Deprecated: The each() function is deprecated. This message will be suppressed on further calls in /home/zhenxiangba/zhenxiangba.com/public_html/phproxy-improved-master/index.php on line 456
JP7720558B2 - Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow - Google Patents
[go: Go Back, main page]

JP7720558B2 - Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow - Google Patents

Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow

Info

Publication number
JP7720558B2
JP7720558B2 JP2021090993A JP2021090993A JP7720558B2 JP 7720558 B2 JP7720558 B2 JP 7720558B2 JP 2021090993 A JP2021090993 A JP 2021090993A JP 2021090993 A JP2021090993 A JP 2021090993A JP 7720558 B2 JP7720558 B2 JP 7720558B2
Authority
JP
Japan
Prior art keywords
liquid
slug
fluid
slug flow
flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
JP2021090993A
Other languages
Japanese (ja)
Other versions
JP2022183588A (en
Inventor
貴史 福田
慎一朗 川▲崎▼
知宏 市塚
明徳 武藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
University Public Corporation Osaka
Original Assignee
National Institute of Advanced Industrial Science and Technology AIST
University Public Corporation Osaka
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by National Institute of Advanced Industrial Science and Technology AIST, University Public Corporation Osaka filed Critical National Institute of Advanced Industrial Science and Technology AIST
Priority to JP2021090993A priority Critical patent/JP7720558B2/en
Publication of JP2022183588A publication Critical patent/JP2022183588A/en
Application granted granted Critical
Publication of JP7720558B2 publication Critical patent/JP7720558B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Physical Or Chemical Processes And Apparatus (AREA)

Description

本発明は、スラグ流の生成デバイス、前記スラグ流の生成デバイスを備えた化学物質の処理装置、並びにスラグ流の生成方法、及びスラグ流を用いた化学物質の処理方法に関する。ここでの処理とは、化学物質に関する反応又は分離(抽出、吸収、晶析等)又は反応分離をさす。 The present invention relates to a slug flow generation device, a chemical substance treatment device equipped with the slug flow generation device, a slug flow generation method, and a chemical substance treatment method using a slug flow. Here, "treatment" refers to reaction or separation (extraction, absorption, crystallization, etc.) of chemical substances, or reactive separation.

従来の化学反応プロセスにおいて、スケールアップによる効率化が求められていた。さらに近年においては、環境負荷の軽減、省資源及び省エネルギーの要求も加わる。
今後の成長が期待される医薬品や機能性化学品ないしはファインケミカルのような高付加価値品の生産においては、少量生産に向くバッチ生産方式が主流である。しかし、エネルギーロスが大きく、共生成物を多く排出するため、近年、反応から分離精製までを連続操作で行うフロー生産方式(以下、「フロープロセス」という。)により各バッチ処理工程間のロスの低減を試みる動きがある。また、必要に応じて反応モジュールや分離精製モジュールを組み替えることで、多種多様な機能性化学品の製造に対応できるよう、フロープロセスに組み込まれる各単位操作をモジュール化する研究開発の動きがある(非特許文献1)。
In conventional chemical reaction processes, there has been a demand for efficiency through scaling up. In recent years, there has also been an increased demand for reducing environmental impact and saving resources and energy.
In the production of high-value-added products such as pharmaceuticals, functional chemicals, and fine chemicals, which are expected to grow in the future, batch production methods suitable for small-scale production are mainstream. However, due to the large energy loss and large amount of co-products emitted, there has been a recent trend to reduce losses between each batch processing step by using flow production methods (hereinafter referred to as "flow processes"), which perform reactions, separation, and purification in a continuous manner. In addition, there is a movement in research and development to modularize each unit operation incorporated into flow processes so that they can be used to manufacture a wide variety of functional chemicals by rearranging reaction modules and separation and purification modules as needed (Non-Patent Document 1).

フロープロセスでは配管内ないしは配管の途中に接続された装置を流体が流通する過程で、温度調整、圧力調整、混合、反応、抽出、分離精製等の操作が行われる。各単位操作のモジュールの要件として、コンパクトかつ高速処理であることが求められる。特にフロープロセスにおいて、重要な対象は、互いに一部が溶け合うか、全く溶け合わない多相流体の流動が関わるプロセスである(例として、液液反応、気液反応、液液抽出、気液抽出、気液分離、液液分離)。通例、多相流体が関わるプロセスにおいて、プロセスのコンパクト化、高速処理化を目指すとき、相間物質移動抵抗を低減することが重要になる(非特許文献2、3、4)。 In flow processes, operations such as temperature adjustment, pressure adjustment, mixing, reaction, extraction, separation and purification are carried out as fluids flow through pipes or equipment connected to the pipes. Compactness and high-speed processing are required for each unit operation module. In particular, important targets in flow processes are processes involving the flow of multiphase fluids that are partially or completely soluble in each other (for example, liquid-liquid reactions, gas-liquid reactions, liquid-liquid extraction, gas-liquid extraction, gas-liquid separation, and liquid-liquid separation). In processes involving multiphase fluids, reducing interphase mass transfer resistance is typically important when aiming for compactness and high-speed processing (Non-Patent Documents 2, 3, 4).

相間物質移動抵抗は、相間の接触界面が大きい程低減され、反応性が向上する。
相間物質移動抵抗を低減する手段としては、反応器内に撹拌機構を組み込んで、相間の接触界面を増大することが知られている。
非特許文献5には、バッチリアクター内の撹拌機構により、乱流と呼ばれる流動状態を積極的に利用することが記載されている。
特許文献1には、複数の試料流体の導入部の下流に超音波振動子を配置して、前記の試料流体を撹拌混合する方法が記載されている。
また、特許文献2には、流路中の凹部でカーボンナノチューブからなる微小な撹拌子を回転させて撹拌し、層流から乱流に変化させて反応時間を短縮することが記載されている。
しかし、上記方法を採用する場合には、流路の形態を複雑にしたり、混合のための振動子や撹拌子を配置したりすることが必要であり、装置設計上必ずしも容易ではなかった。また、互いに相溶しない液体を細かく分散させ過ぎると、エマルジョン状態(図1(f)に示す流動状態)となり、大きな相間の接触界面が得られ、反応又は抽出等に有利である反面、相分離の効率を上げることが困難であった。
The larger the contact interface between the phases, the lower the interphase mass transfer resistance, and the higher the reactivity.
As a means for reducing the interphase mass transfer resistance, it is known to incorporate a stirring mechanism into the reactor to increase the contact interface between the phases.
Non-Patent Document 5 describes the active use of a fluid state called turbulence by means of a stirring mechanism within a batch reactor.
Patent Document 1 describes a method in which an ultrasonic vibrator is disposed downstream of an introduction portion for a plurality of sample fluids, and the sample fluids are stirred and mixed.
Furthermore, Patent Document 2 describes that a minute stirrer made of carbon nanotubes is rotated in a recess in a flow channel to stir the liquid, thereby changing the flow from laminar to turbulent, thereby shortening the reaction time.
However, when adopting the above method, it is necessary to complicate the shape of the flow channel and to install a vibrator or stirrer for mixing, which is not necessarily easy in terms of device design. Also, if incompatible liquids are dispersed too finely, an emulsion state (a flow state shown in Figure 1(f)) is formed, which results in a large contact interface between the phases. While this is advantageous for reactions or extraction, it is difficult to improve the efficiency of phase separation.

