JP5627837B2 - マイクロチャネル技術を用いる蒸留プロセス - Google Patents
マイクロチャネル技術を用いる蒸留プロセス Download PDFInfo
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- F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
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- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04624—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using integrated mass and heat exchange, so-called non-adiabatic rectification, e.g. dephlegmator, reflux exchanger
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- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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- F25J3/04975—Construction and layout of air fractionation equipments, e.g. valves, machines adapted for special use of the air fractionation unit, e.g. transportable devices by truck or small scale use
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- F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
- F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
- F25J5/007—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger combined with mass exchange, i.e. in a so-called dephlegmator
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Description
マイクロチャネル蒸留ユニットのそれぞれを通して蒸気相をマイクロチャネル蒸留ユニットのそれぞれの留出分端の方へ流すこと、
マイクロチャネル蒸留ユニットのそれぞれを通して液体相をマイクロチャネル蒸留ユニットのそれぞれのボトム分端の方へ流すこと、
マイクロチャネル蒸留ユニットのそれぞれの原料入口を通して流体混合物をマイクロチャネル蒸留ユニットのそれぞれの中の少なくとも一つのマイクロチャネル蒸留区画の中に流れ込ませることであって、高揮発性成分の一部を流体混合物から蒸気相へ移動させて高揮発性成分が濃縮された蒸気相を形成させ、低揮発性成分の一部を流体混合物から液体相へ移動させて低揮発性成分が濃縮された液体相を形成させること、
各マイクロチャネル蒸留ユニットの中の複数のマイクロチャネル蒸留区画を通して高揮発性成分が濃縮された蒸気相を各マイクロチャネル蒸留ユニットの流出分端の方へ流すことであって、高揮発性成分が濃縮された蒸気相を各マイクロチャネル蒸留区画の中で液体相と接触させ、高揮発性成分を濃縮させること、
各マイクロチャネル蒸留ユニットの中の複数のマイクロチャネル蒸留区画を通して低揮発性成分が濃縮された液体相を各マイクロチャネル蒸留ユニットのボトム分端の方へ流すことであって、低揮発性成分が濃縮された液体相を各マイクロチャネル蒸留区画の中で蒸気相と接触させ、低揮発性成分を濃縮させること
を含む。
マイクロチャネル蒸留ユニットを通して蒸気相をマイクロチャネル蒸留ユニットの留出分端の方へ流すこと、
マイクロチャネル蒸留ユニットを通して液体相をマイクロチャネル蒸留ユニットのボトム分端の方へ流すこと、
マイクロチャネル蒸留ユニットへの原料入口を通して流体混合物をマイクロチャネル蒸留ユニット内の少なくとも一つのマイクロチャネル蒸留区画の中に流れ込ませることであって、高揮発性成分の一部を流体混合物から蒸気相へ移動させて高揮発性成分が濃縮された蒸気相を形成させ、低揮発性成分の一部を流体混合物から液体相へ移動させて低揮発性成分が濃縮された液体相を形成させること、
マイクロチャネル蒸留ユニットの中の複数のマイクロチャネル蒸留区画を通して高揮発性成分が濃縮された蒸気相をマイクロチャネル蒸留ユニットの留出分端の方へ流すことであって、高揮発性成分が濃縮された蒸気相を各マイクロチャネル蒸留区画の中で液体相と接触させ、高揮発性成分を濃縮させること、
