JP4424991B2 - ホスゲンを製造するための反応器およびホスゲンの製造方法 - Google Patents
ホスゲンを製造するための反応器およびホスゲンの製造方法 Download PDFInfo
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Description
図1は、反応混合物と熱移動媒体を交差向流とした本発明による反応器の第1の実施の形態における縦断面を示し、
図2は、本発明による反応器に別の実施の形態における縦断面を示し、反応混合物と熱移動媒体が交差並流で運ばれ、そして反応混合物が入る領域において触媒管に不活性材料が充填され、
図3は、図1または図2に示されている本発明の反応器におけるA−A面の断面を示し、
図4は、図3の横断面の一部を示し、
図5〜図7は、それぞれ図1または図2における縦断面の一部を示し、
図8は、2領域反応器の好ましい実施の形態を示し、
図9は、図8の反応器の細部を示し、
図10は、3領域反応器の好ましい実施の形態を示し、
図11は、2基の反応器を相互に上方に直接配置し、両方の反応器で熱移動媒体の偏向領域に配管を有していない場合の好ましい実施の形態を示し、
図12は、2基の反応器の相互に上方に直接配置し、2番目の反応器が全ての場所で配管を有している場合の他の好ましい実施の形態を示し、
図13は、2基の反応器を直列に連結した装置を示し、そして
図14は、耐熱対を収納するのに用いられる覆いを備えた図13の一部を示している。
7087kg/h(時)の塩素および2913kg/hの一酸化炭素を、1256本の触媒管(各々、配管の長さ3000mm、配管の内径39.3mmおよび壁部の厚さ2.6mm)を有する円筒形の多管式反応器の触媒管に通過させ、これらの触媒管に、反応混合物が供給される領域で200mmの長さまでに不活性のセラミック材料が充填され、次いで、2700mmの長さまでに、活性炭を備え、4mmの円筒状触媒粒径と5mmの長さおよび多孔率0.404を有する円筒形触媒からなる触媒床が、反応ガスの吸気圧の条件下、即ち反応器の上流側の反応ガスの圧力が4バールの絶対圧の条件下で充填されて、約10000kg/hのホスゲンの生成物流を得た。
Claims (22)
- 1基以上の円筒形の反応器(1)において固体触媒の存在下で一酸化炭素と塩素の気相反応によってホスゲンを製造する方法であって、
反応器の長手方向に平行に並設され、末端部が管状プレート(3)に固定されている触媒管(2)の束と、
反応器(1)の各末端部にキャップ(4)と、
触媒管(2)の間の中間空間(5)に反応器の長手方向に対して垂直に並設され、反応器の内壁で相互に対向して交互に配置される通路(7)を開放状態とする偏向板(6)と、を有し、
触媒管(2)に固体触媒が充填され、
気体の反応混合物が一方のキャップ(4)を介して反応器の一端側から触媒管(2)を通って流れ、そして反応器(1)の反対側の末端部から第2のキャップ(4)を介して取り出され、
液体の熱移動媒体が触媒管(2)の周囲の中間空間(5)を通って通過し、且つ、
当該方法の行われる1基以上の反応器が通路(7)の領域に配管を有していないことを特徴とするホスゲンの製造方法。 - 偏向板(6)は管状部として形成され、全ての偏向板(6)は、それぞれ同寸法通路(7)を開放し、各通路(7)の面積は反応器の断面積に対して5〜20%である請求項1に記載の方法。
- 100〜10000本の触媒管(2)が含まれ、各々の触媒管(2)は、1.5〜6.0mの範囲の長さ、2.0〜4.0mmの範囲の壁厚、20〜90mmの範囲の内径を有している請求項1又は2に記載の方法。
- 触媒管(2)と偏向板(6)の間に0.1〜0.6mmの範囲の間隙(8)が設けられ、偏向板(6)が通路(7)の領域を除いて反応器の内壁に液密形態で固定される請求項1〜3のいずれか1項に記載の方法。
- 偏向板の厚さは8〜30mmの範囲である請求項1〜4のいずれか1項に記載の方法。
- 管状プレート(3)に通気孔及び/又は排出孔(9)が設けられ、補正機(10)が反応器の壁部に設けられ、そして出入口又は一部環状の溝(11)が熱移動媒体を導入及び排出するために反応器の壁部に設けられ、該出入口又は一部環状の溝(11)の反応器の内部へ向けた開口部は、円形または矩形の断面を有し、5〜50%の範囲の開口割合を有している請求項1〜5のいずれか1項に記載の方法。
- 反応器は、該反応器の中段の横断面に対して対称に構成されている請求項1〜6のいずれか1項に記載の方法。
- 反応器(1)は複数の領域を有し、個々の領域を分割板(14)によって液密形態で相互に分離して、熱移動媒体が反応器(1)内で所定の領域からその他の領域に流れないようにしたことを特徴とする請求項1〜7のいずれか1項に記載の方法。
- 2箇所以上の温度計測部を備えるマルチ熱電対(18)を収納し、反応器(1)より下方に開口する覆い(17)が1本以上の触媒管(2)に設けられている請求項1〜8のいずれか1項に記載の方法。
- 直列に連結された2基以上の反応器(1)で行われ、塩素残留量の濃度計測部(19)及び/又は温度計測部(20)を設けたことを特徴とする請求項1〜9のいずれか1項に記載の方法。
- 塩素残留量の濃度計測部(19)及び/又は温度計測部(20)は、上流側の反応器の下側キャップと下流側の反応器の上側キャップとの間の連結部材に設けられている請求項10に記載の方法。
