JP2007291591A5 JP2007007736A JP2007007736A JP2007291591A5 JP 2007291591 A5 JP2007291591 A5 JP 2007291591A5 JP 2007007736 A JP2007007736 A JP 2007007736A JP 2007007736 A JP2007007736 A JP 2007007736A JP 2007291591 A5 JP2007291591 A5 JP 2007291591A5
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- 238000006243 chemical reaction Methods 0.000 claims description 44
- 238000010574 gas phase reaction Methods 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 19
- 239000000376 reactant Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 239000012495 reaction gas Substances 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000002121 nanofiber Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 12
- 239000007792 gaseous phase Substances 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
Description
本発明は気相反応装置に関し、更に詳しくは、粉状あるいは粒子状の被反応物と反応ガスとを接触させる気相反応を間欠的に繰り返す連続バッチ的気相反応装置の改良に関し、特に高品質の１〜３層の中空状ナノファイバーを大量生産するのに好適な気相反応装置に関する。 The present invention relates to a gas phase reactor, more particularly, it relates to an improvement of the powder or particulate of the reactants and the gas phase reaction of contacting a reaction gas intermittently repeated continuously batchwise gas phase reactor, in particular a high The present invention relates to a gas phase reactor suitable for mass-producing high quality 1-3 layers of hollow nanofibers.
本発明の目的は、従来の上記問題を解消し、粉状あるいは粒子状の被反応物を反応ガスと接触させる連続バッチ的反応プロセスのサイクルタイムを短縮するようにした高生産性の気相反応装置を提供することにある。 The object of the present invention is to solve the above-mentioned conventional problems and to reduce the cycle time of a continuous batch reaction process in which a powdery or particulate reactant is brought into contact with a reaction gas. To provide an apparatus .
本発明の他の目的は、従来よりも高品質な反応物を製造することができる気相反応装置を提供することにある。 Another object of the present invention is to provide a gas phase reactor which can produce high-quality reactants than conventional.
本発明の更に他の目的は、高品質な１〜３層のカーボンナノチューブを高い生産性の下に製造可能な気相反応装置を提供することにある。 Still another object of the present invention is to provide a gas phase reaction apparatus capable of producing high-quality 1-3-walled carbon nanotubes with high productivity.
また、上記課題を解決する本発明の気相反応装置は、以下の（１）記載の通りの構成からなる。 Moreover, the gas phase reaction apparatus of the present invention that solves the above problems has a configuration as described in the following (1) .
（１）反応室に、少なくとも反応室加熱手段と、把持体に支持した粉状あるいは粒子状の被反応物を装填及び取り出しする装填・取出手段と、反応ガスを導入する気体導入手段とを設け、前記被反応物と反応ガスとを前記反応室で気相反応させ、該反応室から反応生成物を前記把持体と共に取り出す一連の操作を、新たな被反応物を順次供給しながら連続バッチ的に繰り返す気相反応装置において、
前記反応室の上方に前記反応室に開閉可能なゲート扉で隔離された予備加熱室と、該予備加熱室に前記反応室の気相反応と平行して前記新たな被反応物を昇温処理する予備加熱手段とを設け、前記反応室の下方に前記装填・取出手段を配置し、前記装填・取出手段をシリンダー機構で構成し、該シリンダー機構の合計シリンダーストロークを前記反応室の上下方向の長さよりも長くし、さらに、前記シリンダー機構が、先端にワークを保持する直動部として、少なくとも中空構造の第１シャフトと該第１シャフトの内面に設けたシール部及びガイド部に摺接しながら往復移動する第２シャフトとを設けると共に、前記第１シャフトを往復駆動する第１シリンダーと前記第２シャフトを往復駆動する第２シリンダーとを設け、かつ前記第２シリンダーを該第２シリンダーの軸方向と直交する方向に往復移動させる駆動機構を設けたことを特徴とする気相反応装置。
(1) The reaction chamber is provided with at least a reaction chamber heating unit, a loading / unloading unit for loading and unloading powdery or particulate reactants supported by a gripper, and a gas introduction unit for introducing a reaction gas. A series of operations in which the reactant and the reaction gas are reacted in a gas phase in the reaction chamber, and the reaction product is taken out from the reaction chamber together with the gripper in a continuous batch manner while sequentially supplying new reactants. In the gas phase reactor that repeats
A preheating chamber that is isolated by a gate door that can be opened and closed to the reaction chamber above the reaction chamber , and the preheating chamber is heated in parallel with the gas phase reaction in the reaction chamber. Preheating means, and the loading / unloading means is disposed below the reaction chamber, the loading / unloading means is constituted by a cylinder mechanism, and the total cylinder stroke of the cylinder mechanism is set in the vertical direction of the reaction chamber. The cylinder mechanism is slidably in contact with at least a first shaft having a hollow structure and a seal portion and a guide portion provided on the inner surface of the first shaft as a linear motion portion that holds a workpiece at the tip. A second shaft that reciprocates, a first cylinder that reciprocates the first shaft, and a second cylinder that reciprocates the second shaft, and the second series Gas phase reactor which characterized in that a drive mechanism for reciprocating in a direction orthogonal to loaders and axial of said second cylinder.