マイクロチャネル蒸留ユニットの中の複数のマイクロチャネル蒸留区画を通して低揮発性成分が濃縮された液体相を各マイクロチャネル蒸留ユニットのボトム分端の方へ流すことであって、低揮発性成分が濃縮された蒸気液体相を各マイクロチャネル蒸留区画の中で蒸気相と接触させ、低揮発性成分を濃縮させること
を含む。
試験1
試験2
BPR=背圧調整器
BV=ボールバルブ
KOポット=ノックアウトポット(キャッチコンテナ)
PG=圧力計
PRV=圧力リリーフバルブ
PT=圧力トランスジューサ
RTD=抵抗温度検出器
HXER=熱交換器
TC=熱電対
(1)チラーのスイッチを5℃に入れ、蒸気側の二重管式Hxerの中に送液させる。
(2)KOポットを両方ともデバイスの下に配置する。これらは、製品を回収するために用いられる。
(3)バルブ類を正しい位置にセットしてすべての原料ラインから空気をパージし、室温でシステムへの液体の流れを開始させる。
(4)製品流れ 蒸気および液体出口の計量バルブおよびBPRを開き、KOドレインラインのボールバルブを閉める。
(5)液体側原料
(a)シリンジポンプの電源を1.5ml/分で入れ、液体原料のための液体原料流量計を監視する。液体流れが安定したらシリンジポンプの電源を切り、三方ボールバルブを他のシリンジポンプ側へ切り替え、シリンジポンプによってシステムへの液体流れを1.5ml/分で開始する。
(b)空気がデバイス上流および下流の液体用の配管からパージされ、液体原料流量計のところで液体しか見えなくなったら、液体側の流速を運転計画書に指定の流速に低下させる。
(c)液体製品流量計を監視する。
(6)蒸気側原料
(a)シリンジポンプの電源を1.5ml/分で入れ、液体流れ用の蒸気原料流量計を監視する。液体流れが安定したらシリンジポンプの電源を切り、三方ボールバルブを他のシリンジポンプ側へ切り替え、このシリンジポンプによってシステムへの液体流れを1.5ml/分で開始させる。デバイスの頂部から流れを取り出してシステムからすべての空気を取り除き、デバイスの内部を完全に濡らす。
(b)システムの空気/窒素をパージするために、計量バルブを閉じ、圧力を5psigに増加させ、両方の計量バルブを同時に開く。ロータメータのところで泡が見えたら、プロセスを繰り返す。蒸気側のチューブ・イン・チューブHxerと計量バルブとの間の気泡トラップ配管もチェックする。キャップを開き、液体で配管の少なくとも半ばまで満たさせる。空気/窒素が蒸気外部ロータメータと干渉しないように、シリンジを用いて空気/窒素の一部を抜き出してもよい。
(c)空気がこのラインからパージされ、蒸気原料流量計のところで液体しか見えなくなったら、蒸気側流量を運転計画書に指定の流量に低下させる。製品流量計でそれぞれ予想される液体流れを監視する。製品流速が補正を要するなら、下流の計量バルブを然るべく調節する。BPRを運転計画書に指定の値より−0.5psig低く調節し、液体側KOポットの位置を調節して、BPRの下流のテフロン(登録商標)管で見られる両方の製品ラインで平衡液体相流れを実現する。セラミックヒータを設定して運転計画書に指定の温度に加熱する。ボトムセラミックヒータは、塔頂セラミックヒータより高い設定温度を有してもよい。加熱テープを用いて蒸気および液体供給ラインを≦5℃/分で加熱し始め、運転条件に近づくにつれて加熱速度を確実に遅くする。
(d)飽和条件を実現するように、所定の所望の圧力で、デバイスの中への液体原料温度および蒸気原料温度の熱し過ぎまたは加熱不足をそれぞれできるだけ少なくする。すべての熱源を必要に応じて調節し、運転計画書条件を実現する。計量バルブおよびBPRも必要に応じて調節し、製品ラインの中の所望の動作圧力および単一相製品(すなわち蒸気側では蒸気相、液体側では液体相)を維持する。入口および出口の両方での単一相流れをチェックするために、デバイスの上流および下流でいくつかの絶縁体を瞬間的に引き上げ、液体および蒸気側の透明プラスチック配管をともに検査する。セラミックヒータ温度は、入口温度を超えないようにする。
(7)システムが安定(すなわち、10分間にわたって、入口、出口および装置表面温度で<0.5℃の揺らぎ、4つの流量計すべてで<±0.1ml/分、入口および出口圧力で<±0.1psigの揺らぎ)したら、以下に進む。
(a)流量計で測定した測定値を記録する。
(b)すべての圧力および温度値を監視し、運転中のすべての観測事実および変化を記録する。透明配管で良好な相分離を監視する。データを記録する。チューブを「涸らす」ことのないように注意して各ラインから液体試料を取り出し、ガスクロマトグラフで用いる。10分後、次の運転に移る前に試料を取り出す。
(8)定期的にチェックする項目
