JP5782038B2 - 等温多管式反応器及び該反応器を組み込んだプロセス - Google Patents
等温多管式反応器及び該反応器を組み込んだプロセス Download PDFInfo
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Description
例1A(比較)
1インチ内径のHastelloy反応器を約450℃〜約480℃に加熱する。塩化メチル及びペルクロロエチレンの流れをそれぞれ約50ml/hr〜約150ml/hr、及び約180ml/hr〜約123ml/hrの液流で確立することにより、約10秒〜約23秒の滞留時間を達成する。
混合温度を325℃まで低下させた後、90%を上回る1,1,2,3−テトラクロロプロピレンへの選択率において少なくとも8%のペルクロロエチレン転化率で生成される、例1Aに基づく別の実験では、2インチの混合ゾーンを取り除き、そして反応器の供給ラインの入口から少なくとも6インチ離れた下流側に加熱ゾーンを動かす。この実験は、反応器への供給入口のすぐ後のゾーン内に副生成物及び炭素沈殿物が生成されるのを回避するための反応速度にとって325℃が十分に低い温度であることを示す。
下記のように所望の反応温度から少なくとも約20℃だけ逸脱した入口温度を用いる反応器を使用して、式:CH2-c-gClcFg=CH1-d-hCldFh−CH3-e-fCleFf(式中、cは0〜2であり、dは0〜1であり、eは0〜3であり、fは0〜3であり、そしてgは0〜2であるが、c+g≦2、d+h≦1、そしてe+f≦3である)を有する塩素化及び/又はフッ素化プロペンを調製する。約3000本のスケジュール40の内径1.5インチの60ft長の管をこの例において使用する。調製される所望の塩素化及び/又はフッ素化プロペンに依存する所望の供給材料を等温多管式反応器に提供する。入口の温度を制御し、且つ/又は供給材料の温度を制御することによって、所望の反応温度とは少なくとも約20℃だけ異なる温度で供給材料を提供する。375℃前後の反応温度近くに供給材料温度が上昇するのに伴って、選択率が低下することが予想される。
下記のように所望の反応温度から少なくとも約20℃だけ逸脱した入口温度を用いる反応器を使用して、式:CH2-c-gClcFg=CH1-d-hCldFh−CH3-e-fCleFf(式中、cは0〜2であり、dは0〜1であり、eは0〜3であり、fは0〜3であり、そしてgは0〜2であるが、c+g≦2、d+h≦1、そしてe+f≦3である)を有する塩素化及び/又はフッ素化プロペンを調製する。調製される所望の塩素化及び/又はフッ素化プロペンに依存する所望の供給材料を等温多管式反応器に提供する。入口の温度を制御し、且つ/又は供給材料の温度を制御することによって、所望の反応温度とは少なくとも約20℃だけ異なる温度で供給材料を提供する。
図2に示された反応器を使用して、下記表3に示された塩素化及び/又はフッ素化プロペンを調製する。より具体的には、式:CH4-a-bClaFbを有する供給材料を等温多管式反応器に提供することにより、式:CH2-c-gClcFg=CH1-d-hCldFh−CH3-e-fCleFf(式中、cは0〜2であり、dは0〜1であり、eは0〜3であり、fは0〜3であり、そしてgは0〜2であるが、c+g≦2、d+h≦1、そしてe+f≦3である)を有する塩素化及び/又はフッ素化プロペンを調製する。第1反応器ゾーン(図2の空間214)内で伝熱流体を使用して第1の所望の温度を維持し、そして第2反応器ゾーン内で同じか又は異なる伝熱流体を使用して第2の所望の温度を維持する。伝熱流体流は並流(CoC)又は向流(CC)であってよい。表に示すように、転化率%(%Conv)は著しく増大することはない。比較例において、反応器は1つのゾーンしか含まない。表3及び残りの表において、「Conv」は転化率を意味し、「Sel」は選択率を意味する。