また、上述した本発明の気相反応装置は、以下の（２）〜（６）のいずれかの構成からなることが好ましい。
（２）前記第１シャフトを複数の中空軸を直列に着脱に連結した構成にした上記（１）に記載の気相反応装置。
Moreover, it is preferable that the gas phase reaction apparatus of the present invention described above has any one of the following configurations (2) to (6).
(2) The gas phase reaction apparatus according to (1), wherein the first shaft has a configuration in which a plurality of hollow shafts are connected in a detachable manner in series.
（３）前記予備加熱手段を前記予備加熱室の外側に配置し、該予備加熱室の外壁に取り付けた透明板を介して内部を加熱するようにした上記（１）又は（２）に記載の気相反応装置。 (3) The said preheating means is arrange | positioned on the outer side of the said preheating chamber, and the inside is heated through the transparent plate attached to the outer wall of this preheating chamber, The said (1) or (2) description Gas phase reactor.
（４）前記予備加熱室にゲート扉を介して隔離・連通可能に前記被反応物を待機させる投入室を設け、かつ前記反応室での反応生成物を回収する回収室を設けた上記（１）〜（３）のいずれかに記載の気相反応装置。 (4) The preheating chamber is provided with an input chamber for waiting for the reactant to be isolated and communicated via a gate door, and a recovery chamber for recovering a reaction product in the reaction chamber (1 ) To (3) .
（５）前記回収室の前に前記反応生成物を冷却する冷却室を設けた上記（４）に記載の気相反応装置。 (5) The gas phase reactor according to (4), wherein a cooling chamber for cooling the reaction product is provided in front of the recovery chamber.
（６）中空ノファイバーの製造に使用される上記（１）〜（５）のいずれかに記載の気相反応装置。 (6) The gas phase reactor according to any one of (1) to (5) , which is used for producing hollow fiber.
（７）直動往復移動するシリンダー機構において、先端にワークを保持する直動部として、少なくとも中空構造の第１シャフトと該第１シャフトの内面に設けたシール部及びガイド部に摺接しながら往復移動する第２シャフトとを設けると共に、前記第１シャフトを往復駆動する第１シリンダーと前記第２シャフトを往復駆動する第２シリンダーとを設け、かつ前記第２シリンダーを該第２シリンダーの軸方向と直交する方向に往復移動させる駆動機構を設けたシリンダー機構。 (7) In a cylinder mechanism that moves back and forth in a linear motion, as a linear motion portion that holds a workpiece at the tip, it reciprocates while sliding in contact with at least a hollow first shaft, a seal portion provided on the inner surface of the first shaft, and a guide portion. A moving second shaft, a first cylinder for reciprocating the first shaft, a second cylinder for reciprocating the second shaft, and an axial direction of the second cylinder. Cylinder mechanism with a drive mechanism that reciprocates in a direction perpendicular to the axis.
かかる本発明のシリンダー機構は、以下の（８）〜（１０）のいずれかの構成からなることが好ましい。
（８）前記第１シャフトが複数の中空軸を直列に連結した構成からなる上記（７）に記載のシリンダー機構。
Such a cylinder mechanism of the present invention preferably has any one of the following configurations (8) to (10).
(8) The cylinder mechanism according to (7), wherein the first shaft has a configuration in which a plurality of hollow shafts are connected in series.
（９）反応室内を５００℃以上に加熱する加熱手段を有する気相反応装置であって、前記反応室に対する被反応物の装填・取出手段として、上記（７）又は（８）に記載のシリンダー機構を設けた気相反応装置。 (9) A gas phase reaction apparatus having a heating means for heating the reaction chamber to 500 ° C. or more, wherein the cylinder according to (7) or (8) above is used as a loading / unloading means for the reactant to the reaction chamber. A gas phase reactor equipped with a mechanism.
