WO2020230491A1 - 小流量フロー反応に適した化学反応システム及び装置 - Google Patents
小流量フロー反応に適した化学反応システム及び装置 Download PDFInfo
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Definitions
- the present invention relates to a method and an apparatus for bringing at least two kinds of liquids into contact, which are suitable for chemical reaction, liquid-liquid extraction, etc. in a flow with a small flow rate.
- Micro or millichemical process is a chemical process suitable for high-mix low-volume production. In particular, it is used for the production of pharmaceuticals and pharmaceutical intermediates, and the synthesis of organic compounds on a laboratory scale.
- Micro or millimeter chemical processes include micro or millimeter size reactors, micro or millimeter size separators (micro or millimeter size distillation columns, micro or millimeter size extractors, etc.), micro or millimeter size extractors. It consists of a mixer and a micro-sized or millimeter-sized pump.
- the characteristics of the equipment used in micro or millichemical processes are as follows: (1) The flow of fluid (gas, liquid) in the channel (inside the thin tube or in the narrow groove formed on the flat plate) is laminar flow ( 2) The surface area per unit volume of the fluid is large. If the flow is a laminar flow, liquid-liquid contact may not be sufficiently performed in an incompatible type 2 liquid or a highly viscous type 2 liquid.
- Patent Document 1 a liquid reaction medium containing a chlorinated hydrocarbon such as ethane dichloride as a main component is placed in a loop-type liquid circulation reactor, and ethylene and chlorine are introduced into the liquid reaction medium to react the liquid.
- a method for producing ethane dichloride while circulating a reaction medium ethane dichloride is characterized in that a liquid amount control valve for a liquid circulation flow path is provided and the liquid circulation flow rate is controlled in the range of 50 to 150 cm / sec. The manufacturing method is disclosed.
- Patent Document 2 describes a fixed bed reaction device filled with an immobilized enzyme and a two-phase separation tank for separating the reaction product obtained by the fixed bed reaction device into two phases, a low specific gravity product and a high specific gravity product.
- the formula two-phase immobilized enzyme reactor is disclosed.
- Patent Document 3 is a method for catalytically condensing at least one aldehyde in a two-phase liquid reaction mixture in a loop reactor, wherein the reactor is present in the reaction zone and immediately above it.
- an aldehyde-containing phase dispersed in a continuous aqueous phase containing a catalyst is generated, and the flow of the two-phase reaction mixture from the reaction zone is transferred to the quiescent zone.
- the method is disclosed in which a continuous organic phase is formed in the upper region of the quiescent zone by raising and integrating.
- Patent Document 4 a flow tube equipped with a mixing means or a loop reactor provided with a high-speed rotary pump for mixing is suitable for the continuous method, and the extraction process can also be performed by the same device. I teach you that you can.
- One of the objects of the present invention is to provide a method and an apparatus for bringing at least two kinds of liquids into contact with each other, which are suitable for chemical reaction, liquid-liquid extraction, etc. in a flow with a small flow rate.
- a homogeneous or non-uniform liquid consisting of at least two kinds of liquids is continuously supplied to a loop tube type container having a circulation flow path having a micro size or a millimeter size inside diameter via a supply flow path.
- the supplied liquid is circulated and circulated in the circulation flow path at a flow rate that becomes turbulent in the range from the connection part between the supply flow path and the circulation flow path to the connection part between the discharge flow path and the circulation flow path.
- the liquid is continuously withdrawn from the loop tube type container through the discharge flow path at a flow rate that satisfies the mass balance.
- a homogeneous or non-uniform liquid consisting of at least two kinds of liquids is passed through a supply flow path and placed in a loop tube type container having a circulation flow path having a micro-sized or millimeter-sized inner diameter at 0.01 to 500 cm.
- Continuously supplied at a flow rate of 3 / min The supplied liquid, be in the range up to the connecting portion between the discharge channel and the circulation passage from the connection portion between the supply channel and the circulation passage is calculated by R e ⁇ ⁇ ⁇ A / D H rate (m 3 / Second), circulate the circulation flow path, This includes continuously withdrawing the circulated liquid from the loop tube type container through the discharge flow path at a flow rate that satisfies the mass balance.
- Re is 1000 or more
- ⁇ (m 2 / sec) is the kinematic viscosity coefficient of the circulating liquid.
- a (m 2 ) is the area of the cross section of the circulation flow path from the connection portion between the supply flow path and the circulation flow path to the connection portion between the discharge flow path and the circulation flow path.