(a)定期的に小さなKOポットを空にする。それぞれの側のシリンジポンプの中のシリンジが空になったら、両方の流れで連続的な流れが続くように、ボールバルブを切り替え、他方のシリンジポンプの電源を入れる。必要に応じてシリンジを液で満たし、運転計画を完了する。
(9)運転停止
(a)すべてのヒータおよびポンプの電源を切り、ノックアウトポットの液を抜き、原料ボールバルブを切り替えて、ノックアウトポットの頂部からベントラインへ液体が吹き出さないように注意して、システム全体を窒素でパージし、ラインの液体がほとんどなくなったように見えたら、再びノックアウトポットの液を抜き、その後、冷却時間の残りの間、窒素パージを続ける。冷えたら(<60℃)、窒素パージおよびチラーの電源を切る。
Claims (29)
- マイクロチャネル蒸留ユニットの中で流体混合物を蒸留するためのプロセスであって、前記マイクロチャネル蒸留ユニットは少なくとも一つの原料入口を有し、前記マイクロチャネル蒸留ユニットは複数のプロセスマイクロチャネルからなり、各プロセスマイクロチャネルは最大10ミリメートルの幅を有し、前記幅はプロセスマイクロチャネルを通る流れに垂直であり、前記マイクロチャネル蒸留ユニットは前記流体混合物を前記プロセスマイクロチャネルへ分配する流れ分配チャネルを有し、前記流体混合物は高揮発性成分と低揮発性成分とを含み、前記プロセスは、
前記マイクロチャネル蒸留ユニットの中の前記プロセスマイクロチャネルの中で蒸気相を第一の方向に流すこと、
前記マイクロチャネル蒸留ユニットの中で液体相を前記第一の方向に対して向流となる第二の方向に流すこと、および
前記原料入口を通して前記流体混合物を前記マイクロチャネル蒸留ユニットの流れ分配チャネルの中に流れ込ませ、前記流れ分配チャネルは前記プロセスマイクロチャネルに隣接する層の中で前記原料入口から前記マイクロチャネル蒸留ユニットを横切って延び、前記流れ分配チャネルは前記流体混合物を前記流れ分配チャネルから前記プロセスマイクロチャネルへ流れることを可能とする開口部を有し、前記流体混合物を前記流れ分配チャネルから前記プロセスマイクロチャネルへ流し、前記流体混合物を前記プロセスマイクロチャネルで前記蒸気相と前記液体相と接触させ、前記高揮発性成分の一部を前記流体混合物から前記蒸気相へ移動させて高揮発性成分が濃縮された蒸気相を形成させ、前記低揮発性成分の一部を前記流体混合物から前記液体相へ移動させて低揮発性成分が濃縮された液体相を形成させること
を含むプロセス。 - 前記マイクロチャネル蒸留ユニットは留出分端とボトム分端とを有し、前記マイクロチャネル蒸留ユニットは各プロセスマイクロチャネルの中に複数のマイクロチャネル蒸留区画を備える請求項1に記載のプロセスであって、
前記マイクロチャネル蒸留区画を通して前記高揮発性成分が濃縮された蒸気相を前記留出分端の方へ流し、前記高揮発性成分が濃縮された蒸気相を各マイクロチャネル蒸留区画の中の前記液体相と接触させ、前記高揮発性成分を濃縮させること、および
前記マイクロチャネル蒸留区画を通して前記低揮発性成分が濃縮された液体相を前記ボトム分端の方へ流し、前記低揮発性成分が濃縮された液体相を各マイクロチャネル蒸留区画の中で前記蒸気相と接触させ、前記低揮発性成分を濃縮させること
をさらに含むプロセス。 - 前記マイクロチャネル蒸留ユニットは、少なくとも一つの熱交換器を備える、請求項1に記載のプロセス。
- 各プロセスマイクロチャネルは前記蒸気相の流れを可能にする区域と、前記液体相の流れを可能にする区域とを備える、請求項1に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは留出分端と、前記留出分端にあるマイクロチャネルコンデンサとを有し、前記高揮発性成分が濃縮された蒸気相は前記プロセスマイクロチャネルを通して前記マイクロチャネルコンデンサへ流れるプロセスであって、少なくとも前記高揮発性成分が濃縮された蒸気相の一部が凝縮する、請求項1に記載のプロセス。
- 前記マイクロチャネルコンデンサは、マイクロチャネル蒸留区画の形である、請求項5に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットはボトム分端と、前記ボトム分端にあるマイクロチャネルリボイラとを有し、前記低揮発性成分が濃縮された蒸気相は前記プロセスマイクロチャネルを通して前記マイクロチャネルリボイラへ流れるプロセスであって、少なくとも前記低揮発性成分が濃縮された蒸気相の一部が蒸発する、請求項1に記載のプロセス。
- 前記マイクロチャネルリボイラは、マイクロチャネル蒸留区画の形である、請求項7に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは、複数のマイクロチャネル蒸留ユニットを備えるマイクロチャネル蒸留アセンブリの中にあり、前記複数のマイクロチャネル蒸留ユニットは並列動作する、請求項1に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは、複数のマイクロチャネル蒸留ユニットを備えるマイクロチャネル蒸留アセンブリの中にあり、前記複数のマイクロチャネル蒸留ユニットは直列動作する、請求項1に記載のプロセス。