それぞれ3500〜4500 SCCM、1400〜17000 SCCM、及び700〜980 SCCMの速度で、2インチ内径のInconel 600反応器に、塩化メチル、ペルクロロエチレン、及び四塩化炭素を供給することにより、260 psigにおいて約30〜40秒間の滞留時間を達成した。約410℃〜約420℃の反応器流出物を約10秒未満の滞留時間で約270℃〜約350℃の温度で冷却した後、約80℃未満の温度で内径0.5インチの冷却コイル内で凝縮する。約3.8%〜約5.0%の低いペルクロロエチレン転化率での1週間の実行時間後、反応器は冷却ゾーン内及び凝縮コイル内で重度に詰まることに起因する反応器出口の閉塞により停止させられる。冷却ゾーン及び凝縮コイルを液体急冷チャンバで置き換えることにより、2倍の限定試薬転化率で、2週間を上回る実行時間をもたらした。反応器を開いても、噴霧急冷チャンバ内に詰まりは見られない。
反応器に対して操作可能に配置されたコレクタ内でさもなければ発生し得る逆混合を低減するように改変された反応器を使用して、塩素化及び/又はフッ素化プロペンを調製する。より具体的には、式:CH4-a-bClaFbを有する供給材料を等温多管式反応器に提供することにより、式:CH2-c-gClcFg=CH1-d-hCldFh−CH3-e-fCleFf(式中、cは0〜2であり、dは0〜1であり、eは0〜3であり、fは0〜3であり、そしてgは0〜2であるが、c+g≦2、d+h≦1、そしてe+f≦3である)を有する塩素化及び/又はフッ素化プロペンを調製する。コレクタは、反応器と同じ直径/形状を有するように改変し、いくつかの態様では、表4に示された急冷を施す。
表5に示されているように、速度勾配層内部の反応成分流を最適化するように改変された反応器を使用して、塩素化及び/又はフッ素化プロペンを調製する。より具体的には、式:CH4-a-bClaFbを有する供給材料を等温多管式反応器に提供することにより、式:CH2-c-gClcFg=CH1-d-hCldFh−CH3-e-fCleFf(式中、cは0〜2であり、dは0〜1であり、eは0〜3であり、fは0〜3であり、そしてgは0〜2であるが、c+g≦2、d+h≦1、そしてe+f≦3である)を有する塩素化及び/又はフッ素化プロペンを調製する。反応器内の全ての管への供給材料の混合及び分配を改善するために供給材料分配器を改変することによって、同じ限定試薬転化レベルにおいて選択率を改善することが予想される。同様に、表面粗さを低減し、ひいては副生成物及び詰まりの発生が予想される低速度/層状ゾーンの境界層厚を小さくするように、反応器管壁を前処理又は被覆しても、より良好な選択率が期待される。
例1〜4に従って調製された塩素化及び/又はフッ素化プロペンから、当業者に知られているいくつかの方法のうちのいずれかによって、ヒドロフルオロオレフィンを調製する。例えば、クロム/コバルト系触媒とともにHFを使用して、1,1,2,3−テトラクロロプロペンをHFO−1234yfに転化することは、国際公開第2008/054781号パンフレットに記載された方法に従って行うことができる。国際公開第2009/003084号パンフレットには、1,1,2,3−テトラクロロプロペンの原料を液相中で触媒なしで、続いて触媒気相反応においてフッ素化することによって、2,3,3,3−テトラフルオロプロペン(HFO1234yf)を形成する多工程プロセスが記載されている。このプロセスも好適である。米国特許出願公開第2009/0030244号明細書には、HCFC−1233xfを中間体として、HFによる触媒プロセスを用いて、1,1,2,3−テトラクロロプロペンを使用してHFO1234yfを生成することが記載されている。このプロセスを用いてもよい。最後に米国特許出願公開第2009/0099396号明細書には、HFC−245ebを中間体として、1,1,2,3−テトラクロロプロペンをHVと好適に液相触媒反応させ、続いて気相反応させることが記載されている。これらの特許明細書のそれぞれは、あらゆる目的のためにその全体を参照することによって、ここに組み込まれる。
Claims (5)
- 塩素化及び/又はフッ素化アルカンと塩素化及び/又はフッ素化アルケンの反応から、塩素化及び/又はフッ素化されたプロペン及び炭素原子数3〜6のより高級なアルケンを製造するための連続気相フリーラジカル法で使用するのに適した、シェル内部に配置された複数の反応器管を含む等温多管式反応器であって、該反応器が入口を含み、入口温度が所望の反応温度よりも少なくとも20℃低くされ、そして少なくとも1つの反応器管の少なくとも一部は、少なくとも2100のレイノルズ数によって定義することができ、該反応器は、コレクターを含み、該コレクターは、該反応器からの反応器流出物を受容するように構成され、逆混合を最小化するようにさらに構成されている、等温多管式反応器。
