WO2024150506A1 - フロー合成装置 - Google Patents

フロー合成装置 Download PDF

Info

Publication number
WO2024150506A1
WO2024150506A1 PCT/JP2023/039030 JP2023039030W WO2024150506A1 WO 2024150506 A1 WO2024150506 A1 WO 2024150506A1 JP 2023039030 W JP2023039030 W JP 2023039030W WO 2024150506 A1 WO2024150506 A1 WO 2024150506A1
Authority
WO
WIPO (PCT)
Prior art keywords
flow
measurement
flow path
slug
section
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.)
Ceased
Application number
PCT/JP2023/039030
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
大哲 吉田
太一 中村
瞭 宮
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.)
Panasonic Intellectual Property Management Co Ltd
Original Assignee
Panasonic Intellectual Property Management Co Ltd
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 Panasonic Intellectual Property Management Co Ltd filed Critical Panasonic Intellectual Property Management Co Ltd
Priority to JP2024570043A priority Critical patent/JPWO2024150506A1/ja
Publication of WO2024150506A1 publication Critical patent/WO2024150506A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity

Definitions

  • This disclosure relates to a flow synthesis apparatus, and more specifically, to a flow synthesis apparatus that produces a liquid containing fine particles by a reaction in the liquid phase.
  • Microflow synthesis is a method for precisely and continuously carrying out reactions in the liquid phase.
  • Microflow synthesis is a synthesis method in which multiple unit operations such as mixing and heating are carried out continuously in one go, and has a higher throughput than batch synthesis, a synthesis method in which each unit operation is carried out discontinuously in sequence using a reaction vessel.
  • microflow synthesis in order to prevent the occurrence of defective products in the manufacture of microparticles, it is necessary to detect the concentration of microparticles in the microparticle-containing liquid flowing inside the synthesis device and perform quality control.
  • An example of an analytical device that performs quality control through continuous optical measurement is the flow-type analytical absorbance detection device disclosed in Patent Document 1.
  • a flow synthesis apparatus includes a flow path, a liquid delivery section disposed upstream of the flow path and reacting two or more liquids to produce a microparticle-containing liquid and delivering the microparticle-containing liquid into the flow path, a slug flow former through which the microparticle-containing liquid delivered to the flow path passes in sequence along the flow path, a flow cell, a gas introduction section that introduces gas into the slug flow former, and a measurement section, the slug flow former merges the microparticle-containing liquid and the gas to form a slug flow and delivers it to the flow cell, and the measurement section measures the absorbance of the slug flow in the flow cell.
  • FIG. 1 is a schematic diagram showing an example of a configuration of a flow synthesis apparatus according to an embodiment of the present disclosure.
  • FIG. 2 is a top view showing an example of a configuration of a flow cell of the flow synthesis apparatus of FIG. 1, illustrating the configuration of a flow cell according to the first embodiment of the present disclosure.
  • FIG. 13 is a top view showing another example of the configuration of the flow cell of the flow synthesis apparatus of FIG. 1, which is a configuration of a flow cell according to Example 2 of the present disclosure.
  • FIG. 13 is a side view showing another example of the configuration of the flow cell of the flow synthesis apparatus of FIG. 1, which is a configuration of a flow cell according to Example 3 of the present disclosure.
  • FIG. 1 is a schematic diagram showing an example of a configuration of a flow synthesis apparatus according to an embodiment of the present disclosure.
  • FIG. 2 is a top view showing an example of a configuration of a flow cell of the flow synthesis apparatus of FIG. 1, illustrating the configuration of a flow cell
  • 13 is a top view showing the configuration of a flow cell according to a comparative example of the present disclosure.
  • 1 is a graph showing the measurement results of absorbance for a slug flow in a flow cell according to Example 1.
  • 13 is a graph showing the measurement results of absorbance for a slug flow in a flow cell according to Example 2.
  • 13 is a graph showing the measurement results of absorbance for a slug flow in a flow cell according to Example 3.
  • 13 is a graph showing the measurement results of absorbance for a microparticle-containing liquid in a flow cell according to a comparative example.
  • 1 is a table showing the evaluation results of continuous in-line measurement of the content concentration of ZIF-8 particles carried out in Examples 1-3 and Comparative Example.
