JP4787856B2 - 積層物に基づく管型反応器 - Google Patents
積層物に基づく管型反応器 Download PDFInfo
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- JP4787856B2 JP4787856B2 JP2008071188A JP2008071188A JP4787856B2 JP 4787856 B2 JP4787856 B2 JP 4787856B2 JP 2008071188 A JP2008071188 A JP 2008071188A JP 2008071188 A JP2008071188 A JP 2008071188A JP 4787856 B2 JP4787856 B2 JP 4787856B2
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2882—Catalytic reactors combined or associated with other devices, e.g. exhaust silencers or other exhaust purification devices
- F01N3/2889—Catalytic reactors combined or associated with other devices, e.g. exhaust silencers or other exhaust purification devices with heat exchangers in a single housing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/88—Handling or mounting catalysts
- B01D53/885—Devices in general for catalytic purification of waste gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
- B01F25/421—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions by moving the components in a convoluted or labyrinthine path
- B01F25/422—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions by moving the components in a convoluted or labyrinthine path between stacked plates, e.g. grooved or perforated plates
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- B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
- B01F25/432—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction with means for dividing the material flow into separate sub-flows and for repositioning and recombining these sub-flows; Cross-mixing, e.g. conducting the outer layer of the material nearer to the axis of the tube or vice-versa
- B01F25/4321—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction with means for dividing the material flow into separate sub-flows and for repositioning and recombining these sub-flows; Cross-mixing, e.g. conducting the outer layer of the material nearer to the axis of the tube or vice-versa the subflows consisting of at least two flat layers which are recombined, e.g. using means having restriction or expansion zones
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
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Description
円形横断面に関し、かつ:
図1aは、積層物に基づく管型反応器の主な構造の側面図を示したものであり、その際、構造化された層1、2、3および被覆層4、5は、部分的に切り取られた形で示されている。区分で示された積層物の完全な輪郭は、補助的な破線で示されている。
図3aは、それぞれ孔33(図3e)を有する管型反応器のための2個の重なった層を示し、この場合、これは、並んで配列され、かつその横軸31の方向に伸ばされ、かつ幅31と高さ(32)との幾何学的比が1より大きい。断面的形状33は、スロット(図3e)の断面形と一致し、その際、孔は流れの方向に対して角度αに傾斜している。たとえば、2個の層中の同様の孔33、34の3個の交差領域34’がみられる。管型反応器は、最下部層と同一の少なくとも1個の他の層およびさらには2個の被覆層で提供される。