- 該反応器が、副生成物生成を最小化する設計を含み、該反応器設計が、
i)該反応器への熱移動及び/又は該反応器からの熱移動を促進する設計;
ii)該反応器から出る時の逆混合の低減、及び/又は発生し得る逆混合中の副生成物形成の低減を促進する設計;
iii)該反応成分と、少なくとも1つの反応器管壁の少なくとも一部との間の境界のところでの反応成分流を最適化する設計;及び/又は
iv)反応器流出物の温度を、副生成物の実質的な形成が生じない温度未満に低下させるのを促進する設計
のうちの1つ又は2つ以上を含む、請求項1に記載の反応器。 - 該熱移動を促進する設計が、該反応器のシェル内部に、伝熱流体の並流を提供することを含む、請求項2に記載の反応器。
- 該熱移動を促進する設計が、異なる温度をそれぞれの区分内部で維持することができるように、少なくとも2つの区分に仕切られた該シェルを含む、請求項2に記載の反応器。
- 式:CH 4-a-b Cl a F b (式中、a及びbはそれぞれ独立して0〜3であり、そして4−a−bは0より大きい)を有するメタン、クロロメタン、フルオロメタン又はクロロフルオロメタンを含む供給材料を、等温多管式反応器に提供することを含み、該反応器が入口を含み、入口温度が所望の反応温度よりも少なくとも20℃低くされ、そして少なくとも1つの反応器管の少なくとも一部は、少なくとも2100のレイノルズ数によって定義することができ、該反応器は、コレクターを含み、該コレクターは、該反応器からの反応器流出物を受容するように構成され、逆混合を最小化するようにさらに構成されている、式:CH2-c-gClcFg=CH1-d-hCldFh−CH3-e-fCleFf(式中、cは0〜2であり、dは0〜1であり、eは0〜3であり、fは0〜3であり、そしてgは0〜2であるが、c+g≦2、d+h≦1、そしてe+f≦3である)を有する塩素化及び/又はフッ素化プロペンを製造する方法。
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Application Number | Priority Date | Filing Date | Title |
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US25003009P | 2009-10-09 | 2009-10-09 | |
US61/250,030 | 2009-10-09 | ||
PCT/US2010/052073 WO2011044514A2 (en) | 2009-10-09 | 2010-10-08 | Isothermal multitube reactors and processes incorporating the same |
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JP2013507393A JP2013507393A (ja) | 2013-03-04 |
JP2013507393A5 JP2013507393A5 (ja) | 2013-11-21 |
JP5782038B2 true JP5782038B2 (ja) | 2015-09-24 |
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US20110087054A1 (en) | 2011-04-14 |
WO2011044514A3 (en) | 2011-08-04 |
EP2485832B1 (en) | 2016-11-23 |
BR112012007914A2 (pt) | 2019-09-24 |
CN102596387B (zh) | 2015-11-25 |
EP2485832A2 (en) | 2012-08-15 |
CN102596387A (zh) | 2012-07-18 |
US8926918B2 (en) | 2015-01-06 |
US20140010741A1 (en) | 2014-01-09 |
US8558041B2 (en) | 2013-10-15 |
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