  • the present disclosure aims to solve the above-mentioned problems of the related art by providing a flow synthesis device that can detect the concentration of microparticles in a microparticle-containing liquid flowing inside the synthesis device.
  • a flow synthesis device comprising a flow path, a liquid delivery section disposed upstream of the flow path, which reacts two or more liquids to produce a microparticle-containing liquid and delivers the microparticle-containing liquid into the flow path, a slug flow former through which the microparticle-containing liquid delivered into the flow path passes in sequence along the flow path, a flow cell, a gas introduction section which introduces gas into the slug flow former, and a measurement section, in which the slug flow former merges the microparticle-containing liquid and the gas to form a slug flow of the microparticle-containing liquid which is then delivered to the flow cell, and the measurement section irradiates the slug flow in the flow cell with light and measures absorbance.
  • slug flow refers to fluids with no affinity for each other, for example, in this disclosure, when liquid and gas flow simultaneously within a flow path, the liquid and gas are separated from each other by a phase interface, forming alternating "liquid cells” and “gas cells” that flow alternately alongside each other along the flow path.
  • a circulating flow occurs within the liquid cells, and this circulating flow creates a localized stirring action.
  • the "liquid cells” and “gas cells” referred to here are columnar liquid segments and gas segments, respectively, that flow alternately alongside each other within the flow path.
  • the flow cell includes a measurement flow path section, an upstream connection section, and a downstream connection section
  • the measurement flow path section has a first end on the upstream side and a second end on the downstream side
  • the slag flow introduced into the flow cell flows from the first end to the second end along a first direction and passes through the measurement flow path section
  • the upstream connection section connects the slag flow former and the upstream side of the measurement flow path section
  • the slag flow is introduced into the measurement flow path section via the upstream connection section
  • the downstream connection section is connected to the downstream side of the measurement flow path section
  • the slag flow that has passed through the measurement flow path section is discharged via the downstream connection section
  • light is incident on the slag flow in the measurement flow path section at the first end
  • light that has passed through the slag flow in the measurement flow path section is emitted at the second end
  • the upstream connection section is configured to guide the slag
  • a flow synthesis apparatus as described in the second aspect, in which the first angle is greater than or equal to 0 degrees and less than or equal to 90 degrees.
  • a flow synthesis device as described in the second or third aspect, in which the measurement flow path section is arranged such that the first direction forms a second angle with the vertical direction, and the second angle is 90 degrees or less.
  • a flow synthesis apparatus as described in the fourth aspect, in which the second angle is 5 degrees or less.
  • a flow synthesis apparatus according to any one of the first to fifth aspects, in which the gas introduction section is positioned so as to introduce gas into the slug flow former from a direction intersecting the flow of the microparticle-containing liquid fed by the liquid delivery section.
  • a flow synthesis apparatus according to any one of the first to sixth aspects, further comprising a control unit electrically connected to the gas introduction unit and the measurement unit, the control unit controlling the gas introduction from the gas introduction unit based on a measurement signal of the absorbance of the slug flow in the flow cell.
  • Fig. 1 is a schematic diagram showing an example of the configuration of a flow synthesis apparatus 100 according to an embodiment of the present disclosure.
  • the flow synthesis apparatus 100 shown in Fig. 1 includes a flow path 10, a liquid delivery section 20, a gas introduction section 30, a slug flow former 40, a flow cell 60, a measurement section 70, a control section 80, and a collection container 90.
  • the flow synthesis apparatus 100 can be used to react two or more liquids to generate a microparticle-containing liquid.
  • the liquid delivery section 20 includes a liquid supply section 22 and a mixing and reaction section 24, and is used to react two or more liquids to produce a liquid containing fine particles.