（１０）反応室を減圧する減圧手段を設けた気相反応装置であって、前記反応室に対する被反応物の装填・取出手段として、上記（７）又は（８）に記載のシリンダー機構を設けた気相反応装置。 (10) A gas-phase reaction apparatus provided with a decompression means for decompressing the reaction chamber, wherein the cylinder mechanism according to (7) or (8) is provided as a means for loading / removing the reactant to / from the reaction chamber Gas phase reactor.
本発明の気相反応装置によれば、粉状あるいは粒子状の被反応物と反応ガスとを連続バッチ的に気相反応させる場合に、次の気相反応に供する被反応物を昇温処理する予備加熱室を反応室とは独立に設け、その予備加熱室において反応室の反応工程と平行に昇温処理を実施するようにしたので、従来の気相反応処理よりも反応プロセスのサイクルタイムを短縮し、高い生産性の気相反応処理を行うことが可能になる。 According to the gas phase reaction apparatus of the present invention, when a powdery or particulate reactant and a reaction gas are subjected to a gas phase reaction in a continuous batch manner, the reactant to be subjected to the next gas phase reaction is heated. Since the preheating chamber is provided independently of the reaction chamber and the temperature raising process is performed in parallel with the reaction process of the reaction chamber in the preheating chamber, the cycle time of the reaction process is longer than the conventional gas phase reaction process. This makes it possible to perform gas phase reaction treatment with high productivity.
以下、本発明の気相反応装置と、この気相反応装置において行われる気相反応について、図に示す実施形態を参照しながら具体的に説明する。 Hereinafter, the gas phase reaction apparatus of the present invention and the gas phase reaction performed in the gas phase reaction apparatus will be specifically described with reference to the embodiments shown in the drawings.
図１は本発明の気相反応装置について、その実施形態を例示した概略断面図であり、また図２は図１の気相反応装置における反応室及び予備加熱室を拡大して示す概略断面図である。 FIG. 1 is a schematic cross-sectional view illustrating an embodiment of the gas phase reaction apparatus of the present invention , and FIG. 2 is a schematic cross-sectional view showing an enlarged reaction chamber and preheating chamber in the gas phase reaction apparatus of FIG. It is.
予備加熱ヒーター２１としては、所望の加熱速度、温度分布特性を実現し、かつ加熱雰囲気に対する耐性を有するものであれば特に限定されるものではないが、急速加熱に優れるＳｉＣヒーター、赤外線ヒーターが好ましく適用される。特に、大面積が容易で、安価で製作可能なハロゲンランプ等の赤外線ヒーターが適している。 The preheating heater 21 is not particularly limited as long as it achieves a desired heating rate and temperature distribution characteristics and has resistance to a heating atmosphere, but a SiC heater and an infrared heater excellent in rapid heating are preferable. Applied. In particular, an infrared heater such as a halogen lamp, which has a large area and can be manufactured at low cost, is suitable.
なお、図４に示すシリンダー機構は、予備加熱室を備えた気相反応装置への適用のみに限定されるものではない。反応室のほか、加熱炉、真空チャンバー等に代表される高温、真空、特殊ガス雰囲気等によって内部が特殊環境に晒される構造物に付設して、処理ワークの搬送手段として適用すれば、コンパクトな装置構成でワークを特殊環境下に対して搬送することができる。特に、５００℃以上の反応室への被反応物の装填、取出手段として、このシリンダー機構を適用すれば、ガイド部やシール部などを高温下に晒すことが少なく、シリンダーの耐久性、動作の高い信頼性を確保することができる。また、減圧された反応室への被反応物の装填・取出手段としてこのシリンダー機構を適用すれば、中空構造の第１シャフトの外側と内側に設けたシール部によって反応室内部の密閉性を確保できるので、減圧状態を維持したまま、被反応物の装填・回収が行えて、サイクルタイムの短縮化を可能することができる。 Note that the cylinder mechanism shown in FIG. 4 is not limited to application to a gas phase reaction apparatus having a preheating chamber. In addition to the reaction chamber, if it is attached to a structure that is exposed to a special environment due to high temperature, vacuum, special gas atmosphere, etc. represented by a heating furnace, vacuum chamber, etc., it can be used as a transport means for processing work. The workpiece can be transported to a special environment with the device configuration. In particular, if this cylinder mechanism is applied as a means for loading and unloading a reaction product into a reaction chamber of 500 ° C. or higher, the guide part and the seal part are not exposed to high temperatures, and the durability and operation of the cylinder are reduced. High reliability can be ensured. In addition, if this cylinder mechanism is applied as means for loading / removing the reactants to / from the decompressed reaction chamber, the inside of the reaction chamber is secured by the sealing portions provided on the outer and inner sides of the hollow first shaft. since it, while maintaining the vacuum state, and can be loaded and recovery of the reactants, it is possible to allow the shortening of the cycle time.