多相流体プロセスにおいて、目的とする単位操作に有利な流動状態を積極的に利用するために装置をコンパクト化することも挙げられる。通例少量生産を目的としたフロープロセスでは、バッチプロセスで扱われる空間に比べてスケールが小さく、また流量が低いため、レイノルズ数が低く、層流が支配的になる。このような層流域においても、分離状態にある異なる相の流体が交互に流れるスラグ流(セグメンテッド流、テイラー流とも呼ばれる。図1(a)、(b)に示す流動状態。)は、壁面からのせん断に由来にするスラグ内の内部循環流により、界面更新が促進されることで物質移動抵抗が低減する。また、大きな流体塊を形成可能であるため、相分離に要する時間が比較的短いという長所がある(特許文献3)。
図1は混相流の代表的な流動状態であり、例えば図1(c)~(f)に示す流動状態では、物質移動抵抗の低減効果が得られないのに対して、(a)、(b)に示すスラグ流では、内部循環流による物質移動抵抗の低減効果が発揮される。
In multiphase fluid processes, one approach is to compact the equipment to actively utilize flow conditions favorable for the target unit operation. Flow processes, typically aimed at small-scale production, are smaller in scale and have lower flow rates than batch processes, resulting in a low Reynolds number and dominant laminar flow. Even in this laminar flow regime, slug flow (also known as segmented flow or Taylor flow; see Figures 1(a) and 1(b) ) in which different phases of separated fluids alternately flow reduces mass transfer resistance by promoting interface renewal due to internal circulating flow within the slug caused by shear from the wall. Another advantage is the ability to form large fluid masses, resulting in a relatively short phase separation time (Patent Document 3).
Figure 1 shows typical flow states of multiphase flow. For example, the flow states shown in Figures 1(c) to 1(f) do not provide a reduction in mass transfer resistance, whereas the slug flow shown in (a) and (b) provides a reduction in mass transfer resistance due to the internal circulation flow.

従来、スラグ流は、異なる相の複数の流体を、それぞれの流体に対応する複数の流体移送手段であるポンプを用いて圧送することにより生成されてきた。
図2(a)、(b)に従来のスラグ流の生成デバイスの概念図を示す。
具体的には、2相流体の場合、特許文献3(請求項9)、非特許文献4(Fig.2)に示されるように、互いに相溶しない液体をそれぞれポンプで送液してT字流路等で合流させてスラグ流を生成している。
三相流体の場合も、3つ以上のポンプを用いて送液された流体を合流させて、スラグ流を生成することができる(非特許文献6 Fig.1、非特許文献7 Fig.1)。
Conventionally, slug flow has been generated by pumping a plurality of fluids of different phases using a plurality of fluid transport means, namely, pumps, corresponding to the respective fluids.
2(a) and (b) show conceptual diagrams of a conventional slug flow generating device.
Specifically, in the case of two-phase fluids, as shown in Patent Document 3 (claim 9) and Non-Patent Document 4 (Fig. 2), two immiscible liquids are pumped separately and merged in a T-shaped channel or the like to generate a slug flow.
In the case of three-phase fluids, a slug flow can also be generated by combining the fluids pumped using three or more pumps (Fig. 1 in Non-Patent Document 6, Fig. 1 in Non-Patent Document 7).

また、スラグ流の生成をより安定的に行う手段として、特許文献8には、互いに相溶しない2種類の液体を、流路内に設置した弁の切り替えによって、交互に流してスラグ流を生成し、抽質を抽出分離する方法が記載されている。このような方法によれば、層流支配の状況において、再現性良く交互に送流を行うことが可能である。
非特許文献9には、2台のピエゾマイクロポンプの動作を、電圧と周波数を変化させて連動して制御することにより、スラグ長さを制御できることが記載されている。
Furthermore, as a means for more stably generating a slug flow, Patent Document 8 describes a method in which two incompatible liquids are alternately flowed by switching a valve installed in a flow path to generate a slug flow and extract and separate the extracted substance. This method makes it possible to alternately send the liquids with good reproducibility in a laminar flow-dominated environment.
Non-Patent Document 9 describes that the slug length can be controlled by controlling the operation of two piezoelectric micropumps in conjunction with each other by changing the voltage and frequency.

特開平11-347392号公報Japanese Patent Application Publication No. 11-347392 特開2004-321063号公報Japanese Patent Application Laid-Open No. 2004-321063 特開2020-32346号公報Japanese Patent Application Laid-Open No. 2020-32346

NEDO、「機能性化学品の連続精密生産プロセス技術の開発」2020/06/25, https://www.nedo.go.jp/activities/ZZJP_100152.html 「機能性化学品の連続精密生産プロセス技術の開発」基本計画、https://www.nedo.go.jp/content/100893512.pdf (最終更新日2021年3月3日)NEDO, "Development of Continuous Precision Production Process Technology for Functional Chemicals," 2020/06/25, https://www.nedo.go.jp/activities/ZZJP_100152.html. "Development of Continuous Precision Production Process Technology for Functional Chemicals" Basic Plan, https://www.nedo.go.jp/content/100893512.pdf (Last updated March 3, 2021). J. R. Burns and C. Ramshaw、The intensification of rapid reactions in multiphase systems usingslug flow in capillaries、Lab Chip, 2001, 1, 10-15J. R. Burns and C. Ramshaw, The intensification of rapid reactions in multiphase systems using slug flow in capillaries, Lab Chip, 2001, 1, 10-15 Matthew W. Losey, Martin A. Schmidt, and Klavs F. Jensen、Microfabricated MultiphasePacked-Bed Reactors: Characterization of Mass Transfer and Reactions、Ind. Eng. Chem. Res.2001, 40, 12, 2555-2562Matthew W. Losey, Martin A. Schmidt, and Klavs F. Jensen, Microfabricated MultiphasePacked-Bed Reactors: Characterization of Mass Transfer and Reactions, Ind. Eng. Chem. Res.2001, 40, 12, 2555-2562 Madhvanand N. Kashid、Albert Renken、Lioubov Kiwi-Minske、Gas-liquid and liquid-liquid mass transfer in microstructuredreactors、Chemical Engineering Science 66 (2011) 3876-3897Madhvanand N. Kashid, Albert Renken, Lioubov Kiwi-Minske, Gas-liquid and liquid-liquid mass transfer in microstructure reactors, Chemical Engineering Science 66 (2011) 3876-3897 Fanfu Guan, Nikil Kapur, J. Taylor, Jialin Wen, Xumu Zhang and A.John Blacker、A universal reactor platform for batch and flow: application tohomogeneous and heterogeneous hydrogenation、React. Chem. Eng., 2020, 5, 1903-1908Fanfu Guan, Nikil Kapur, J. Taylor, Jialin Wen, Xumu Zhang and A.John Blacker, A universal reactor platform for batch and flow: application tohomogeneous and heterogeneous hydrogenation, React. Chem. Eng., 2020, 5, 1903-1908 Shusaku Asano, Yu Takahashi, Taisuke Maki, Yosuke Muranaka, Nikolay Cherkasov& Kazuhiro Mae、Contactless mass transfer for intra-droplet extraction、Scientific Reports、10 (2020)、pp. 7685-7693Shusaku Asano, Yu Takahashi, Taisuke Maki, Yosuke Muranaka, Nikolay Cherkasov& Kazuhiro Mae, Contactless mass transfer for intra-droplet extraction, Scientific Reports, 10 (2020), pp. 7685-7693 Nobuaki Aoki, Ryuichi Ando, and Kazuhiro、Mae,Gas-Liquid-Liquid Slug Flow for Improving Liquid-Liquid Extraction inMiniaturized Channels、Ind. Eng. Chem. Res. 2011, 50, 8, 4672-4677Nobuaki Aoki, Ryuichi Ando, and Kazuhiro, Mae,Gas-Liquid-Liquid Slug Flow for Improving Liquid-Liquid Extraction inMiniaturized Channels, Ind. Eng. Chem. Res. 2011, 50, 8, 4672-4677 門脇信傑、マイクロ化学プロセス用三方電磁弁の開発と応用、岡山大学大学院博士論文、3章、2014年3月Nobutaka Kadowaki, Development and Application of Three-Way Solenoid Valves for Micro Chemical Processes, Okayama University Graduate School Doctoral Dissertation, Chapter 3, March 2014 化学工学会第86年会K301 SCEJ 86th Annual Meeting 連動した2台のポンプによる液液スラグ流の発生K301 SCEJ 86th Annual Meeting Generation of liquid-liquid slug flow by two pumps operating in tandem