- DH (m) is the length calculated by 4 ⁇ A / P
- P (m) is the connection between the discharge flow path and the circulation flow path from the connection portion between the supply flow path and the circulation flow path. Perimeter of the cross section of the circulation flow path up to the part, A method of contacting at least two liquids.
- a loop tube type container having a circulation flow path having a micro-sized or millimeter-sized inner diameter. Connected to a circulation flow path for continuously supplying a homogeneous or non-uniform liquid consisting of at least two kinds of liquid to a loop tube reactor at a flow rate of 0.01 to 500 cm 3 / min.
- Discharge channel The supplied liquid, in the connecting portion between the supply channel and the circulation passage to the connecting portion between the discharge channel and the circulation passage, the flow rate calculated by R e ⁇ ⁇ ⁇ A / D H (m 3 / In seconds), it is connected to a positive displacement pump for flowing and circulating in the circulation flow path, and a circulation flow path for continuously extracting the circulated liquid from the loop tube type container at a flow rate that satisfies the mass balance.
- Discharge channel Equipped with Re is 1000 or more, ⁇ (m 2 / sec) is the kinematic viscosity coefficient of the circulating liquid.
- a (m 2 ) is the area of the cross section of the circulation flow path from the connection portion between the supply flow path and the circulation flow path to the connection portion between the discharge flow path and the circulation flow path.
- DH (m) is calculated as 4 ⁇ A / P
- P (m) is the circulating flow from the connection between the supply flow path and the circulation flow path to the connection part between the discharge flow path and the circulation flow path.
- liquid-liquid contact can be efficiently performed even in a flow with a small flow rate, so that it is suitable for chemical reactions and liquid-liquid extraction.
- the residence time can be arbitrarily set, a high reaction rate can be realized even in a chemical reaction having a slow reaction rate.
- the device of the present invention is compact and has excellent safety.
- the homogeneous liquid is a mixed liquid of at least two kinds of liquids having high compatibility with each other, such as water and methanol, water and acetone, and the like.
- the heterogeneous liquid is a liquid-liquid mixed phase liquid or emulsion (emulsion) of at least two liquids having high incompatibility with each other, such as water and oil, water and toluene, and the like. ..
- a heterogeneous liquid one liquid often forms a continuous phase and the other liquid often forms a dispersed phase.
- the micro size or the millimeter size refers to a size generally called by a person having ordinary knowledge in the art, for example, a size of 1 ⁇ m or more and less than 1000 mm, preferably a size of 10 ⁇ m or more and 100 mm or less. It is more preferably 100 ⁇ m or more and 50 mm or less, further preferably 0.3 mm or more and 10 mm or less, and further preferably 0.5 mm or more and 5 mm or less.
- the device of the present invention has a supply flow path 1, a loop tube type container, and a discharge flow path 5.
- the supply flow path 1 is a portion from a container for storing at least two kinds of liquids to a loop tube type container (hereinafter, may be referred to as a loop tube type reactor).
- the inner diameter of the supply flow path 1 is not particularly limited, but is preferably micro size or millimeter size.
- the supply flow path 1 is provided with a pump, an adsorption device, a dehydrator, a deaerator, a filter (filter cloth, etc.), a stirrer, a liquid conditioner, a temperature controller, a cooler, a heater, etc., as necessary. You may.
- a static mixing device also referred to as a static mixer
- the first liquid is supplied from the first reservoir (not shown) at a flow rate Q 1
- the second liquid is supplied from the second reservoir at a flow rate Q 2 (not shown)
- both solutions are mating at the merging portion 10, and flows into the circulation flow passage 3 out, 3 ret at a connection portion 2 at a flow rate Q F.
- a commercially available stirrer for example, Soda Engineering "Millireactor” or the like
- Soda Engineering "Millireactor” or the like may be used for the merging part 10 and the connecting part 2 in order to promote the mixing of the two liquids, or a device such as an ejector may be used. It may be provided.
- the ejector is a device that can suck in a low-pressure fluid (liquid or gas) by using the force of a high-pressure fluid and discharge it at a medium pressure. If the volume does not change with mixing, the flow rate Q F is the sum of the flow rate Q 1 and the flow rate Q 2 .
- the liquid dispenser is for combining at least two kinds of raw material liquids to obtain a homogeneous liquid or a non-uniform liquid consisting of at least two kinds of liquids.