図4aは、管型反応器のためのハウジング40を示し、この場合、これは、同軸の温度調節ジャケット41および供給管路42、ならびに熱伝達媒体のための排出管路43を有している。ハウジングは、付加的に、閉鎖されたヘッド44および装入口46および排出口47を有する他のヘッド45を有している。ヘッドは、スクリュー(示されていない)によってハウジング40と連結する。ハウジング40は、その中心に2個の中空領域を有し、その中に、2個の層の構造化されたパケット48、49が挿入されている。層の2個のパケット48、49は、ハウジングの一部であり、かつ挿入された構造化された層のパケット自体よりも短い、中心の隔壁40’によって互いに分離されており、したがって、材料を逐次、積層物中に流すことが可能である。隔壁40’は、層の隣接するパケット48、49のための共用の被覆層を形成する。層のパケット48、49は、図1aで示されたのと同様の方法でかつ互いにハンダ付けされた、互いに上に重ねられた9個の構造化された金属シートから成っている。反応のための開始材料は、装入口46で装入され、パケット49の流路中を流れ、ギャップを介してパケット48中に流れ、この中を移動して、排出口47で反応器から排出される。
図5は積層物に基づく管型反応器を示し、この場合、これは同様にハウジング50に挿入されていてもよく、この場合、これは、ヘッド51で封鎖されている。ハウジングは、装入口52を有し、これを通して液体材料または気体材料が流れ、かつ層53のパケットに入ってもよい。層のパケット53からの生成物排出口は、ヘッド51を介して排出口54に開放されている。層のパケットは12個の金属シートを含有し、この場合、これは、図1で示された金属シートと同様に構造化され、かつ二者択一的な配置において互いにハンダ付けされている。示された態様において、積層物から成る層のパケットは、双方の側において、有孔の被覆層55を有し、この場合、変法においては膜であってもよく、かつこれを介して他の液状成分または気体成分は積層物中を流れる流に装入されてもよい。気体成分または液体成分は、供給管路56、57を介して、分配チャンバー58、59に提供され、その結果、その後に有孔の層中を通過し、かつ層のパケットの外側の層の孔を介して、その長さに亘って均一に流れ、かつ積層物の流路中に流れる。
図6aは、おおよそ同軸の断面を有する管型反応器を形成するための構造化された層の構造を示す。孔603の平行な並びを有する2個の構造化された層601、602は、図6a中でみることができる。層は、ステンレス鋼シートから成り、かつ極めて薄い(0.2mm)ので容易に巻き上げることができる。孔の平行な並びは、区分604を包含し、この場合、これは、多重の円形の周縁に相当する。孔の平行な並びは、側面に延伸した非構造化領域605と隣接する。2個の重なった層は、同一形状の金属シートから成り、この場合、これは、互いに180℃回転しているものであり、したがって、1個の層の孔の並びは、隣接する層の孔と交差している。
606が存在し、この周囲で、孔603の平行な並びを有する構造化された層601、602はスパイラル状にきつく巻き上げられ、別個の層601、602のスパイラル状に巻かれた非構造化領域(被覆層605)によって順に包囲された、同軸の流れ断面を形成する。非構造化層の末端は、それ自体を外周で、たとえば、図6dに示されたようにして溶接する。
図7bは同一の構造を有する2個の重なり合った層(金属シート)700、701を示す。しかしながら、層は、その幅で、重複する周縁によって伸長され、したがって、伸長において有孔の孔領域703は、孔702の平行な並びと隣接する。これは、完全な開口領域704と隣接し、かつ他の伸長では非構造化層領域705がある。この層は、たとえば、ホイルまたは金属シートが、異なる課題の要求を満たすために、種々に構造化されてよいことを示す。
例8は、積層物80に基づく長い管型反応器を示し、その中で孔の並び81は、蛇行した形(ループ状)で、大きい領域の金属シート中に配置される。複数個の同一の構造化された金属シート82、83は、互いに上部に配置され、それぞれの場合において180℃回転し、その結果、並び中の孔は交差し、かつ孔間のウェブは放射線状の流れを補助する程度の角度である。長い流路は、一定の流れ断面および供給開口84および排出開口85を有する。積層物は、被覆層を有するが、しかしながら、図8中には示されていない。
図9aにおいて、流路系90は、3個の分離した流路91、92、93を有する積層物に基づき、この場合、これは、異なる流れ断面積を有し、かつ並び中の孔の異なる輪郭が示された。3個の分離した流路は、供給される別個の成分が、これらが共通の集合流路94(入口95)に導かれる前に、たとえば、別個に加熱/冷却することを可能にする。集合流路94は、反応のために特別に構築されてもよい。流路系90は、反応が、増加した温度で、反応に対して影響をもつことのない独立した加熱可能な供給流路中で、関与する反応成分の加熱層を用いて、開始することを可能にする。
図10は、2個の管型反応器を含有する反応系を示し、この場合、これは、それぞれ9個の構造化された層を有する層101、102の2個のパケットを一続きに連結する。層101、102の2個のパケットは、図1aで示された例と同様の方法で、流れの主方向に対して角度αで傾斜した延びた孔103の並びで提供されている。2個の積層物は、互いに角度β=90゜で回転されている。層101、102のパケットは、ハウジング中に押し込まれ(示されていない)、この場合、これは、層のパケットのための被覆層を形成し、かつプロセス材料の装入および排出を提供する。
管型反応器中の化学反応