  • the liquid supply unit 22 may be configured with a liquid delivery device such as a syringe pump, plunger pump, diaphragm pump, tube pump, mono pump, or piezo pump (not shown) as long as it is capable of delivering multiple liquids.
  • a liquid delivery device such as a syringe pump, plunger pump, diaphragm pump, tube pump, mono pump, or piezo pump (not shown) as long as it is capable of delivering multiple liquids.
  • the mixing and reaction section 24 only needs to be able to mix and react multiple liquids, and can be constructed, for example, from a flow path connection member made by bonding or stacking and fixing multiple flat plates to a flat plate with grooves, through holes, etc., and a union tee or manifold as a piping joint.
  • FIG. 1 shows an example in which two types of liquid are mixed and reacted, but the present disclosure is not limited to this. Three or more types of liquid can be supplied by the liquid supply unit 22 and reacted in the mixing and reaction unit 24.
  • the microparticle-containing liquid 25 generated in the liquid delivery section 20 is sent to the flow path 10 along the direction A3 shown in the figure. Note that, in the embodiment shown in FIG. 1, only the flow path 10 is shown as being connected to the outlet of the mixing and reaction section 24, but the present disclosure is not limited to this. For example, multiple branch flow paths (not shown) may be connected to the outlet of the mixing and reaction section 24, and a portion of the generated microparticle-containing liquid 25 may be sent to the flow path 10.
  • the microparticle-containing liquid 25 sent from the liquid delivery section 20 to the flow path 10 flows downstream along the flow path 10 and reaches the slug flow former 40.
  • the slug flow former 40 is connected to the gas introduction section 30.
  • the gas introduction section 30 is used to introduce gas for forming a slag flow into the slag flow former 40.
  • the gas introduction section 30 can be provided with, for example, a syringe pump (not shown), and a predetermined amount of gas can be pumped to the slag flow former 40 through a pipe (not shown) by the pressure of the syringe pump.
  • the gas introduction section 30 can also be provided with a flow rate adjustment means for feeding the gas, for example, a gas flow regulator (not shown) such as a mass flow controller or a needle valve connected to the pipe.
  • the gas flow regulator of the gas introduction section 30 is electrically connected to the control section 80, and operates under the control of the control section 80, thereby controlling the introduction of gas into the slag flow former 40. This will be described in detail later.
  • the slug flow former 40 is configured to merge the microparticle-containing liquid 25 fed from the liquid feed section 20 with the gas introduced by the gas introduction section 30 to form a slug flow of the microparticle-containing liquid.
  • the slug flow former 40 can be configured, for example, with a union tee or manifold as a piping joint, and a flow path connection member made by bonding or stacking and fixing a plurality of flat plates to a flat plate provided with grooves or through holes. It can also include a flow path switching device such as an electromagnetic switching valve that introduces gas into the flow path at regular intervals.
  • the gas introduction section 30 is arranged to introduce gas for forming a slug flow into the slug flow former 40 from a direction B intersecting the flow direction A3 of the microparticle-containing liquid 25 fed by the liquid delivery section 20.
  • the gas introduced in this manner merges with the microparticle-containing liquid 25 in the slug flow former 40 to form a slug flow 50 of the microparticle-containing liquid in which liquid cells and gas cells flow alternately side-by-side.
  • the slug flow 50 of the microparticle-containing liquid formed in the slug flow former 40 flows further downstream along the flow path 10 in the direction C1 from the slug flow former 40 and is introduced into the flow cell 60.
  • the slug flow former 40 and the flow cell 60 may be connected by a pipe joint (not shown) or the like provided in the flow path 10.
  • the configuration of the flow cell 60 and the introduced slug flow 50 of the microparticle-containing liquid will be described with reference to FIG. 2.
  • Fig. 2 is a top view showing an example of the configuration of a flow cell of the flow synthesis apparatus 100 of Fig. 1, and shows the configuration of a flow cell 60 according to the first embodiment of the present disclosure.
  • the flow cell 60 shown in Fig. 2 can be composed of a measurement flow path section 61, an upstream connection section 66, and a downstream connection section 67.
  • the flow cell 60 shown in Fig. 2 is disposed on an XY plane perpendicular to the vertical direction G.