本発明の気相反応装置を用いることによって、気相反応は、以下に説明するようにして行われる。 By using the gas phase reaction apparatus of the present invention , the gas phase reaction is performed as described below .
本発明の気相反応装置を用いて行われる気相反応方法は、中空カーボンファイバーの製造に好適に使用することができる。すなわち、担体に触媒金属を担持させ、５００℃〜１２００℃、好ましくは６００℃〜９５０℃の温度で触媒金属と炭素含有化合物とを接触させて気相反応を行わせることにより、電子放出特性、導電性、強度、触媒担持分散性に優れた特に単層〜３層を主成分とする直径が細く、高品質のカーボンナノチューブを製造することができる。 The gas phase reaction method carried out using the gas phase reaction apparatus of the present invention can be suitably used for the production of hollow carbon fibers. That is, a catalyst metal is supported on a carrier, and a gas phase reaction is performed by contacting the catalyst metal and a carbon-containing compound at a temperature of 500 ° C. to 1200 ° C., preferably 600 ° C. to 950 ° C. High-quality carbon nanotubes that are excellent in electrical conductivity, strength, and catalyst-supporting dispersibility, especially having a single-layer to three-layer main component, can be produced.
Claims (10)
前記反応室の上方に前記反応室に開閉可能なゲート扉で隔離された予備加熱室と、該予備加熱室に前記反応室の気相反応と平行して前記新たな被反応物を昇温処理する予備加熱手段とを設け、前記反応室の下方に前記装填・取出手段を配置し、前記装填・取出手段をシリンダー機構で構成し、該シリンダー機構の合計シリンダーストロークを前記反応室の上下方向の長さよりも長くし、さらに、前記シリンダー機構が、先端にワークを保持する直動部として、少なくとも中空構造の第１シャフトと該第１シャフトの内面に設けたシール部及びガイド部に摺接しながら往復移動する第２シャフトとを設けると共に、前記第１シャフトを往復駆動する第１シリンダーと前記第２シャフトを往復駆動する第２シリンダーとを設け、かつ前記第２シリンダーを該第２シリンダーの軸方向と直交する方向に往復移動させる駆動機構を設けたことを特徴とする気相反応装置。 The reaction chamber is provided with at least a reaction chamber heating means, a loading / unloading means for loading and unloading powdery or particulate reactants supported by a gripper, and a gas introducing means for introducing a reaction gas, A series of operations in which a reactant and a reaction gas undergo a gas phase reaction in the reaction chamber and a reaction product is taken out of the reaction chamber together with the gripper are repeated in a continuous batch while sequentially supplying new reactants. In the phase reactor,
A preheating chamber that is isolated by a gate door that can be opened and closed to the reaction chamber above the reaction chamber , and the preheating chamber is heated in parallel with the gas phase reaction in the reaction chamber. Preheating means, and the loading / unloading means is disposed below the reaction chamber, the loading / unloading means is constituted by a cylinder mechanism, and the total cylinder stroke of the cylinder mechanism is set in the vertical direction of the reaction chamber. The cylinder mechanism is slidably in contact with at least a first shaft having a hollow structure and a seal portion and a guide portion provided on the inner surface of the first shaft as a linear motion portion that holds a workpiece at the tip. A second shaft that reciprocates, a first cylinder that reciprocates the first shaft, and a second cylinder that reciprocates the second shaft, and the second series Gas phase reactor which characterized in that a drive mechanism for reciprocating in a direction orthogonal to loaders and axial of said second cylinder.
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| JP2007007736A JP4973208B2 (en) | 2006-03-29 | 2007-01-17 | Gas phase reactor |
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| WO2009128349A1 (en) * | 2008-04-16 | 2009-10-22 | 日本ゼオン株式会社 | Equipment and method for producing orientated carbon nano-tube aggregates |
| US9174847B2 (en) * | 2008-05-01 | 2015-11-03 | Honda Motor Co., Ltd. | Synthesis of high quality carbon single-walled nanotubes |
| JP5147556B2 (en) * | 2008-06-12 | 2013-02-20 | 日立造船株式会社 | Carbon nanotube production equipment |
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| JP5277511B2 (en) * | 2003-08-05 | 2013-08-28 | 東レ株式会社 | Gas phase reaction method and apparatus |
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