- the liquid conditioner for combining at least two kinds of raw material liquids to obtain a homogeneous or non-uniform system liquid consisting of at least two kinds of liquids may be a simple confluence 10 formed by cheese or the like. It may be a mixer such as a microreactor or a millireactor, or it may be an emulsifier, a disperser or the like provided with a container and a stirring mechanism.
- the loop tube type reactor has a circulation flow path.
- the circulation flow path starts from the connection part 2 which is the part connected to the supply flow path 1, passes through the connection part 4 which is the part connected to the discharge flow path 5, and returns to the connection part 2 again, which is a loop type flow. It's a road.
- the range from the connection part 2 to the connection part 4 is referred to as the outward flow path 3 out
- the range from the connection part 4 to the connection part 2 is referred to as the return flow path 3 ret .
- the entire loop-type flow path is called a circulation flow path.
- the circulation flow path preferably has an inner diameter of at least the outward flow path 3 out of micro size or millimeter size, and the inner diameter of both the forward flow path 3 out and the return flow path 3 ret is micro size or millimeter size. More preferred.
- a pump, a filter (filter cloth, etc.), a stirrer, a cooler, a heater, a temperature controller, and the like may be provided in the circulation flow path, if necessary.
- the pump is preferably provided in the return channel 3 ret .
- the pump P is preferably a positive displacement pump because it can flow a liquid at an accurate flow rate.
- positive displacement pumps include reciprocating pumps such as piston pumps, plunger pumps and diaphragm pumps, and rotary pumps such as gear pumps, vane pumps and screw pumps. Of these, the plunger pump is preferable because it can handle a minute flow rate.
- a static mixing device is preferably used as the stirring device.
- a device such as an ejector 8 may be provided in the connection portion 2 in order to promote mixing of the liquid from the supply flow path 1 and the liquid from the return flow path 3 ret .
- a commercially available mixer for example, "Millireactor” manufactured by Nippon Soda Engineering Co., Ltd.
- Millireactor manufactured by Nippon Soda Engineering Co., Ltd.
- the filling material 9 can be packed in the circulation flow path, preferably in the outbound flow path 3 out (see FIG. 4).
- the filling can facilitate mixing.
- the filling may not contribute to the chemical reaction or may contribute to the chemical reaction. Examples of those that contribute to the chemical reaction include catalysts and adsorbents.
- the shape of the filling material is not particularly limited, and examples thereof include a granular shape, a needle shape, and a plate shape.
- the liquid's flow rate Q R of the outward passage 3 out if there is a change in volume ⁇ V by chemical reaction, and the flow rate Q F of the liquid from the supply channel 1, a return passage 3 ret and the flow rate Q c of the liquid from, which is the sum of the ⁇ V.
- the discharge flow path 5 is a flow path starting from the connection portion 4 and extending to the outside of the system of the apparatus of the present invention. If necessary, the discharge flow path 5 includes a pump, a gas-liquid separator, a liquid-liquid separator, an emulsifier, a filter (filter cloth), a stirrer, a temperature controller, a cooler, a heater, a damper, and a back. A pressure regulator or the like may be provided.
- the inner diameter of the discharge flow path 5 is not particularly limited, but is preferably micro size or millimeter size.
- the damper 12 can be appropriately used in order to suppress the pulsation generated by the reciprocating pump.
- the circulation flow path, the supply flow path 1, and the discharge flow path 5 are generally straight flow paths, but may be coil-shaped or zigzag-shaped flow paths.
- a homogeneous or non-uniform liquid consisting of at least two kinds of liquids is continuously passed through a supply flow path 1 into a loop tube type container having a circulation flow path having a micro-sized or millimeter-sized inner diameter.
- a circulation flow path having a micro-sized or millimeter-sized inner diameter.
- It includes circulating the circulation flow path at a turbulent flow rate and continuously extracting the circulated liquid from the loop tube type container through the discharge flow path 5 at a flow rate that satisfies the mass balance. ..
- the flow rate Q F of the liquid in the supply flow path 1 is determined by the supply amount of at least two liquid supplied from the reservoir, the flow conditions is a laminar flow It may be a turbulent flow.
- the laminar flow means a flow in which the fluid moves regularly, and in a straight pipe having a circular cross section, the flow line of the fluid is always parallel to the pipe axis.