スラグ流の生成は、相間物質移動抵抗の低減に効果的であるが、従来の生成デバイスにおいては、1種類の流体の圧送に一つ以上のポンプが必要であり、また流量制御のための機構や交互送液を行うための切換え弁等が必要となるため、装置が大型化、複雑化していた。また、各ポンプには個体差があるため、複数のポンプの組み合わせを変える度に送液量や送液速度条件を調整する必要があった。
また、非特許文献9に記載されたピエゾマイクロポンプ(PMP)は圧電素子を用いたダイヤフラム式ポンプで、電圧によりダイヤフラムの振幅巾を変えて吐出圧を制御しており、吐出圧が低圧であるため、逆流の発生を抑止し難く、精密な送液が困難であった。
さらに、既存技術で発生させた三相スラグ流においては、抽出分離できる液体種の組み合わせが制限されており、汎用性に乏しかった。
そこで、本発明は、スラグ流の発現に要するポンプの台数を減らして小型化、簡略化し、相間物質移動抵抗の低減に効果的な条件を保持しながら精密な送液を行えるスラグ流の生成デバイスを提供すること、及びこのスラグ流の生成デバイスを備えた化学物質の処理装置を提供することを課題とする。
Although generating a slug flow is effective in reducing interphase mass transfer resistance, conventional generation devices require more than one pump to pump one type of fluid, and also require mechanisms for flow control and switching valves for alternate liquid transfer, making the device large and complex. Furthermore, because each pump has its own individual characteristics, it is necessary to adjust the liquid transfer volume and liquid transfer speed conditions each time the combination of multiple pumps is changed.
Furthermore, the piezoelectric micropump (PMP) described in Non-Patent Document 9 is a diaphragm pump using a piezoelectric element, and controls the discharge pressure by changing the amplitude of the diaphragm using voltage. Since the discharge pressure is low, it is difficult to prevent backflow, making it difficult to deliver liquid precisely.
Furthermore, the three-phase slug flow generated by existing technology is limited in the combinations of liquid species that can be extracted and separated, making it less versatile.
Therefore, an object of the present invention is to provide a slug flow generating device that reduces the number of pumps required to generate a slug flow, thereby making it smaller and simpler, and that can perform precise liquid transfer while maintaining conditions that are effective in reducing interphase mass transfer resistance, and to provide a chemical substance treatment apparatus equipped with this slug flow generating device.

本発明者らは、1台のダブルプランジャーポンプの各プランジャーが交互に流体を圧送する機構に着目し、完全相溶しない複数の流体を、一流体が流れている間はそれ以外の流体が流れない圧送方法とすることで、スラグ流を生成することができることを見いだした。 The inventors focused on the mechanism by which each plunger of a double plunger pump alternately pumps fluids, and discovered that a slug flow can be generated by using a pumping method for multiple fluids that are not completely miscible, such that one fluid does not flow while the other fluids do.

すなわち、上記課題を解決するために、本発明では、以下の手段を採用するものである。
[1]複数の流体のスラグ流を生成するデバイスであって、
前記複数の流体をそれぞれ保持する複数の流体保持部、
逆止的に作動する吸引側の弁と吐出側の弁に挟まれた空間を画定する複数の筐体を有し、各筐体内の流体が、カムシャフトを用いた機械的な駆動方式により吸引と吐出を行うことにより、交互に間欠的に圧送される往復動ポンプ、
前記複数の流体保持部と前記複数の筐体をそれぞれ接続する複数の吸引配管部、
前記複数の筐体と流体合流部をそれぞれ接続する複数の吐出配管部、及び、
前記流体合流部の下流に接続する流体滞留部を有するスラグ流の生成デバイス。
]前記流体滞留部で反応又は分離が行われる前記[1]のスラグ流の生成デバイス。
]前記複数の筐体の少なくとも1つが、筐体内を流通する流体の液体状態を保つ温度調節機能を有する前記[1]又は[2]のスラグ流の生成デバイス。
]前記スラグ流の一相が液化二酸化炭素であり、他の相が液体である前記[]のスラグ流の生成デバイス。
]前記[1]~[]のいずれか1のスラグ流の生成デバイスを備えた化学物質の処理装置。
]前記スラグ流の生成デバイスの下流に液液分離機構を有する前記[]の化学物質の処理装置。
]前記スラグ流の生成デバイスと前記液液分離機構の間に気液分離機構を有する前記[]の化学物質の処理装置。
]前記気液分離機構の上部には圧力制御機構を備えた気体排出管が接続され、下部には、前記液液分離機構に接続する液体排出管が接続されている前記[]の化学物質の処理装置。
]逆止的に作動する吸引側の弁と吐出側の弁に挟まれた空間を画定する複数の筐体を有し、カムシャフトを用いた機械的な駆動方式により吸引と吐出を行う1台の往復動ポンプを用い、
複数の流体供給部と前記複数の筐体のそれぞれを接続する複数の吸引配管手段、及び前記複数の筐体のそれぞれと複数の流体の合流部を接続する複数の吐出配管手段を介して複数の流体を交互に間欠的に送液し、
前記合流部の下流に設けられた流体滞留部で前記複数の流体のスラグ流を生成する方法。
10]前記[]のスラグ流を生成する方法を含む化学物質の処理方法。
11]生成したスラグ流を液液分離する前記[10]の化学物質の処理方法。
12]生成したスラグ流を気液分離してから液液分離する前記[11]の化学物質の処理方法。
13]前記気液分離された気体に背圧を加えて流体全体の圧力を制御する前記[12]の化学物質の処理方法。
That is, in order to solve the above problems, the present invention employs the following means.
[1] A device for generating a slug stream of multiple fluids, comprising:
a plurality of fluid holding portions each holding the plurality of fluids;
A reciprocating pump has a plurality of housings that define a space between a suction-side valve and a discharge-side valve that operate in a check manner, and the fluid in each housing is alternately and intermittently pumped by suction and discharge using a mechanical drive system using a camshaft ;
a plurality of suction pipes respectively connecting the plurality of fluid holding units to the plurality of housings;
a plurality of discharge pipes respectively connecting the plurality of housings to a fluid confluence portion; and
A slug flow generating device having a fluid retention section connected downstream of the fluid confluence section.
[ 2 ] The slug flow generating device according to [1 ] , wherein reaction or separation occurs in the fluid retention section.
[ 3 ] The slug flow generating device according to [1] or [2] , wherein at least one of the plurality of housings has a temperature control function for maintaining the fluid circulating within the housing in a liquid state.
[ 4 ] The device for generating a slug stream according to [ 3 ], wherein one phase of the slug stream is liquefied carbon dioxide and the other phase is a liquid.
[ 5 ] A chemical substance treatment device equipped with the slug flow generating device according to any one of [1] to [ 4 ].
[ 6 ] The chemical substance treatment device according to [ 5 ], which has a liquid-liquid separation mechanism downstream of the slug flow generation device.
[ 7 ] The chemical substance treatment device according to [ 6 ], further comprising a gas-liquid separation mechanism between the slug flow generating device and the liquid-liquid separation mechanism.
[ 8 ] A gas discharge pipe equipped with a pressure control mechanism is connected to the upper part of the gas-liquid separation mechanism, and a liquid discharge pipe connected to the liquid-liquid separation mechanism is connected to the lower part. The chemical substance treatment device of [ 7 ].
[ 9 ] A reciprocating pump having a plurality of housings defining a space between a suction-side valve and a discharge-side valve that operate in a check manner, and that performs suction and discharge by a mechanical drive system using a camshaft ,
alternately and intermittently sending the plurality of fluids through a plurality of suction piping means connecting the plurality of fluid supply units to the plurality of housings, respectively, and a plurality of discharge piping means connecting the plurality of housings to a confluence of the plurality of fluids;
A method for generating slug flows of the plurality of fluids in a fluid retention section provided downstream of the confluence section.
[ 10 ] A method for treating chemical substances, comprising the method for generating a slug flow according to [ 9 ].
[ 11 ] The method for treating chemical substances according to [ 10 ], wherein the generated slag stream is subjected to liquid-liquid separation.
[ 12 ] The method for treating a chemical substance according to [ 11 ], wherein the generated slag stream is subjected to gas-liquid separation and then liquid-liquid separation.
[ 13 ] The method for treating a chemical substance according to [ 12 ], wherein a back pressure is applied to the gas after gas-liquid separation to control the pressure of the entire fluid.