  • the measurement flow path section 61 of the flow cell 60 has a first end 62 on the upstream side and a second end 63 on the downstream side.
  • the slug flow 50 is introduced into the upstream side of the measurement flow path section 61 via the upstream connection section 66 and flows from the first end 62 to the second end 63 along the direction C2, passing through the measurement flow path section 61.
  • the measurement section 70 irradiates light onto the slug flow 50 passing through the measurement flow path section 61 and measures the absorbance.
  • the measurement section 70 will be described in detail later.
  • the measurement flow path section 61 is configured so that light emitted by the measurement section 70 enters at the first end 62, and light that has passed through the slug flow 50 in the measurement flow path section 61 exits at the second end 63.
  • the first end 62 and the second end 63 can be configured to transmit light from a light source used in the absorbance measurement, and for example, openings can be provided.
  • the first end 62 and the second end 63 can be made of a light-transmitting material, such as a glass material such as quartz glass or borosilicate glass, or a resin material such as polyvinyl chloride or polypropylene.
  • This disclosure is not limited to the dimensions or cross-sectional shape of the measurement flow channel section 61.
  • the length and cross-sectional area of the measurement flow channel section 61 can be set according to the application, and the first end 62 and the second end 63 can be configured in any shape.
  • Light for measuring absorbance can be input or output, for example, via optical fibers coupled to the first end 62 and the second end 63.
  • the upstream connection 66 of the flow cell 60 is connected to the outlet of the slug flow former 40 (not shown in FIG. 2) and the upstream side of the measurement flow path section 61.
  • the slug flow 50 is introduced from the slug flow former 40 through the upstream connection 66 along the introduction direction C1 to the upstream side of the measurement flow path section 61.
  • the upstream connection 66 is configured to guide the slug flow 50 to the upstream side of the measurement flow path section 61 so that the introduction direction C1 of the slug flow 50 and the flow direction C2 of the slug flow 50 in the measurement flow path section 61 form an angle ⁇ .
  • the downstream connection part 67 of the flow cell 60 is connected to the downstream side of the measurement flow path part 61.
  • the slug flow 50 that has passed through the measurement flow path part 61 is discharged through the downstream connection part 67 along the discharge direction C3, flows into the collection container 90, and is collected (see FIG. 1).
  • the downstream connection part 67 may be provided with a connection means such as a pipe joint and connected to the collection container 90.
  • the downstream connection section 67 is configured to discharge the slag flow 50 from the downstream side of the measurement flow channel section 61 such that the discharge direction C3 of the slag flow 50 forms an angle ⁇ with the flow direction C2 of the slag flow 50 within the measurement flow channel section 61.
  • the present disclosure is not limited to the discharge direction C3 of the slag flow 50.
  • FIG. 2 shows the angles ⁇ and ⁇ to be generally the same, the present disclosure is not limited thereto. The angles ⁇ and ⁇ may be different angles, and the discharge direction C3 of the slag flow 50 may be set to any direction depending on the use.
  • FIG. 2 shows an example of the state of the slug flow 50.
  • the slug flow 50 includes liquid cells 51a, 51b, and 51c and gas cells 52a and 52b.
  • the liquid cells 51a, 51b, and 51c and the gas cells 52a and 52b are arranged alternately along the measurement flow path section 61 and flow in the direction C2.
  • a circulating flow 55 is generated within the liquid cell, creating a localized stirring action. This makes it difficult for the microparticles in the liquid cell of the slug flow 50 to settle.
  • the surface tension of the liquid cell makes it difficult for the microparticles to leave the liquid cell, it is possible to prevent the microparticles from accumulating and adhering to the inner wall of the flow cell 60. This makes it possible to detect the concentration of microparticles in the microparticle-containing liquid flowing within the flow cell 60.
  • the concentration of microparticles in the microparticle-containing liquid is detected by measuring the absorbance of the slug flow 50 in the measurement flow path section 61 of the flow cell 60.