- the flow rate Q R of the liquid in the outward passage 3 out is in the range of liquid flow in the outward passage 3 out becomes turbulent. Turbulence refers to a flow in which the velocity and pressure of a fluid fluctuate irregularly. Liquid-liquid contact is promoted by setting the flow rate to be turbulent.
- the flow rate Q F of the liquid in the supply flow path usually, 0.01 ⁇ 500 cm 3 / min, more preferably 0.1 ⁇ 100 cm 3 / min, more preferably 1 ⁇ 50 cm 3 / Set to minutes.
- the flow rate Q R of the liquid in the outward passage 3 out is set to a flow rate calculated by R e ⁇ ⁇ ⁇ A / D H (m 3 / sec). Re is 1000 or more, preferably 1300 or more, and more preferably 1800 or more.
- ⁇ (m 2 / sec) is the kinematic viscosity coefficient of the circulating liquid.
- a (m 2 ) is the area of the cross section of the circulation flow path from the connection portion 2 between the supply flow path 1 and the circulation flow path 3 to the connection portion 4 between the discharge flow path 5 and the circulation flow path 3.
- DH (m) is a length calculated by 4 ⁇ A / P, and P (m) is from the connection portion 2 between the supply flow path 1 and the circulation flow path 3 to the discharge flow path 5 and the circulation flow. It is the peripheral length of the cross section of the circulation flow path up to the connection portion 4 with the road 3.
- the liquid flow rate Q E in the exhaust passage 5 is a flow satisfying mass balance.
- the average residence time in the loop tube reactor is a value obtained by dividing the capacity of the circulation flow path by the flow rate Q F or Q E.
- Example 1 An experiment of liquid-liquid contact was carried out using the experimental apparatus shown in FIG. A spiral-shaped outward flow path 3 out consisting of a 1/8 inch tube (outer diameter 3.18 mm, inner diameter 2.17 mm) and a spiral diameter of 200 mm, and a return flow path 3 ret consisting of a 1/8 inch tube. A constructed circulation flow path having a capacity of 20 ml was prepared.
- Circulation pump 3B double plunger pump manufactured by Nippon Seimitsu Kagaku Co., Ltd., NP-HX-200, maximum discharge pressure 10 MPa
- pulsation damping damper 12 1/2 inch-PFA tube
- the supply flow path 1 was connected to the connection portion 2 between the inlet of the forward flow path 3 out and the outlet of the return flow path 3 ret .
- the discharge flow path 5 was connected to the connection portion 4 between the outlet of the forward flow path 3 out and the inlet of the return flow path 3 ret .
- a back pressure regulator nitrogen gas pressurization, inert gas seal pressure control automatic valve
- reaction rate (Q b + Q a ) / (Q 1B ) ⁇ 100.
- Q b Mass flow rate of 4-methoxyphenol in the discharged aqueous phase
- Q a Mass flow rate of 4-methoxyphenol in the discharged toluene phase
- Q 1B Mass flow rate of 4-methoxyphenol in the supplied aqueous solution 1B Flow rate
- Example 2 Except for changing the flow rate of the fluid supplied to the inlet of the outward passage 3 out through the return passage 3 ret from the outlet of the outward passage 3 out using a circulation pump to 50.0 ml / min to 100.0 ml / min , Liquid-liquid contact was carried out in the same manner as in Example 1.
- the Reynolds number in the outward flow path 3 out was 1240, and the average residence time in the circulation flow path was about 2 minutes.
- the reaction rate was 75.9% and the extraction rate was 53.2%.
- Example 3 Except for changing the flow rate of the fluid supplied to the inlet of the outward passage 3 out through the return passage 3 ret from the outlet of the outward passage 3 out using a circulation pump to 50.0 ml / min to 150.0 ml / min Liquid-liquid contact was performed in the same manner as in Example 1.
- the Reynolds number in the outward flow path 3 out was 1800, and the average residence time in the circulation flow path was about 2 minutes.
- the reaction rate was 100.0% and the extraction rate was 69.5%.
- Example 4 The experimental apparatus shown in FIG. 6 was used.
- a one-pass flow path 3 pr consisting of a 1/8 inch tube (outer diameter 3.18 mm, inner diameter 2.17 mm) having a spiral diameter of 200 mm and a spiral capacity of 20 ml was prepared.
- One-pass flow path 3 The supply flow path 1 was connected to the entrance of pr .
- the discharge flow path 5 was connected to the outlet of the flow path 3 pr .