本発明によれば、幅広い流量範囲でスラグ流を安定的に生成することができるので、スラグ流を利用した化学物質の製造装置をコンパクト化しつつ、高速処理を可能とする。
また、往復動ポンプの駆動方式が、モーターの回転に連動して偏心するカムシャフトによるものであるため、高い吐出圧が得られ、逆流の発生を防いで高精度な送液を実現することができる。
According to the present invention, a slug flow can be stably generated over a wide range of flow rates, thereby enabling high-speed processing while making a chemical manufacturing device that utilizes a slug flow more compact.
Furthermore, the reciprocating pump is driven by an eccentric camshaft that moves in conjunction with the rotation of the motor, which allows for high discharge pressure, prevents backflow, and achieves highly accurate liquid delivery.

混相流の代表的な流動状態図 (a)二相スラグ流、(b)三相スラグ流、(c)並行流、(d)環状流、(e)液滴流、(f)分散流Representative flow diagrams for multiphase flows: (a) two-phase slug flow, (b) three-phase slug flow, (c) parallel flow, (d) annular flow, (e) droplet flow, (f) dispersed flow. 従来のスラグ流生成デバイスの構成図 (a)二相系、(b)三相系Diagram of a conventional slug flow generating device (a) Two-phase system, (b) Three-phase system 本発明のスラグ流生成デバイスの構成図 (a)二相系、(b)三相系1. Diagram of the slug flow generating device of the present invention. (a) Two-phase system, (b) Three-phase system プランジャーポンプとピエゾマイクロポンプ(PMP)の送液精度を示すグラフGraph showing the liquid delivery accuracy of a plunger pump and a piezoelectric micropump (PMP) 流体合流部の合流パターン (a)二相系、(b)三相系Confluence pattern of fluid confluence area (a) Two-phase system, (b) Three-phase system 本発明のスラグ流生成デバイスを用いた化学物質処理装置の構成図1 is a diagram showing the configuration of a chemical substance treatment apparatus using a slug flow generating device according to the present invention. トルエン/水(実施例1と比較例1)の各液流量における目視の流動状態Visual flow state of toluene/water (Example 1 and Comparative Example 1) at each liquid flow rate トルエン/エタノール:水=1:1(実施例2と比較例2)の各液流量における目視の流動状態Visual flow state at each liquid flow rate of toluene/ethanol:water=1:1 (Example 2 and Comparative Example 2) トルエン/エタノール:水=2:1(実施例3と比較例3)の各液流量における目視の流動状態Visual flow state at each liquid flow rate for toluene/ethanol:water=2:1 (Example 3 and Comparative Example 3) トルエン/エタノール:水=3:1(実施例4と比較例4)の各液流量における目視の流動状態Visual flow state at each liquid flow rate of toluene/ethanol:water=3:1 (Example 4 and Comparative Example 4) トルエンリッチ相/エタノールリッチ相(実施例5と比較例5)の各液流量における目視の流動状態Visual flow state of the toluene-rich phase/ethanol-rich phase (Example 5 and Comparative Example 5) at each liquid flow rate トルエン/水(実施例1と比較例1)の各液流量4mL/minにおける流動状態の経時変化Change in flow state over time of toluene/water (Example 1 and Comparative Example 1) at a liquid flow rate of 4 mL/min トルエン/エタノール:水=2:1(実施例3と比較例3)の各液流量4mL/minにおける流動状態の経時変化Change in flow state over time at a liquid flow rate of 4 mL/min for toluene/ethanol:water = 2:1 (Example 3 and Comparative Example 3)

以下、本明細書で使用する用語について説明する。
ポンプの「逆止的に作動する吸引側の弁と吐出側の弁に挟まれた空間を画定する複数の筐体」を「ヘッド」という。
ポンプのヘッド数に応じた液体種を各ヘッドで供給し、一流体が流れている間はそれ以外の流体が流れていない圧送方法を「交互圧送」という。
一流体を一つ以上のヘッドを有する1台のポンプで送液することを特徴とした一般的な圧送方法を「一液圧送」という。
The terms used in this specification will be explained below.
The pump's "multiple housings that define the space between the suction-side valve and the discharge-side valve that operate in a non-return manner" are called the "head."
A pumping method in which a type of liquid corresponding to the number of pump heads is supplied at each head, and while one fluid is flowing, the other fluids do not flow is called "alternate pumping."
A common pumping method characterized by pumping one fluid with one pump having one or more heads is called "single fluid pumping."

本発明は、通常のスラグ流が、一つ以上のヘッドを有する1台のポンプで一流体を圧送する一液圧送を複数のポンプを組み合わせて行って生成されるのに対して、複数のヘッドを有する1台のポンプを用いて、一流体が流れている間はそれ以外の流体が流れていないように複数の流体を交互に間欠的に圧送する交互圧送によりスラグ流を生成する点に特徴を有する。
また、本発明は、前記スラグ流の滞留中で反応又は分離(抽出、吸収、晶析等)又は反応分離された化学物質を液液分離、必要に応じて気液分離することにより、化学物質の処理を可能とする点に特徴を有する。
以下、本発明の実施形態(以下、「本実施形態」という。)に基づいて説明するが、本発明は本実施形態に限定されるものではない。
While a typical slug flow is generated by a combination of multiple pumps, in which a single pump with one or more heads pumps a single fluid, the present invention is characterized in that a slug flow is generated by alternating pumping, in which a single pump with multiple heads is used to pump multiple fluids alternately and intermittently so that while one fluid is flowing, the other fluids are not flowing.
Another feature of the present invention is that it enables the treatment of chemical substances by reacting or separating (extracting, absorbing, crystallizing, etc.) the chemical substances that have been reacted or separated in the slag flow, or by subjecting the chemical substances that have been reacted and separated to liquid-liquid separation, and, if necessary, gas-liquid separation.
Hereinafter, the present invention will be described based on an embodiment (hereinafter referred to as "the present embodiment"), but the present invention is not limited to the present embodiment.