- ウィック用層が蒸気相の流れのための前記区域と液体相の流れのための前記区域とを分離する、請求項4に記載のプロセス。
- 各プロセスマイクロチャネルは、蒸気相の流れのための前記区域の中の内壁と、液体相の流れのための前記区域の中の内壁とを有し、前記壁のそれぞれは互いに対向し、表面構成要素は前記壁のそれぞれの上および/または中に形成され、前記表面構成要素は、各壁の中の溝または各壁の上の突起物の形状である、請求項3に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットはプロセスマイクロチャネルと熱連通する熱交換チャネルを有し、熱交換流体は前記熱交換チャネルの中に存在し、前記熱交換流体は前記熱交換ゾーン群の中で一部沸騰する、請求項1に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは前記プロセスマイクロチャネルの前記マイクロチャネル蒸留区画と熱連通する熱交換流体を含む熱交換ゾーンを有し、前記熱交換流体は前記熱交換ゾーン群の中で一部沸騰し、前記熱交換ゾーン群のそれぞれの中の前記温度は異なる、請求項2に記載のプロセス。
- 前記高揮発性成分が濃縮された蒸気相の少なくとも一部は凝縮し、前記マイクロチャネル蒸留ユニットから抜き出される、請求項1に記載のプロセス。
- 前記高揮発性成分が濃縮された蒸気相はマイクロチャネルコンデンサの中で凝縮する、請求項15に記載のプロセス。
- 前記高揮発性成分が濃縮された蒸気相の少なくとも一部はマイクロチャネルコンデンサの中で凝縮し、前記マイクロチャネル蒸留ユニットの中に流れる、請求項5に記載のプロセス。
- 前記低揮発性成分が濃縮された液体相の少なくとも一部は、前記マイクロチャネル蒸留ユニットから抜き出される、請求項1に記載のプロセス。
- 前記低揮発性成分が濃縮された液体相の少なくとも一部は、前記マイクロチャネルリボイラの中で蒸発し、前記マイクロチャネル蒸留ユニットの中に流れる、請求項7に記載のプロセス。
- 前記マイクロチャネルリボイラはマイクロチャネル蒸留区画の形である、請求項19に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは、複数のマイクロチャネル蒸留ユニットを備えるマイクロチャネル蒸留アセンブリの中にあり、前記複数のマイクロチャネル蒸留ユニットのいくつかは動作中であり、前記複数のマイクロチャネル蒸留ユニットのいくつかは動作中でない、請求項1に記載のプロセス。
- 各マイクロチャネル蒸留ユニットは、最大3メートルの高さを有する、請求項1に記載のプロセス。
- 各マイクロチャネル蒸留ユニットの換算理論段の平均高さは1フィート(30.5cm)未満である、請求項1に記載のプロセス。
- 各マイクロチャネル蒸留ユニットの換算理論段の平均高さは1インチ(2.54cm)未満である、請求項1に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは、複数の前記マイクロチャネル蒸留ユニットと熱交換器を備えるマイクロチャネル蒸留アセンブリの中にあり、前記流体混合物を前記マイクロチャネル蒸留ユニットの中に流す前に、前記マイクロチャネル蒸留アセンブリは、−40℃の温度を有する前記熱交換器の中の熱交換流体を用いて室温から−33℃に冷却することができ、前記マイクロチャネル蒸留アセンブリを室温から−33℃に冷却するための時間は24時間より少ない、請求項1に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットは留出分端とボトム分端とを有し、前記原料入口は前記留出分端と前記ボトム分端との間に配置される、請求項1に記載のプロセス。
- 前記マイクロチャネル蒸留ユニットはプロセスマイクロチャネルと熱連通する熱交換ゾーンを有し、前記熱交換ゾーン群のそれぞれは少なくとも一つの熱交換流体ループを備える、請求項1に記載のプロセス。
- 熱交換流体が一つの熱交換流体ループから別の熱交換流体ループへ流れる、請求項27に記載のプロセス。
- 少なくとも二つの熱交換流体ループが入れ子構造になっている、請求項27に記載のプロセス。
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EP1781389A2 (en) | 2007-05-09 |
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CA2574113A1 (en) | 2006-02-23 |
US7610775B2 (en) | 2009-11-03 |
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