- a back pressure regulator nitrogen gas pressurization, inert gas seal pressure control automatic valve
- Toluene solution 1A of 92ppm benzoic acid and aqueous solution 1B of 80ppm 4-methoxyphenol sodium salt were added at 5.0ml / min, respectively, to a pulseless flow plunger pump (NP-KX-500, manufactured by Nippon Seimitsu Kagaku Co., Ltd.).
- NP-KX-500 pulseless flow plunger pump
- the solution was continuously supplied to the one-pass flow path 3 pr via the supply flow path 1.
- the liquid that passed through the one-pass flow path 3 pr was continuously discharged through the discharge flow path 5 at 10 ml / min. Reynolds number in a single pass flow path 3 pr 110, the average residence time in the one-pass passage 3 pr was about 2 minutes.
- the reaction rate was 73.9% and the extraction rate was 50.0%.
- Example 5 In a separating funnel, 75 ml of a toluene solution of 92 ppm benzoic acid and 75 ml of an aqueous solution of 80 ppm of 4-methoxyphenol sodium salt were placed and shaken for about 2 to 3 minutes. Then, the separatory funnel was allowed to stand. The reaction rate was 78.3% and the extraction rate was 57.4%.
- the apparatus of the present invention is not limited to the embodiment shown in the drawings, and the shape, size, color, and material of each part constituting the apparatus of the present invention are changed, or the apparatus of the present invention is provided with well-known or commonly used parts. The additions are also included in the technical scope of the present invention.
- Supply flow path 2 Connection part between supply flow path and circulation flow path 3 out : Outward flow path 3 ret : Return flow path 4: Connection part between discharge flow path and circulation flow path 5: Discharge flow path 6, 7: In-line mixer 8: Ejector 9: Filling 10: Confluence P: Positive displacement pump 12: Pulsation damping damper 3B: Circulation pump 3 pr : One-pass flow path
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Abstract
Description
供給された液を、供給流路と循環流路との接続部から排出流路と循環流路との接続部までの範囲において乱流となる流量にて、循環流路を循環させ、且つ
循環させた液を、ループ管型容器から、排出流路を経て、マスバランスを満たす流量にて、連続的に抜き出すことを含む、
少なくとも2種の液を接触させる方法。
供給された液を、供給流路と循環流路との接続部から排出流路と循環流路との接続部までの範囲においてRe×ν×A/DHで算出される流量(m3/秒)にて、循環流路を循環させ、
循環させた液を、ループ管型容器から、排出流路を経て、マスバランスを満たす流量にて、連続的に抜き出すことを含み、
Reが、1000以上であり、
ν(m2/秒)が、循環させる液の動粘性係数であり、
A(m2)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の面積であり、
DH(m)が、4×A/Pで算出される長さであり、且つ