化学反応は、連続的にミニチュア化された試験装置中でおこなわれ、この場合、これは、積層物に基づく熱交換器および管型反応器が使用される。反応は、望ましくない副生成物が形成されることのない短い反応時間後に、完了すべきである。酸化剤として、ジメチルジオキシラン(DMSO)を用いての、有機スルフィドフェニルチオアセトニトリルの相当するスルホキシドへの均質な液相酸化が試験された。通常のバッチ反応の主な問題は、逆混合後の過酸化によって、最初に生じたスルホキシドから、著量のスルホン副生成物が形成されることである。さらに、DMSOが、保存することができず、かつ酸化反応での使用直前に製造しなければならない不安定な酸化剤であることに注意すべきである。
C6H5−S−CH2−CN+CH3−CO2−CH3→C6H5−SO−CH2−CN+CH3−CO−CH3
ミニチュア化された管型反応器に、1,2−ジクロロエタン(0.1N溶液)で150mlにされたフェニルチオアセトニトリル 2.25gの供給物を供給し、受け器中で20℃で放置した。新たに製造されたアセトン中のジメチルジオキシラン 0.1N溶液を、第2供給容器中で同様に20℃に置いた。スルフィドを、ダブルピストンポンプ(流量=1.0ml/分)を用いて管型反応器(40℃に予め加熱した)に汲み上げた。予加熱を、層のプラグ−イン パケットに基づく熱交換器中で実施した。熱交換器は、図4で示された加熱可能/冷却可能なジャケットを有する管型ハウジングを含むが、しかしながら、層の一つのみのパケットおよび管型ハウジングの下部末端での排出口を備えていた。ハウジング軸に沿ってその中心で、管型ハウジングは、6x6mmの長方形の孔のみを有しており、その際、厚い層(鋼シート)30x0.2mmから成る層(48)の構造化されたパケットを取り付けた。別個の層は、幅6mmおよび長さ99mmを有していた。層中の孔(図3)の長軸31は、流れの主な方向に対して45゜の角度αであった。孔(図3e)の幾何学的直径は、長さ31=約5.4mm、幅32=0.81mmおよびウェブ幅=0.25mmであり、したがって、66個の孔の並びを形成する。
一連の試験において、積層物に基づく管型反応器の熱交換性能を、比較可能な通常の管型熱交換器と比較する(リービッヒ管)。
積層物に基づく管型反応器(図1と同様のもの)は、積層パケット上で溶接された2個の0.5mmの厚さの被覆層4、5によって覆われた積層パケット1、2、3から成る99mmの長さの流路を含有する。積層物のパケットは、20x0.1mmの厚さの層から成る(鋼シート)。個々の層は幅6mmおよび長さ99mmを有していた。層中の孔6の長軸は、流れの主な方向に対して45゜の角度αであった。孔の幾何学的寸法(図3e)は長さ31=約5.4mm、幅32=0.81mmおよびウェブ幅=0.25mmであり、したがって、66個の孔の並びが形成された。層のパケットは流路断面比W/H約1.9を有していた。記載された流路は、Φ12x1.5mm、外径12mm、壁厚1.5mmの管40中に、図4aで示されたのと同様の方法で入れられ、かつ熱伝導媒体のための接続部42、43を備えていた。
双方の装置を、同一条件下で試験した。約20〜25℃の温度を有する液体流を、一定の流速で(水の場合には0.4m/sおよびグリセロールの場合には0.1m/s)で通過させ、かつジャケット中に向流で熱水(60℃および90℃)を通すことによって加熱した。
性能は、熱伝導効率平均(k値)を用いることで最も適切に比較することができる。性能中で観察された改善の一部分は、W/H比 1.9を有する流路断面を平坦化することに帰因していてもよいが、しかしながら、主要な部分は、積層の混合作用によるものである。最初に、エネルギーは、より効率的に液体容量中に装入されるが、それというのも、金属積層物の良好な熱伝導のためであり、第2には、積層物の混合構造は強制対流を生じ、したがって、改善された熱伝達性が生じるためである。
試験において、まさに図10aで示されたのと同様の形式で組み立てられた層のパケットに基づく管型反応器中で、層流の場合の混合作用を、従来の熱交換器と比較する。この目的のために、20個の有孔の層(スチール鋼)を含む約100mmの長さの管型反応器を、透明なポリカーボネートハウジング中に取り付けた。層中での孔は、図3eで示されたような幾何学的形状を有し、かつ同一の大きさを有する。選択された大きさは:長さ=5mm、幅=0.8mmおよび孔間のウェブ幅=0.25mmであった。
管型反応器の混合の課題としては、異なる流量を有する2個の流が均一に混合されることである。選択された物質は、10Pa・sの粘度を有するシリコンオイルである。第1流は透明であり、かつ第2流は透明なプラスチックケーシング中で、積層物の混合性能が可視的に評価できる程度に黒色に染色されている。全ての物質流量は、約1.4g/分であり、かつ約3.2バールの圧力低下が立証された。
特許出願 WO98/55812中に記載された熱交換器は、層の平面上での混合作用がみられず、かつ積層の方向中でのわずかな混合作用のみがみられた。これによって、独立した流路間に横方向に連結される流路が存在するといった事実にもかかわらず、平行な孔を有する有孔の層が4個の独立した流路を形成し、かつ、個々の流路は交差混合(cross mixing)を示すことがないことが明らかであった。
従来の熱交換器(WO98/55812)と比較して、単一流路の流れは、本発明の管型反応器中で達成された。異なる流および異なる密度および粘度を有する流の場合においては、分配の問題が生じることなく、通常は迅速および良好な混合が生じ、この場合、これは、反応器の効率および機能を著しく改善し、特に、物質移動を著しく改善させる。
Claims (7)
- コアチューブまたはロッド(606)の周囲に巻かれた少なくとも2個の構造化された層(601、602)を含む積層物に基づく管型反応器において、それぞれの層(601、602)が、コアチューブまたはロッドの方向に沿って一つまたはそれ以上の並びで配置されかつ延びた複数個の孔(603,603’)を有し、かつ被覆層(605)が、積層物の外周上に配置され、かつその層(601)の孔(603)は、隣接する層(602)の孔(603’)と交差し、その際、一連の交差する孔が、コアチューブまたはロッド(606)の方向に沿って流路を形成することを特徴とする、積層物に基づく管型反応器。