  • the upstream connection part 66 of the flow cell 60 is configured so that the angle ⁇ between the introduction direction C1 of the slug flow and the flow direction C2 in the measurement flow path part 61 is greater than or equal to 0 degrees and less than or equal to 90 degrees. This makes it possible to suppress changes in the flow direction when the slug flow is introduced into the measurement flow path part 61, and to achieve more stable absorbance measurements.
  • the measurement flow path section 61 can be arranged so that the flow direction C2 of the slug flow 50 forms an angle of 90° or less, preferably 45° or less, and more preferably 5° or less with respect to the vertical direction.
  • This makes it possible to utilize gravity to further reduce the settling of fine particles in the slug flow 50 flowing in the measurement flow path section 61, and to prevent the accumulation and adhesion of fine particles at the ends where the light for measuring absorbance enters and exits. In this way, more accurate absorbance measurement can be achieved. This will be further explained later with reference to FIG. 4 showing the configuration of a flow cell according to Example 3.
  • the measurement unit 70 can detect the concentration of microparticles in the microparticle-containing liquid by performing optical measurement on the slug flow 50 in the flow cell 60.
  • the measurement unit 70 is configured to irradiate light onto the slug flow 50 in the measurement flow path section 61 of the flow cell 60 and measure the absorbance.
  • the measurement unit 70 may include, for example, a light source unit and a light receiving unit.
  • the light source unit (not shown) of the measurement unit 70 may include, but is not limited to, a light source such as an LED, a halogen lamp, or a deuterium lamp, and a spectrometer, and may be provided with a darkroom unit to block light from outside.
  • the light emitted from the light source unit is incident on the first end 62 of the measurement flow path unit 61 of the flow cell 60 via, for example, an optical fiber (not shown), and irradiates the slug flow 50 in the measurement flow path unit 61.
  • the present disclosure is not limited to the wavelength or power of the light of the light source unit.
  • the wavelength and power of the light used for the absorbance measurement can be set according to the type of microparticle-containing liquid to be measured.
  • the light receiving section (not shown) of the measurement section 70 may be, but is not limited to, a CCD or CMOS that detects light in the visible light range, or a diode array detector (DAD) that detects light in a wider wavelength range.
  • the light incident on the first end 62 of the measurement flow path section 61 and the light that passes through the slug flow 50 and exits from the second end 63 are detected by the light receiving section via, for example, an optical fiber (not shown), and the light receiving section can be configured to convert the detected optical signal into an electrical signal to obtain absorbance data.
  • the absorption and scattering of incident light changes depending on the particle size and dispersion concentration of the microparticles, so by irradiating the microparticle-containing liquid with light, measuring the intensity of the incident light and the transmitted light, and obtaining the absorbance, the microparticle concentration in the microparticle-containing liquid can be quantitatively derived.
  • the flow synthesis apparatus 100 of this embodiment can further include a control unit 80.
  • the control unit 80 can control the ratio of liquid cells and gas cells contained in the slug flow 50 in the measurement flow path section 61 so as to obtain a stable absorbance measurement signal.
  • control unit 80 is composed of an electronic control device such as a programmable logic controller (PLC) or a personal computer, and is electrically connected to the gas introduction unit 30 and the measurement unit 70.
  • a measurement signal of the absorbance of the slug flow in the flow cell 60 acquired by the measurement unit 70 is transmitted to the control unit 80.
  • the transmission of the measurement signal may be achieved by a wired connection or a wireless connection.
  • the control unit 80 can control, for example, the gas introduction of the gas introduction unit 30 so that the measurement signal of the absorbance of the slug flow is constant.
  • a gas flow regulator (not shown) of the gas introduction section 30 is electrically connected to the control section 80 and operates under the control of the control section 80, thereby controlling the amount of gas introduced into the microparticle-containing liquid. This makes it possible to adjust the ratio of liquid cells and gas cells contained in the slug flow 50 in the measurement flow path section 61 within a predetermined range, thereby achieving stable absorbance measurement.
  • FIG. 1 shows the control unit 80 connected to the gas introduction unit 30 and the measurement unit 70