[スラグ流生成デバイス及びスラグ流生成方法]
複数のヘッドを有する往復動ポンプとして、1台のポンプに2つ以上のプランジャーを有するダブルプランジャーポンプ又は3連プランジャーポンプが既に知られている。これらのポンプは、複数のヘッドを有し、各プランジャーの往復動により各ヘッド内の流体を交互に送液し、各ヘッドからの流量変動を相殺し合い、脈動の発生を抑制する機構を内在している。しかし、通常、各ヘッドから送液される流体は同一であるから、これらのポンプの送液は定流量の一液圧送である。
[Slug flow generating device and slug flow generating method]
Known reciprocating pumps with multiple heads include double plunger pumps and triple plunger pumps, which have two or more plungers in one pump. These pumps have multiple heads, and the reciprocating motion of each plunger alternately pumps fluid from each head, offsetting fluctuations in flow rate from each head and suppressing pulsation. However, because the fluid pumped from each head is usually the same, these pumps pump a single liquid at a constant flow rate.

本実施形態では、上記既知のポンプの脈動の抑制機構を利用し、各ヘッドにそれぞれ異なる流体を供給する。図3(a)、(b)に、プランジャーポンプを用いた場合の構成を示す。なお、前記往復動ポンプの駆動方式は、精密な送液が行われるように高い圧送力が得られる機械式であることが好ましく、モーターの回転に連動して偏心するカムシャフトによるものであることが好ましい。代表的には、上記のプランジャーポンプのほかにダイヤフラムポンプが挙げられる。
図4に、後述する本実施例に使用したプランジャーポンプと、往復動が圧電素子により電気式に行わるピエゾマイクロポンプ(PMP)との送液精度の比較を示す。前者の結果の一例が図4(a)であり、後者の結果の一例が図4(b)である。近似直線のR値を指標とすると、前者はR=1.0(>0.999)であり、後者のR=0.968であることから、プランジャーポンプはPMPよりも送液精度が高いことがわかる。
In this embodiment, a different fluid is supplied to each head by utilizing the known pump pulsation suppression mechanism. Figures 3(a) and (b) show a configuration using a plunger pump. The reciprocating pump is preferably driven mechanically to obtain a high pumping force for precise liquid delivery, and preferably by an eccentric camshaft that rotates in conjunction with the rotation of the motor. In addition to the plunger pump, a diaphragm pump is also a typical example.
Figure 4 shows a comparison of the liquid delivery accuracy between the plunger pump used in this example (described later) and a piezoelectric micropump (PMP), in which reciprocation is performed electrically by a piezoelectric element. An example of the results for the former is shown in Figure 4(a), and an example of the results for the latter is shown in Figure 4(b). Using the R2 value of the approximate line as an index, the former has R2 = 1.0 (> 0.999), while the latter has R2 = 0.968, indicating that the plunger pump has higher liquid delivery accuracy than the PMP.

異なる流体としては、相溶する流体同士ではスラグ流を生成しないから、完全には相溶しない流体を組み合わせる。水相と油相の液-液であってよく、液相と気相の気-液でもよい。液相は液化ガス、例えば液化二酸化炭素であってもよい。超臨界流体、亜臨界流体、イオン液体が相溶しない流体のいずれか1つであってもよい。 The different fluids are fluids that are not completely miscible, since miscible fluids do not form a slug flow. They may be liquid-liquid, consisting of an aqueous phase and an oil phase, or gas-liquid, consisting of a liquid phase and a gas phase. The liquid phase may be a liquefied gas, such as liquefied carbon dioxide. They may also be any one of the following fluids: supercritical fluid, subcritical fluid, or ionic liquid, which are immiscible with each other.

流体の1つ以上が常温常圧で気体である場合、当該流体がポンプのヘッドを通過する際に液化するために、当該流体が通過するヘッドに当該流体の液体状態を保つ温度調節機能を有することが好ましい。
スラグ流を生成し得る好ましい気体としては、気液平衡温度が31℃度以下である二酸化炭素が挙げられる。
If one or more of the fluids is a gas at room temperature and pressure, the fluids will liquefy as they pass through the pump head, so it is preferable that the head through which the fluids pass has a temperature control function to maintain the fluids in a liquid state.
A preferred gas capable of forming a slug flow is carbon dioxide, which has a gas-liquid equilibrium temperature of 31°C or less.

水相と二酸化炭素の組み合わせの一例として、ポンプ吐出時は液化二酸化炭素である場合が想定される。その場合、プロセスは二酸化炭素の臨界圧(7.4MPa)以上であることが好ましく、スラグ流領域の下流に背圧弁を設けて、ポンプから背圧弁までの圧力を制御することができる。二酸化炭素は高圧条件下でのみ、有機溶剤の代替が可能となるため、水相中の疎水性有価物は高圧二酸化炭素によって抽出されることが期待される。 As an example of a combination of aqueous phase and carbon dioxide, consider a case where the carbon dioxide is liquefied when discharged from the pump. In this case, it is preferable that the process be at or above the critical pressure of carbon dioxide (7.4 MPa), and a back-pressure valve can be installed downstream of the slug flow region to control the pressure from the pump to the back-pressure valve. Since carbon dioxide can only replace organic solvents under high-pressure conditions, it is expected that hydrophobic valuables in the aqueous phase will be extracted by the high-pressure carbon dioxide.

前記複数の流体は、各流体を保持する複数の流体保持部(液体タンク又はガスボンベ等)と前記複数のヘッドを接続する複数の吸引配管部、及び前記各ヘッドと流体合流部を接続する複数の吐出配管部を介して、前記流体合流部へ交互に間欠的に圧送され、流体合流部の下流に接続する流体滞留部でスラグ流を生成することができる。 The multiple fluids are alternately and intermittently pumped to the fluid junction via multiple suction pipes connecting multiple fluid holding units (liquid tanks, gas cylinders, etc.) that hold each fluid to the multiple heads, and multiple discharge pipes connecting each head to the fluid junction, generating a slug flow in the fluid retention unit connected downstream of the fluid junction.

図5(a)、(b)に流体合流部の合流パターンを示す。ただし、衝突順序、衝突角θは図5に規定されるものではない。
前記流体滞留部では、液液反応、気液反応、固体触媒反応を含む反応、抽出、吸収、晶析等による分離、又は反応分離を行うことができる。
5(a) and 5(b) show the confluence patterns of the fluid confluence portion, but the collision order and collision angle θ are not specified in FIG.
In the fluid retention section, reactions including liquid-liquid reactions, gas-liquid reactions, and solid catalyst reactions, separation by extraction, absorption, crystallization, etc., or reaction separation can be carried out.