- 少なくとも部分的に有孔の被覆層(703)、および被覆層(703)を包囲しかつ装入口(707)を有するほぼ同軸の分配チャンバー(704)を有する、請求項1に記載の管型反応器。
- 反応器の内部表面が触媒性被膜を有するか、または構造化された層が触媒材料から成る、請求項1または2に記載の管型反応器。
- 化学反応を実施するための、請求項1から3までのいずれか1項に記載の反応器の使用。
- 熱的分離工程におけるカラム充填物としての、請求項1または2に記載の反応器の使用。
- 排気ガス浄化のための、請求項3に記載の反応器の使用。
- 自動車の排気ガス浄化のための、請求項6に記載の反応器の使用。
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JP5704786B2 (ja) * | 2004-11-16 | 2015-04-22 | ヴェロシス,インク. | マイクロチャネル技術を用いる多相反応プロセス |
EP1890802A2 (en) * | 2005-05-25 | 2008-02-27 | Velocys, Inc. | Support for use in microchannel processing |
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DE3643750A1 (de) * | 1986-12-20 | 1988-06-30 | Hoechst Ag | Waermetauschermodul aus gebranntem keramischen material |
GB8910241D0 (en) * | 1989-05-04 | 1989-06-21 | Secretary Trade Ind Brit | Heat exchangers |
US5114582A (en) * | 1991-04-12 | 1992-05-19 | W. R. Grace & Co.-Conn. | Filter element and spiral-wound membrane cartridge containing same |
US5193661A (en) * | 1992-02-05 | 1993-03-16 | Foster Raymond K | System of linear hydraulic motors |
FR2701554B1 (fr) * | 1993-02-12 | 1995-05-12 | Transcal | Echangeur de chaleur pour composants électroniques et appareillages électro-techniques. |
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US6167952B1 (en) * | 1998-03-03 | 2001-01-02 | Hamilton Sundstrand Corporation | Cooling apparatus and method of assembling same |
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DE20007356U1 (de) * | 1999-04-20 | 2000-08-10 | Mannesmann Ag | Reaktor zum Herstellen eines Brennstoffs, insbesondere von Wasserstoff |
US6746651B1 (en) * | 1999-08-10 | 2004-06-08 | Aerojet-General Corporation | Axial flow catalyst pack |
FR2809483B1 (fr) * | 2000-05-26 | 2003-08-15 | Spirec | Perfectionnements aux echangeurs thermiques de type spirale |
CA2314545A1 (fr) * | 2000-07-13 | 2002-01-13 | Jacek Mlynarek | Massif oriente de filtration et de biofiltration |
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2001
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2002
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- 2002-07-31 US US10/209,351 patent/US20030103879A1/en not_active Abandoned
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CA2396664A1 (en) | 2003-02-08 |
EP1284159A2 (de) | 2003-02-19 |
DE10138970A1 (de) | 2003-02-20 |
US20030103879A1 (en) | 2003-06-05 |
JP4386621B2 (ja) | 2009-12-16 |
CA2396664C (en) | 2010-12-14 |
JP2003159527A (ja) | 2003-06-03 |
EP1284159A3 (de) | 2004-10-20 |
JP2008149323A (ja) | 2008-07-03 |
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