  • the present disclosure is not limited to this.
  • the control unit 80 can also be configured to be further connected to the liquid delivery unit 20 and control the delivery of the microparticle-containing liquid to the flow path 10.
  • the flow synthesis apparatus 100 can suppress the settling of microparticles in the microparticle-containing liquid, or the accumulation and adhesion of microparticles on the inner wall of the flow cell, by introducing a slug flow of the microparticle-containing liquid into the flow cell 60. By measuring the absorbance of the slug flow in the flow cell 60, the concentration of microparticles in the microparticle-containing liquid can be detected.
  • the concentration of microparticles in the microparticle-containing liquid flowing within the synthesis apparatus can be continuously measured during microflow synthesis. Therefore, continuous in-line measurements can be performed without the need to interrupt the production of microparticles. This minimizes the occurrence of defective products during microparticle production, enabling continuous in-line quality control.
  • Fig. 3 is a top view showing another example of the configuration of the flow cell of the flow synthesis apparatus 100 of Fig. 1, and a configuration of a flow cell 60a according to Example 2 of the present disclosure.
  • Fig. 4 is a side view showing another example of the configuration of the flow cell of the flow synthesis apparatus 100 of Fig. 1, and a configuration of a flow cell 60b according to Example 3 of the present disclosure.
  • Fig. 5 is a top view showing a configuration of a flow cell 60c according to a comparative example of the present disclosure. Note that in Figs. 2 to 5, similar elements are given the same reference numerals, and descriptions of duplicated contents are omitted.
  • the liquid supply section 22 used two Flom plunger pumps (UI-22-110) as liquid supply pumps.
  • the mixing and reaction section 24 used a Flom three-way joint with an inner diameter of 0.3 mm, which was connected to each of the liquid supply pumps in the liquid supply section 22 with a tube with an inner diameter of 1 mm and made of PAF.
  • the gas introduction section 30 was a syringe pump (ULTRA) manufactured by HARVARD Apparatus with a syringe filled with nitrogen attached.
  • ULTRA syringe pump
  • the slug flow former 40 was a 3-way joint with an inner diameter of 1 mm manufactured by Flom, and the measurement unit 70 was a FLAME-T-TR manufactured by Ocean Photonics.
  • the control unit 80 connected a computer to the measurement unit 70 and the gas introduction unit 30, and controlled the gas introduction based on the absorbance measurement signal.
  • microflow synthesis and absorbance measurements carried out in the examples and comparative examples In Examples 1 to 3 and the Comparative Example, microflow synthesis of the metal-organic framework ZIF-8 was carried out under the same reaction conditions, and absorbance measurement was performed.
  • each liquid supply pump in the liquid supply section 22 supplied two types of reaction liquid so that the flow rate was 2 mL/min, and in the mixing and reaction section 24, the two types of reaction liquid were mixed and reacted, and the resulting ZIF-8 particle-containing liquid was sent to the flow path 10.
  • the measurement unit 70 set the wavelength of the FLAME-T-TR spectrometer to 500 nm.
  • the absorbance signal detected by the spectrometer was continuously acquired at 1 second intervals to continuously measure the absorbance of the ZIF-8 particle-containing liquid during the production of ZIF-8 particles.
  • the control unit 80 controlled the syringe pump of the gas introduction unit 30 and set the nitrogen introduction flow rate of the gas introduction unit 30 to 3.5 mL/min so that the ratio of liquid cells and gas cells contained in the slug flow in the measurement flow path unit 61 was constant.
  • the flow cell 60 according to Example 1 of the present disclosure has the configuration described above and shown in FIG. 2.
  • the measurement flow path section 61, the upstream connection section 66, and the downstream connection section 67 of the flow cell 60 were fabricated by forming a flow path in two PEEK resin plates and bonding them together.
  • the first end 62 and the second end 63 of the measurement flow path section 61 were each fabricated by bonding borosilicate glass with a thickness of 1 mm to the measurement flow path section 61.
  • Example 1 As shown in FIG. 2, the flow cell 60 was placed on an XY plane perpendicular to the vertical direction G.
  • the upstream connection portion 66 of the measurement flow path portion 61 was configured to guide the slug flow 50 to the measurement flow path portion 61 so that the angle ⁇ was 45 degrees. Note that the flow cell 60 in Example 1 had an angle ⁇ of approximately 45 degrees.