P(m)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の周長である、
少なくとも2種の液を接触させる方法。
〔4〕 少なくとも2種の液を合わせて、均一系若しくは不均一系の液を得ることをさらに含む、〔1〕、〔2〕または〔3〕に記載の方法。
少なくとも2種の液からなる均一系若しくは不均一系の液を、ループ管型反応器に、0.01~500cm3/分の流量にて、連続的に供給するための、循環流路に接続された供給流路、
供給された液を、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおいて、Re×ν×A/DHで算出される流量(m3/秒)にて、循環流路に流して循環させるための容積式ポンプ、および
循環させた液をループ管型容器からマスバランスを満たす流量にて連続的に抜き出すための、循環流路に接続された排出流路、
を具備し、
Reが、1000以上であり、
ν(m2/秒)が、循環させる液の動粘性係数であり、
A(m2)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の面積であり、
DH(m)が、4×A/Pで算出され、且つ
P(m)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の周長である、
少なくとも2種の液を接触させるための装置。
〔7〕 少なくとも2種の原料液を合わせて、少なくとも2種の液からなる均一系若しくは不均一系の液を得るための調液器をさらに具備する、〔5〕または〔6〕に記載の装置。
〔8〕 供給流路は、液を撹拌する機構を有する、〔5〕~〔7〕のいずれかひとつに記載の装置。
〔9〕 循環流路は、液を撹拌する機構を有する、〔5〕~〔8〕のいずれかひとつに記載の装置。
本発明の装置は、供給流路1と、ループ管型容器と、排出流路5とを有する。
供給流路1には、必要に応じて、ポンプ、吸着装置、脱水装置、脱気装置、フィルタ(濾布など)、撹拌装置、調液器、温度調節器、冷却器、加熱器などを設けてもよい。撹拌装置としては、静止型混合装置(スタティックミキサとも呼ばれる。)が好ましく用いられる。
図1に示す装置においては、第一液が流量Q1で第一貯留容器(図示せず)から供給され、第二液が流量Q2で第二貯留容器(図示せず)から供給され、両液が合流部10で合わさり、流量QFで接続部2にて循環流路3out,3retに流入している。合流部10および接続部2には、2液の混合を促進するために、市販の攪拌装置(例えば日曹エンジニアリング「ミリリアクター」等が挙げられる)を用いてもよいし、エジェクタ等の装置を設けてもよい。なお、エジェクタとは、高圧流体の力を利用し低圧の流体(液体や気体)を吸込んで、中圧にて排出することができる装置のことを言う。混合に伴って体積変化が生じない場合には、流量QFは流量Q1と流量Q2との合計である。調液器は、少なくとも2種の原料液を合わせて、少なくとも2種の液からなる均一系若しくは不均一系の液を得るためのものである。少なくとも2種の原料液を合わせて、少なくとも2種の液からなる均一系若しくは不均一系の液を得るための調液器は、チーズなどによって形成できる単なる合流部10であっても良いし、マイクロリアクター又はミリリアクターの様な混合器であっても良いし、容器と撹拌機構を具備する乳化器、分散器などであってもよい。
本発明の一つの実施態様において、往流路3outにおける液の流量QRは、往流路3outにおける液の流れが乱流となる範囲である。乱流とは、流体の速度や圧力などが不規則に変動する流れをいう。乱流となる流量とすることによって、液液接触が促される。
なお、Reは、1000以上、好ましくは1300以上、より好ましくは1800以上であり、
ν(m2/秒)は、循環させる液の動粘性係数であり、
A(m2)は、供給流路1と循環流路3との接続部2から排出流路5と循環流路3との接続部4までにおける循環流路の断面の面積であり、
DH(m)は、4×A/Pで算出される長さであり、且つ
P(m)は、供給流路1と循環流路3との接続部2から排出流路5と循環流路3との接続部4までにおける循環流路の断面の周長である。
(例1)
図5に示す実験装置を用いて液液接触の実験を行った。
1/8インチチューブ(外径3.18mm、内径2.17mm)からなる螺旋径が200mmである螺旋形状の往流路3outと、1/8インチチューブからなる復流路3retとで、構成された、容量20mlの循環流路を用意した。
復流路3retには、循環用ポンプ3B(日本精密科学(株)製ダブルプランジャーポンプ、NP-HX-200、最大吐出圧力10MPa)、および脈動減衰ダンパ12(1/2インチ-PFAチューブ(内径9mm))を取り付けた。往流路3outの入口と復流路3retの出口との接続部2に供給流路1を接続した。往流路3outの出口と復流路3retの入口との接続部4に排出流路5を接続した。排出流路5には、図示しないが、背圧調整器(窒素ガス加圧、不活性ガスシール圧制御自動弁)を取り付けた。
NaOC6H4OCH3 + C6H5COOH → HOC6H4OCH3 + C6H5COONa
4-メトキシフェノールはトルエンに溶解しやすく、安息香酸ナトリウムは水に溶解しやすいので、生成した安息香酸ナトリウムの一部はトルエン相から水相に移動し、生成した4-メトキシフェノールの一部は水相からトルエン相に移動した。
反応率は、式:反応率=(Qb+Qa)/(Q1B)×100 で算出した値である。
抽出率は、式:抽出率=(Qa)/(Q1B)×100 で算出した値である。