- 直列に連結された2基以上の反応器(1)で行われる請求項1〜10のいずれか1項に記載の方法であって、2番目の反応器の触媒管(2)は、最初の反応器(1)と比較して大きな内径の配管であり、20〜110mmの範囲の内径を有し、反応器(1)は、これらの間にキャップ(4)を配設することなく直列に直接連結され、そしてスペーサー(16)が各反応器(1)の間に設けられていることを特徴とする方法。
- 2番目の反応器(1)及び/又はさらに他の反応器(1)は上流側の反応器(1)より小さな外部寸法を有している請求項10〜12のいずれか1項に記載の方法。
- 反応器(1)を安全チャンバーで包囲する請求項1〜13のいずれか1項に記載の方法。
- 熱移動媒体として、水、水酸化ナトリウム水溶液又は1種以上の炭化水素を使用し、気体の反応混合物及び液体の熱移動媒体を交差向流又は交差並流で反応器(1)に通過させる請求項1〜14のいずれか1項に記載の方法。
- 一酸化炭素と塩素を1.01〜1.10の範囲のモル割合で上側から又は下側から触媒管(2)を通って通過し、そして反応器(1)の長手方向軸は鉛直方向にある請求項1〜15のいずれか1項に記載の方法。
- 触媒管(2)に配置される固体触媒は、球、円錐、円筒、押出物、リング又はペレットの形の活性炭又は少なくとも部分的に開放気孔を有する炭素フォームであり、触媒管(2)の、気体の反応混合物が供給される末端部の領域に、該触媒管(2)の全長に対して5〜20%の長さに不活性材料が充填されている請求項1〜16のいずれか1項に記載の方法。
- 触媒管(2)は、熱移動媒体側で500〜2000W/m2/Kの範囲の熱移動係数を有している請求項1〜17のいずれか1項に記載の方法。
- 固体触媒の存在下で一酸化炭素と塩素の気相反応によってホスゲンを製造するのに用いられる円筒形の反応器(1)であって、
該反応器は、
反応器の長手方向に平行に並設され、末端部が管状プレート(3)に固定されている触媒管(2)の束と、
反応器(1)の各末端部にキャップ(4)と、
触媒管(2)の間の中間空間(5)に反応器の長手方向に対して垂直に並設され、反応器の内壁で相互に対向して交互に配置される通路(7)を開放状態とする偏向板(6)と、を有し、
通路(7)の領域に配管を有しておらず、
触媒管(2)に固体触媒が充填され、
気体の反応混合物が一方のキャップ(4)を介して反応器の一端側から触媒管(2)を通って通過し、そして反応器(1)の反対側の末端部から他方のキャップ(4)を介して取り出され、
液体の熱移動媒体が触媒管(2)の周囲の中間空間(5)を通って通過し、且つ、
最下部の偏向板(6)と最上部の偏向板(6)は、連続する偏向板(6)の間の距離と比較してそれぞれ管状プレート(3)からなおいっそう離されており、触媒管(2)と偏向板(6)の間に0.1〜0.6mmの範囲の間隙(8)が設けられ、そして触媒管(2)がステンレススチール又は2相スチールから作製されていることを特徴とする反応器(1)。 - 最下部の偏向板(6)と最上部の偏向板(6)は、二枚の連続する偏向板(6)の間の距離と比較して、それぞれの管状プレート(3)から1.5倍離れている請求項19に記載の反応器(1)。
- 偏向板(6)は管状部として形成され、全ての偏向板(6)は、同寸法通路(7)を開放し、各通路(7)の面積は反応器の断面積に対して5〜20%であり、触媒管(2)と偏向板(6)との間に0.2〜0.3mmの範囲の間隙(8)が設けられている請求項19又は20に記載の反応器(1)。
- 100〜10000本の触媒管(2)を有し、各々の触媒管(2)は、1.5〜6.0mの範囲の長さ、2.0〜4.0mmの範囲の壁厚、20〜90mmの範囲の内径を有している請求項19〜21のいずれか1項に記載の反応器(1)。
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KR20040087326A (ko) | 2004-10-13 |
ATE309856T1 (de) | 2005-12-15 |
KR100936420B1 (ko) | 2010-01-12 |
US8409539B2 (en) | 2013-04-02 |
ES2253661T3 (es) | 2006-06-01 |
EP1485195B1 (de) | 2005-11-16 |
AU2003208834A1 (en) | 2003-09-09 |
BR0307973A (pt) | 2004-12-21 |
CN1302842C (zh) | 2007-03-07 |
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EP1485195A1 (de) | 2004-12-15 |
DE50301676D1 (de) | 2005-12-22 |
CN1638856A (zh) | 2005-07-13 |
US20050118088A1 (en) | 2005-06-02 |
JP2005525986A (ja) | 2005-09-02 |
US20130072717A1 (en) | 2013-03-21 |
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US8821829B2 (en) | 2014-09-02 |
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