  • the flow cell 60a according to Example 2 of the present disclosure is shown in Figure 3.
  • the flow cell 60a used was an FIA-Z-SMA flow cell manufactured by Ocean Insight.
  • the flow cell 60a was disposed on an XY plane perpendicular to the vertical direction G, and was configured similarly to the flow cell 60 according to Example 1, except for the configuration of the upstream connection part 66a and downstream connection part 67a of the measurement flow path part 61a.
  • Example 2 as shown in FIG. 3, the upstream connection portion 66a of the measurement flow path portion 61a was configured to guide the slug flow 50 to the upstream side of the measurement flow path portion 61a so that the angle ⁇ 1 was 135 degrees. Note that the flow cell 60a in Example 2 had an angle ⁇ 1 of approximately 135 degrees.
  • flow cell 60b according to Example 3 of the present disclosure is shown in FIG. 4.
  • flow cell 60b is configured similarly to flow cell 60 according to Example 1, but is arranged so that the flow direction C2 of slug flow 50 in measurement flow passage section 61b is vertical G.
  • the flow cell 60c according to the comparative example of the present disclosure is shown in FIG. 5.
  • the flow cell 60c was configured similarly to the flow cell 60a according to Example 2.
  • the set flow rate of the gas introduction section 30 was set to 0 ml/min, no slug flow was formed, and the ZIF-8 particle-containing liquid 50a in which no slug flow was formed was introduced into the measurement flow path section 61c of the flow cell 60c.
  • FIG. 6 is a graph showing the results of the absorbance measurements for the slug flow in the flow cell in Example 1
  • Figure 7 is a graph showing the results of the absorbance measurements for the slug flow in the flow cell in Example 2
  • Figure 8 is a graph showing the results of the absorbance measurements for the slug flow in the flow cell in Example 3.
  • Figure 9 is a graph showing the results of the absorbance measurements for the microparticle-containing liquid in the flow cell in Comparative Example.
  • Figure 10 is a table showing the evaluation results of the continuous in-line measurement of the content concentration of ZIF-8 particles carried out in Examples 1-3 and Comparative Example.
  • the absorbance measurement data obtained was evaluated as the results of continuous in-line measurement of the concentration of ZIF-8 particles.
  • the standard deviation of the absorbance measurement value was less than 0.003, it was rated as "very good”, if the standard deviation was 0.003 or more and less than 0.05, it was rated as "good”, and if the standard deviation was 0.05 or more or the measurement could not be performed, it was rated as "poor”.
  • Example 1 and Example 2 obtained good results in the continuous in-line measurement of the content concentration of ZIF-8 particles. It was also found that the standard deviation value of the absorbance measurement value in Example 1, 0.0031, was smaller than the standard deviation value of the absorbance measurement value in Example 2, 0.0177. As shown in Figure 2, in Example 1, the flow cell 60 was configured so that the upstream connection part 66 of the measurement flow path part 61 guides the slug flow 50 to the measurement flow path part 61 so that the angle ⁇ is 45 degrees.
  • Example 3 the standard deviation value of the absorbance measurement value was 0.0015, which was the smallest in the continuous in-line measurement of the concentration of ZIF-8 particles, and very good results were obtained.
  • the flow cell 60b was positioned so that the flow direction C2 of the slug flow 50 in the measurement flow path section 61b was vertical direction G. This further reduces the settling of fine particles in the slug flow 50 flowing in the measurement flow path section 61b, and prevents the accumulation and adhesion of fine particles at the ends where the light for measuring absorbance enters and exits. Therefore, it was possible to perform continuous in-line measurement of the concentration of fine particles more stably.
  • the measurement flow path section 61c of 60c was washed with pure water, and then absorbance measurement was attempted with the measurement flow path section 61c filled with pure water, but the absorbance measurement value remained increased. It was found that the state in which fine particles were attached to the measurement flow path section 61c or both ends 62c, 63c of the measurement flow path section 61c was not improved, and in-line measurement of the content concentration of ZIF-8 particles was still impossible to perform.
  • This disclosure is applicable to the production of fine particles using reactions in the liquid phase.
  • This disclosure is applicable to the production of, for example, various inorganic particles, polymers, proteins, etc.