[化学物質の処理装置及び処理方法]
本実施形態では、図6に示すように、スラグ流が生成された前記流体滞留部で反応、分離、又は反応分離が行われた後、前記流体滞留部の下流に液液分離器を配置し、また、必要に応じて、前記流体滞留部と前記液液分離器の間に気液分離器を配置して、化学物質を含む相を連続的に分離精製する。
気液分離器を配置する場合、気液分離器の上部には背圧弁を設けた気体排出管が接続され、下部には前記液液分離器に接続する液体排出管が接続される。
背圧弁によりポンプ出口から背圧弁の間の圧力を制御することができる。
[Chemical substance treatment device and treatment method]
In this embodiment, as shown in FIG. 6, after reaction, separation, or reaction separation is carried out in the fluid retention section where the slug flow is generated, a liquid-liquid separator is disposed downstream of the fluid retention section, and if necessary, a gas-liquid separator is disposed between the fluid retention section and the liquid-liquid separator, so that the phase containing the chemical substance is continuously separated and purified.
When a gas-liquid separator is provided, a gas discharge pipe equipped with a back pressure valve is connected to the top of the gas-liquid separator, and a liquid discharge pipe connected to the liquid-liquid separator is connected to the bottom.
The back pressure valve can control the pressure between the pump outlet and the back pressure valve.

以下、実施例及び比較例に基づいて本発明を具体的に説明するが、実施例は、本発明の好適な例を示すものであり、本発明は、実施例によって何ら限定されるものではない。 The present invention will be specifically explained below based on examples and comparative examples. However, the examples are intended to illustrate preferred examples of the present invention, and the present invention is not limited in any way by the examples.

<実施例1>
カムシャフトにより駆動し、脈流を抑制する機構を有するダブルプランジャーポンプ(日本精密科学NP-KX-220P、プランジャー径4.6mm、ストローク長:5mm(1ストローク当たりの送液量0.0831mL))を用い、一方のヘッドの吸引側にA液としてトルエンを貯留するタンクを吸引配管を介して接続し、他方のヘッドの吸引側にB液として水を貯留するタンクを他の吸引配管を介して接続した。各ヘッドの吐出側には、それぞれの吐出配管を介して内径2mmのSUSティで構成されたA液とB液の合流部を接続した。前記合流部の下流に内径2mm、長さ30cmのガラスチューブからなる流体滞留部を接続した。
A液及びB液の各流量が、それぞれ0.5、1、2、4、6、8及び10mL/min相当となるように各プランジャーを往復動させて交互圧送し、前記流体滞留部における流動状態を目視でチェックした。
Example 1
A double plunger pump (Nihon Seimitsu Kagaku NP-KX-220P, plunger diameter 4.6 mm, stroke length: 5 mm (liquid delivery volume per stroke: 0.0831 mL)) driven by a camshaft and equipped with a mechanism for suppressing pulsation was used. A tank storing toluene as liquid A was connected to the suction side of one head via a suction pipe, and a tank storing water as liquid B was connected to the suction side of the other head via another suction pipe. A confluence of liquid A and liquid B, composed of a SUS tee with an inner diameter of 2 mm, was connected to the discharge side of each head via the respective discharge pipes. A fluid retention section composed of a glass tube with an inner diameter of 2 mm and a length of 30 cm, was connected downstream of the confluence.
The plungers were reciprocated to alternately pump the A and B solutions so that their flow rates were equivalent to 0.5, 1, 2, 4, 6, 8, and 10 mL/min, respectively, and the flow state in the fluid retention section was visually checked.

<実施例2~4>
B液を、エタノール/水の体積比が1:1(実施例2)、2:1(実施例3)、3:1(実施例4)の溶液に変更した以外は、実施例1と同様に交互圧送した。
<Examples 2 to 4>
Alternate pumping was carried out in the same manner as in Example 1, except that solution B was changed to a solution in which the volume ratio of ethanol/water was 1:1 (Example 2), 2:1 (Example 3), or 3:1 (Example 4).

<比較例1~4>
実施例1と同じダブルプランジャーポンプを2台用い、一方のポンプの二つのヘッドにA液を供給し、他方のポンプの二つのヘッドにB液を供給し、各流量が実施例1と同じになるように各ポンプでA液及びB液を一液圧送した以外は実施例1~4と同様にして、比較例1とした。
また、B液をそれぞれ実施例2~4と同じ体積比のエタノール/水の溶液に変更した以外は、比較例1と同様に送液し、それぞれ比較例2~4とした。
<Comparative Examples 1 to 4>
Comparative Example 1 was prepared in the same manner as in Examples 1 to 4, except that two double plunger pumps identical to those in Example 1 were used, liquid A was supplied to the two heads of one pump, and liquid B was supplied to the two heads of the other pump, and liquid A and liquid B were pressure-fed one by one by each pump so that the respective flow rates were the same as in Example 1.
In addition, the liquid was transferred in the same manner as in Comparative Example 1, except that the liquid B was changed to an ethanol/water solution with the same volume ratio as in Examples 2 to 4, and these were designated Comparative Examples 2 to 4, respectively.

<実施例5>
トルエンと、エタノール/水の体積比が1:1の液体とを同量混合後、分液し、トルエンリッチ液をA液、エタノールリッチ液をB液とした。すなわちA液とB液は完全に非相溶な二液である。このA液及びB液を実施例1と同様に1台のダブルプランジャーポンプを用いて交互圧送を行った。
Example 5
Equal amounts of toluene and a liquid with a volume ratio of ethanol/water of 1:1 were mixed, and then the liquids were separated, with the toluene-rich liquid being designated as Liquid A and the ethanol-rich liquid being designated as Liquid B. In other words, Liquid A and Liquid B are two completely immiscible liquids. Liquid A and Liquid B were alternately pumped using a single double plunger pump, as in Example 1.

<比較例5>
実施例5と同じA液及びB液を、比較例1と同様に2台のダブルプランジャーポンプを用いて一液圧送した。
Comparative Example 5
The same liquids A and B as in Example 5 were pumped together using two double plunger pumps in the same manner as in Comparative Example 1.

図7~11に実施例1~5、及び比較例1~5の各液流量における流体滞留部における流動状態を示す。
図中、〇はスラグ流、●は下流でスラグ流発生、□は層状流、△は環状流を表し、サイズを問わず液滴が混ざった流動は‘(プライム)を付けた。
また、図12、13は、実施例1と比較例1、及び実施例3と比較例3において、各液流量が4mL/minのときの流体滞留部における流動状態の経時変化を、光電センサにより二値化された電位によって可視化したものである。スラグ流が安定な状態で流れれば、2相の交互流れを反映した規則的な矩形の電位変化を示す。
7 to 11 show the flow state in the fluid stagnation portion at each liquid flow rate in Examples 1 to 5 and Comparative Examples 1 to 5.
In the figure, circles indicate slug flow, black circles indicate slug flow occurring downstream, squares indicate stratified flow, and triangles indicate annular flow. Flows containing droplets of any size are marked with a prime.
12 and 13 show the time-dependent changes in the flow state in the fluid retention area when the flow rate of each liquid was 4 mL/min, visualized by the potential digitized by a photoelectric sensor, in Example 1 and Comparative Example 1, and in Example 3 and Comparative Example 3. If the slug flow is stable, it will show regular rectangular potential changes that reflect the alternating two-phase flow.