Qb=排出された水相中の4-メトキシフェノールの質量流量
Qa=排出されたトルエン相中の4-メトキシフェノールの質量流量
Q1B=供給した水溶液1B中の4-メトキシフェノール換算の質量流量
循環用ポンプを用いて往流路3outの出口から復流路3retを経て往流路3outの入口に供給する液の流量を50.0ml/分から100.0ml/分に変えた以外は、例1と同じ方法で液液接触を行った。往流路3outにおけるレイノルズ数は1240、循環流路における平均滞留時間は約2分であった。反応率は75.9%、抽出率は53.2%であった。
循環用ポンプを用いて往流路3outの出口から復流路3retを経て往流路3outの入口に供給する液の流量を50.0ml/分から150.0ml/分に変えた以外は例1と同じ方法で液液接触を行った。往流路3outにおけるレイノルズ数は1800、循環流路における平均滞留時間は約2分であった。反応率は100.0%、抽出率は69.5%であった。
図6に示す実験装置を用いた。
1/8インチチューブ(外径3.18mm、内径2.17mm)からなる螺旋径が200mmである螺旋形状の容量20mlのワンパス流路3prを用意した。
ワンパス流路3prの入口に供給流路1を接続した。流路3prの出口に排出流路5を接続した。排出流路には、図示しないが背圧調整器(窒素ガス加圧、不活性ガスシール圧制御自動弁)を取り付けた。
分液漏斗に、92ppmの安息香酸のトルエン溶液75mlと80ppmの4-メトキシフェノールナトリウム塩の水溶液75mlとを入れ、約2~3分間、振騰させた。その後、分液漏斗を静置した。反応率は78.3%、抽出率は57.4%であった。
2:供給流路と循環流路との接続部
3out:往流路
3ret:復流路
4:排出流路と循環流路との接続部
5:排出流路
6,7:インラインミキサ
8:エジェクタ
9:充填物
10:合流部
P:容積式ポンプ
12:脈動減衰ダンパ
3B:循環用ポンプ
3pr:ワンパス流路
Claims (9)
- 少なくとも2種の液からなる均一系若しくは不均一系の液を、供給流路を経て、内径がマイクロサイズまたはミリサイズの循環流路を有するループ管型容器に、連続的に供給し、
供給された液を、供給流路と循環流路との接続部から排出流路と循環流路との接続部までの範囲において乱流となる流量にて、循環流路を循環させ、且つ
循環させた液を、ループ管型容器から、排出流路を経て、マスバランスを満たす流量にて、連続的に抜き出すことを含む、
少なくとも2種の液を接触させる方法。 - 少なくとも2種の液からなる均一系若しくは不均一系の液を、供給流路を経て、内径がマイクロサイズまたはミリサイズの循環流路を有するループ管型容器に、0.01~500cm3/分の流量にて、連続的に供給し、
供給された液を、供給流路と循環流路との接続部から排出流路と循環流路との接続部までの範囲においてRe×ν×A/DHで算出される流量(m3/秒)にて、循環流路を循環させ、
循環させた液を、ループ管型容器から、排出流路を経て、マスバランスを満たす流量にて、連続的に抜き出すことを含み、
Reが、1000以上であり、
ν(m2/秒)が、循環させる液の動粘性係数であり、
A(m2)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の面積であり、
DH(m)が、4×A/Pで算出される長さであり、且つ
P(m)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の周長である、
少なくとも2種の液を接触させる方法。 - 供給流路および排出流路は、内径がマイクロサイズまたはミリサイズである、請求項1または2に記載の方法。
- 少なくとも2種の液を合わせて、均一系若しくは不均一系の液を得ることをさらに含む、請求項1、2または3に記載の方法。
- 内径がマイクロサイズまたはミリサイズの循環流路を有するループ管型容器、
少なくとも2種の液からなる均一系若しくは不均一系の液を、ループ管型反応器に、0.01~500cm3/分の流量にて、連続的に供給するための、循環流路に接続された供給流路、
供給された液を、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおいて、Re×ν×A/DHで算出される流量(m3/秒)にて、循環流路に流して循環させるための容積式ポンプ、および
循環させた液をループ管型容器からマスバランスを満たす流量にて連続的に抜き出すための、循環流路に接続された排出流路、
を具備し、
Reが、1000以上であり、
ν(m2/秒)が、循環させる液の動粘性係数であり、
A(m2)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の面積であり、
DH(m)が、4×A/Pで算出され、且つ
P(m)が、供給流路と循環流路との接続部から排出流路と循環流路との接続部までにおける循環流路の断面の周長である、
少なくとも2種の液を接触させるための装置。 - 供給流路および排出流路は、内径がマイクロサイズまたはミリサイズである、請求項5に記載の装置。
- 少なくとも2種の原料液を合わせて、少なくとも2種の液からなる均一系若しくは不均一系の液を得るための調液器をさらに具備する、請求項5または6に記載の装置。
- 供給流路は、液を撹拌する装置を有する、請求項5~7のいずれかひとつに記載の装置。
- 循環流路は、液を撹拌する装置を有する、請求項5~8のいずれかひとつに記載の装置。
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