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
PCT/JP2023/039030 2023-01-11 2023-10-30 フロー合成装置 Ceased WO2024150506A1 (ja)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2024570043A JPWO2024150506A1 (https=) 2023-01-11 2023-10-30

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2023002668 2023-01-11
JP2023-002668 2023-01-11

Publications (1)

Publication Number Publication Date
WO2024150506A1 true WO2024150506A1 (ja) 2024-07-18

Family

ID=91896852

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2023/039030 Ceased WO2024150506A1 (ja) 2023-01-11 2023-10-30 フロー合成装置

Country Status (2)

Country Link
JP (1) JPWO2024150506A1 (https=)
WO (1) WO2024150506A1 (https=)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006043642A1 (ja) * 2004-10-20 2006-04-27 Ebara Corporation 流体反応装置
JP2007254176A (ja) * 2006-03-20 2007-10-04 Ymc Co Ltd 微粒子製造方法、微粒子製造に用いるスタティックミキサー及びスタティックミキサーを用いた複数の流体の混合方法。
JP2013006130A (ja) * 2011-06-22 2013-01-10 Kobe Steel Ltd 液体混合方法及び装置
WO2014157282A1 (ja) * 2013-03-26 2014-10-02 積水メディカル株式会社 フロー式分析用吸光度検出装置及びフロー式分析装置
WO2016031527A1 (ja) * 2014-08-29 2016-03-03 株式会社ダイセル 酸化反応装置、及び酸化物の製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006043642A1 (ja) * 2004-10-20 2006-04-27 Ebara Corporation 流体反応装置
JP2007254176A (ja) * 2006-03-20 2007-10-04 Ymc Co Ltd 微粒子製造方法、微粒子製造に用いるスタティックミキサー及びスタティックミキサーを用いた複数の流体の混合方法。
JP2013006130A (ja) * 2011-06-22 2013-01-10 Kobe Steel Ltd 液体混合方法及び装置
WO2014157282A1 (ja) * 2013-03-26 2014-10-02 積水メディカル株式会社 フロー式分析用吸光度検出装置及びフロー式分析装置
WO2016031527A1 (ja) * 2014-08-29 2016-03-03 株式会社ダイセル 酸化反応装置、及び酸化物の製造方法

Also Published As

Publication number Publication date
JPWO2024150506A1 (https=) 2024-07-18

Similar Documents

Publication Publication Date Title
JP5008815B2 (ja) プロセス材料を混合する方法及び装置
US10987649B2 (en) Microreactor system
EP2345476B1 (en) Method and apparatus for monitoring polyolefin production
Saerens et al. Process monitoring and visualization solutions for hot-melt extrusion: a review
JP7116975B2 (ja) 逸脱処理装置及び逸脱処理方法
CN118731405B (zh) 一种快速原样液体分流配送系统及其配送方法
WO2020076681A1 (en) A novel continuous flow reactor for low ph viral inactivation
WO2024150506A1 (ja) フロー合成装置
US12012471B2 (en) Device and methods to actively control the production of multi-stage polymer production
JP7296273B2 (ja) 重合体製造システム及び重合体製造方法
EP2554251A1 (en) Pipe type circulation-based reaction apparatus
CN114392712B (zh) 一种烯烃模试连续溶液聚合装置和工艺
JP2024098881A (ja) フロー合成装置およびフロー合成方法
CN1927440A (zh) 浆液或液体催化剂加料装置
JP7850933B2 (ja) 液体混合装置及び液体混合方法
CN106018317A (zh) 一种用于监测气体组分含量的系统及方法
CN206304709U (zh) 一种浆液或液体催化剂进料装置
CN223439803U (zh) 一种微反应装置和微反应系统
CN220951450U (zh) 一种基于釜式反应器的叠氮试剂废水连续淬灭装置
CN107115829B (zh) 激光引发的循环流化床生产氯化聚乙烯的装置及方法
US8059264B2 (en) Monitoring velocities in a polymerization process
CN206546309U (zh) 一种熔体在线粘度测量系统
CN221848657U (zh) 银粉湿法合成粒度智控系统
CN112516949A (zh) 具有产品分离功能的反应设备
CN118419870B (zh) 一种硫酸肼的制备方法及其制备装置

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 23916124

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 2024570043

Country of ref document: JP

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 23916124

Country of ref document: EP

Kind code of ref document: A1