図7によると、実施例1と比較例1では、各液の流量が0.5~10mL/minのいずれであってもスラグ流が発生したことがわかる。しかし、図12によると、比較例1では、スラグ流の交互周期が平均0.20secと短く、流体滞留部に引き続く化学物質の分離精製の困難性が予測される一方、実施例1では、平均1.24secと長周期の交互流が観察され、スラグ流中で反応、抽出等が行われた後の分離精製が容易であることが見て取れる。 Figure 7 shows that in Example 1 and Comparative Example 1, slug flow occurred regardless of the flow rate of each liquid, from 0.5 to 10 mL/min. However, Figure 12 shows that in Comparative Example 1, the alternating period of the slug flow was short, averaging 0.20 seconds, suggesting that separation and purification of chemical substances following the fluid stagnation area would be difficult. In Example 1, on the other hand, alternating flows with a long period, averaging 1.24 seconds, were observed, indicating that separation and purification would be easy after reactions, extractions, etc., occurred in the slug flow.

図8によると、比較例2では、スラグ流を生成する流量範囲が狭く限られているが、実施例2では、1~10mL/minの流量でスラグ流が生成したことがわかる。図9における比較例3と実施例3の関係も同様であり、比較例3では、4mL/min以下の流量でないとスラグ流が生成しないが、実施例3では、8mL/minの流量まででスラグ流が生成したことがわかる。
また、図10によると、比較例2、3よりB液の有機分が多い比較例4(A液との極性、比重の差がより小さい)では、スラグ流が得られていないが、実施例4では、幅広い流量範囲でスラグ流の生成が見られたことがわかる。
8, it can be seen that the flow rate range in which a slug flow was generated was narrow and limited in Comparative Example 2, but a slug flow was generated at a flow rate of 1 to 10 mL/min in Example 2. The relationship between Comparative Example 3 and Example 3 in Figure 9 is similar; in Comparative Example 3, a slug flow was not generated unless the flow rate was 4 mL/min or less, but in Example 3, a slug flow was generated at a flow rate of up to 8 mL/min.
Furthermore, as shown in FIG. 10, in Comparative Example 4, in which the organic content of Liquid B was higher than in Comparative Examples 2 and 3 (the difference in polarity and specific gravity with Liquid A was smaller), no slug flow was obtained, whereas in Example 4, the generation of a slug flow was observed over a wide range of flow rates.

実施例3の液滴を含むスラグ流について、流動状態の経時変化を図13で確認すると、A液とB液の交互送液に由来するとみられる平均1.27secの周期的な波形が見られた。一方、比較例3からは規則性のないランダムな波形しか得られなかった。 When examining the change in flow state over time for the droplet-containing slug flow of Example 3 in Figure 13, a periodic waveform with an average of 1.27 seconds was observed, which is thought to be due to the alternating flow of liquids A and B. On the other hand, only a random waveform with no regularity was obtained from Comparative Example 3.

図11によると、トルエンリッチ、エタノールリッチの2相流においても、比較例5ではスラグ流の生成が殆ど見られなかったのに対して、実施例5では、1~10mL/minの流量範囲で、液滴を含むものの、スラグ流の生成が見られた。 Figure 11 shows that even in the case of toluene-rich and ethanol-rich two-phase flows, the generation of slug flow was barely observed in Comparative Example 5, whereas in Example 5, the generation of slug flow, although containing droplets, was observed in the flow rate range of 1 to 10 mL/min.

本発明に係るスラグ流の生成デバイスは、幅広い流量範囲で精密度の高いスラグ流を安定的に生成することができるので、異なる流体間の物質移動を促進し、高品質な化学物質の合成反応が可能である。また、この生成デバイスの下流に液液分離機構、気液分離機構等を連結することにより、抽出分離等を高速、低コストで行うことが期待される。本発明により多種多様な機能性化学品を含む化学物質に関する反応から分離精製までのプロセスを連続的に行うことが可能となる。また、連続プロセスへの適用に限らず、バッチプロセスで実施される反応または抽出分離等に適用することで同様に高速、低コストで行うことが期待される。

The slug flow generating device of the present invention can stably generate highly precise slug flows over a wide flow rate range, facilitating mass transfer between different fluids and enabling high-quality chemical synthesis reactions. Furthermore, by connecting a liquid-liquid separation mechanism or a gas-liquid separation mechanism downstream of this generating device, extraction and separation processes can be performed quickly and at low cost. The present invention enables continuous processes from reaction to separation and purification for chemical substances, including a wide variety of functional chemicals. Furthermore, the present invention is not limited to application to continuous processes; it can also be applied to reactions or extraction and separation performed in batch processes, enabling similar high-speed and low-cost performance.

Claims (13)

複数の流体のスラグ流を生成するデバイスであって、
前記複数の流体をそれぞれ保持する複数の流体保持部、
逆止的に作動する吸引側の弁と吐出側の弁に挟まれた空間を画定する複数の筐体を有し、各筐体内の流体が、カムシャフトを用いた機械的な駆動方式により吸引と吐出を行うことにより、交互に間欠的に圧送される1台の往復動ポンプ、
前記複数の流体保持部と前記複数の筐体をそれぞれ接続する複数の吸引配管部、
前記複数の筐体と流体合流部をそれぞれ接続する複数の吐出配管部、及び、
前記流体合流部の下流に接続する流体滞留部を有するスラグ流の生成デバイス。
1. A device for producing a slug stream of multiple fluids, comprising:
a plurality of fluid holding portions each holding the plurality of fluids;
A reciprocating pump having a plurality of housings defining a space between a suction-side valve and a discharge- side valve that operate in a check manner, in which the fluid in each housing is alternately and intermittently pumped by suction and discharge using a mechanical drive system using a camshaft ;
a plurality of suction pipes respectively connecting the plurality of fluid holding units to the plurality of housings;
a plurality of discharge pipes respectively connecting the plurality of housings to a fluid confluence portion; and
A slug flow generating device having a fluid retention section connected downstream of the fluid confluence section.
前記流体滞留部で反応又は分離が行われる請求項1に記載のスラグ流の生成デバイス。 The device for generating a slug flow according to claim 1 , wherein a reaction or separation takes place in the fluid retention section. 前記複数の筐体の少なくとも1つが、筐体内を流通する流体の液体状態を保つ温度調節機能を有する請求項1又は2に記載のスラグ流の生成デバイス。 3. The slug flow generating device according to claim 1 , wherein at least one of the plurality of housings has a temperature control function for maintaining the fluid flowing within the housing in a liquid state. 前記スラグ流の一相が液化二酸化炭素であり、他の相が液体である請求項に記載のスラグ流の生成デバイス。 4. The device for generating a slug stream according to claim 3 , wherein one phase of the slug stream is liquefied carbon dioxide and the other phase is a liquid. 請求項1~のいずれかに記載のスラグ流の生成デバイスを備えた化学物質の処理装置。 A chemical substance treatment apparatus comprising the slug flow generating device according to any one of claims 1 to 4 . 前記スラグ流の生成デバイスの下流に液液分離機構を有する請求項に記載の化学物質の処理装置。 6. The chemical substance treatment apparatus according to claim 5 , further comprising a liquid-liquid separation mechanism downstream of the slug flow generating device. 前記スラグ流の生成デバイスと前記液液分離機構の間に気液分離機構を有する請求項に記載の化学物質の処理装置。 7. The chemical substance treatment apparatus according to claim 6 , further comprising a gas-liquid separation mechanism between the slug flow generating device and the liquid-liquid separation mechanism. 前記気液分離機構の上部には圧力制御機構を備えた気体排出管が接続され、下部には前記液液分離機構に接続する液体排出管が接続されている請求項に記載の化学物質の処理装置。 8. The chemical substance treatment device according to claim 7 , wherein a gas discharge pipe equipped with a pressure control mechanism is connected to the upper part of the gas-liquid separation mechanism, and a liquid discharge pipe connected to the liquid-liquid separation mechanism is connected to the lower part. 逆止的に作動する吸引側の弁と吐出側の弁に挟まれた空間を画定する複数の筐体を有し、カムシャフトを用いた機械的な駆動方式により吸引と吐出を行う1台の往復動ポンプを用い、
複数の流体供給部と前記複数の筐体のそれぞれを接続する複数の吸引配管手段、及び前記複数の筐体のそれぞれと複数の流体の合流部を接続する複数の吐出配管手段を介して複数の流体を交互に間欠的に送液し、
前記合流部の下流に設けられた流体滞留部で前記複数の流体のスラグ流を生成する方法。
The pump has a plurality of housings that define a space between a suction-side valve and a discharge-side valve that operate in a check manner, and uses one reciprocating pump that performs suction and discharge using a mechanical drive system using a camshaft .
alternately and intermittently sending the plurality of fluids through a plurality of suction piping means connecting the plurality of fluid supply units to the plurality of housings, respectively, and a plurality of discharge piping means connecting the plurality of housings to a confluence of the plurality of fluids;
A method for generating slug flows of the plurality of fluids in a fluid retention section provided downstream of the confluence section.
請求項に記載のスラグ流を生成する方法を含む化学物質の処理方法。 A method for treating chemicals comprising the method for generating a slug stream according to claim 9 . 生成したスラグ流を液液分離する請求項10に記載の化学物質の処理方法。 11. The method for treating chemical substances according to claim 10 , wherein the resulting slug stream is subjected to liquid-liquid separation. 生成したスラグ流を気液分離してから液液分離する請求項11に記載の化学物質の処理方法。 12. The method for treating a chemical substance according to claim 11 , wherein the generated slug stream is subjected to gas-liquid separation and then liquid-liquid separation. 前記気液分離された気体に背圧を加えて流体全体の圧力を制御する請求項12に記載の化学物質の処理方法。 The method for treating a chemical substance according to claim 12 , wherein a back pressure is applied to the gas separated from the liquid to control the pressure of the entire fluid.
JP2021090993A 2021-05-31 2021-05-31 Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow Active JP7720558B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2021090993A JP7720558B2 (en) 2021-05-31 2021-05-31 Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2021090993A JP7720558B2 (en) 2021-05-31 2021-05-31 Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow

Publications (2)

Publication Number Publication Date
JP2022183588A JP2022183588A (en) 2022-12-13
JP7720558B2 true JP7720558B2 (en) 2025-08-08

Family

ID=84437897

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2021090993A Active JP7720558B2 (en) 2021-05-31 2021-05-31 Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow

Country Status (1)

Country Link
JP (1) JP7720558B2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024150477A1 (en) * 2023-01-13 2024-07-18 株式会社トクヤマ Method for producing amino group-containing compound, method for separating amino group-containing compound, and apparatus for producing amino group-containing compound
CN120457138A (en) * 2023-01-13 2025-08-08 株式会社德山 Method for producing amino-containing compound, method for separating amino-containing compound, and device for producing amino-containing compound

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090023223A1 (en) 2005-03-08 2009-01-22 Authentix, Inc. Plug flow system for identification and authentication of markers
JP2014023981A (en) 2012-07-25 2014-02-06 Tokyo Institute Of Technology Microchannel device and microchannel
JP2015208718A (en) 2014-04-25 2015-11-24 大陽日酸株式会社 Gas-liquid reaction method and aminosilane production method
JP2020032346A (en) 2018-08-29 2020-03-05 公立大学法人大阪 Extraction apparatus and extraction method

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0523129U (en) * 1991-05-02 1993-03-26 サヌキ工業株式会社 Liquid detector
JPH0915115A (en) * 1995-06-27 1997-01-17 Sanuki Kogyo Kk Check valve for physical and chemical apparatus and liquid mixer employing the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090023223A1 (en) 2005-03-08 2009-01-22 Authentix, Inc. Plug flow system for identification and authentication of markers
JP2014023981A (en) 2012-07-25 2014-02-06 Tokyo Institute Of Technology Microchannel device and microchannel
JP2015208718A (en) 2014-04-25 2015-11-24 大陽日酸株式会社 Gas-liquid reaction method and aminosilane production method
JP2020032346A (en) 2018-08-29 2020-03-05 公立大学法人大阪 Extraction apparatus and extraction method

Also Published As

Publication number Publication date
JP2022183588A (en) 2022-12-13

Similar Documents

Publication Publication Date Title
JP7720558B2 (en) Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow
Zhao et al. Intensification of liquid-liquid two-phase mass transfer by oscillating bubbles in ultrasonic microreactor
EP1259316B1 (en) Capillary reactor distribution device and method
JP7320852B2 (en) Devices, systems, and methods for continuous production of nanomaterials and high-purity chemicals
CN103328092B (en) Vibration fluid micro-reactor
Yang et al. An Experimental study of copper extraction characteristics in a T‐junction microchannel
CN105013547B (en) Microbubble/drop formation regulation device and method
JP5749987B2 (en) Liquid mixing method and apparatus
US10449509B2 (en) Synthesis of organic peroxydes using an oscillatory flow mixing reactor
US20180050313A1 (en) Homogenization device
Mi et al. Ethylene/ethane absorption with AgNO3 solutions in ultrasonic microreactors
Wang et al. Microdispersion of gas or water in an anthraquinone working solution for the H2O2 synthesis process intensification
Singh et al. Hydrodynamics and mass transfer studies of liquid-liquid two-phase flow in parallel microchannels
Chen et al. Liquid-liquid extraction performance in a miniaturized magnetic extractor
CN204816577U (en) Novel microbubble / liquid drop generates regulation and control device
Liu et al. A novel approach to intensify fluid mixing by introducing a “pre‐cavitation” stage in an ultrasonic microreactor
Aljbour et al. Ultrasound-assisted capillary microreactor for aqueous–organic multiphase reactions
Zhang et al. Chlorohydrination of allyl chloride to dichloropropanol in a microchemical system
JP7704334B2 (en) Slug flow generating device, chemical substance treatment device equipped with said slug flow generating device, slug flow generating method, and chemical substance treatment method using slug flow
Luo et al. Experimental investigations of liquid-liquid dispersion in a novel helical tube reactor
Wang et al. Deep deoxidation of water in a miniaturized annular rotating device: Experimental investigation and machine learning modeling
Ji et al. Preparation of microdispersed droplets by phase inversion in gas/liquid/liquid microdispersion system
US20080175768A1 (en) Reaction apparatus
KR102919480B1 (en) Chemical reaction system and device suitable for small-volume flow reactions
JP2024162278A (en) Slug flow generating device, chemical substance processing device equipped with said slug flow generating device, slug flow generating method, and chemical substance processing method using said slug flow generating method

Legal Events

Date Code Title Description
A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20210628

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20210708

A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20240509

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20250122

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20250204

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20250403

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20250702

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20250717

R150 Certificate of patent or registration of utility model

Ref document number: 7720558

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150