Microchannel-based perfluorohexanone stable emulsion and preparation method thereof

Abstract

The invention provides a perfluorohexanone stable emulsion based on a microchannel and a preparation method thereof, and belongs to the technical field of fire extinguishing agent preparation. The perfluorohexanone stable emulsion is in an oil-in-water type, an outer water phase wraps an oil phase, the oil phase is a perfluorohexanone phase, and the preparation and regulation of the perfluorohexanone stable emulsion are realized by adjusting the injection pump rates of the water phase and the perfluorohexanone phase; and the water phase comprises the following components: a polysorbate surfactant, alkylphenol polyoxyethylene ether, polyvinyl alcohol, deionized water and glycerol. The stable perfluorohexanone emulsion prepared by the invention continuously absorbs heat when being in contact with a combustible material, and effective cooling is finally realized. When the environment temperature rises, the water and the perfluorohexanone are vaporized and expanded, the expanded water vapor and perfluorohexanone steam occupy a combustion area and weaken air supply, the local oxygen volume fraction is reduced, and therefore the combustion intensity is reduced, and finally fire extinguishing is achieved.

Description

Technical Field

[0001] This invention belongs to the field of fire extinguishing agent preparation technology, and relates to a microchannel-based perfluorohexanone stabilized emulsion and its preparation method. Background Technology

[0002] In the 21st century, with the continuous research on alternatives to halon fire extinguishing agents, fluorinated compounds have shown significant advantages. Among them, perfluorohexanone, as a representative fluorinated ketone fire extinguishing agent, combines good fire extinguishing performance with relatively environmentally friendly properties and is considered one of the alternatives to halon. This substance is a colorless, odorless, and low-toxicity liquid at room temperature, with a relative molecular mass of approximately 316.04 and a density of approximately 1.60 g·cm³. -3 Its fire extinguishing effect is mainly through endothermic cooling, accompanied by the generation of vapors that dilute and replace the combustion zone, thereby reducing flame temperature and oxygen supply. Furthermore, perfluorohexanone has environmental advantages such as low ozone depletion potential and a relatively short atmospheric lifetime.

[0003] Currently, the preparation of perfluorohexanone emulsions generally employs methods such as stirring, high shear, ultrasonication, or high-pressure homogenization. The high energy consumption leads to temperature gradients and solvation differences, resulting in a wide particle size distribution and amplified batch-to-batch variations in the prepared emulsion. To suppress aggregation and sedimentation, high amounts of surfactants and thickeners are often required. Due to the combined effects of density differences and interfacial tension, small-sized droplets are more prone to Austronesian ripening and aggregation, resulting in insufficient storage stability. This invention employs a microchannel emulsification method, controlling the droplet size through channel pore size, pipeline wettability, and flow ratio, thereby reducing surfactant usage and evaporation losses.

[0004] Perfluorohexanone has a high interfacial tension with water. Existing technologies generally use fluorinated surfactants as emulsifiers. Using such emulsifiers can form relatively stable microemulsions or nanoemulsions under certain conditions, but it faces problems such as high cost, strict environmental and regulatory constraints, and limited supply chain. This invention combines and optimizes non-fluorinated surfactants to achieve small particle size, low volatility, and long-term stability, while taking into account cost control and safety of use.

[0005] Invention CN 112546528 A proposes a perfluorohexanone stabilized emulsion and its preparation method, using hot melting and mixing to prepare the emulsion; however, the emulsion has a relatively long fire extinguishing time. Invention CN 119425003 A develops a fluorine-containing fire extinguishing microcapsule and its preparation method, which improves the coating effect on low-boiling-point fluoride core materials, but the use of fluorine-containing emulsifiers causes some environmental pollution.

[0006] Perfluorohexanone has a boiling point of 49.2 °C and is easily volatile at room temperature, requiring high sealing of containers during storage and transportation. Conventional liquid filling methods are prone to problems such as large evaporation losses and poor storage stability. This invention can maintain perfluorohexanone in a stable storage form at room temperature, solving the defects of existing technologies that make it difficult to store perfluorohexanone stably and pose significant risks in use. Summary of the Invention

[0007] To address the problems existing in the prior art, this invention provides a microchannel-based perfluorohexanone stable emulsion and its preparation method. The perfluorohexanone stable emulsion prepared by this invention can solve the problems of difficult stable storage and high risk of use of perfluorohexanone in the prior art.

[0008] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0009] A microchannel-based perfluorohexanone stabilized emulsion is prepared and controlled by adjusting the injection pump rates of the aqueous phase and the perfluorohexanone phase. The emulsion has an oil-in-water structure, with the outer aqueous phase encapsulating the oil phase perfluorohexanone, and the overall emulsion is milky white.

[0010] The aqueous phase is formulated with the following proportions: 3.55%–8.91% polysorbate surfactant, 0.45%–5.89% alkylphenol polyoxyethylene ether, 0.05%–3.55% polyvinyl alcohol, 62.09%–83.40% deionized water, and 12.55%–19.56% glycerol. The sum of the mass percentages of the above components is 100%. The aqueous phase is obtained after all components are stirred evenly.

[0011] The perfluorohexanone phase is a perfluorohexanone solution with a purity of 99.9%;

[0012] Furthermore, the polysorbate surfactant is one or more of polysorbate 20, 21, 40, 60, 61, 65, 80, 81, 85, and 120 surfactants;

[0013] Furthermore, the glycerol used in the aqueous phase configuration can be replaced with propylene glycol.

[0014] A method for preparing a microchannel-based perfluorohexanone-stabilized emulsion includes the following steps:

[0015] The first step is to prepare microchannels;

[0016] The microchannel described is a Y-shaped structure, comprising two branches and a main channel;

[0017] The interfaces of the two branches of the Y-shaped structure are respectively connected to syringe A and syringe B;

[0018] The Y-shaped main pipe is filled with solid beads.

[0019] The second step is to mix the components of the aqueous phase and stir until homogeneous.

[0020] The third step is to prepare the perfluorohexanone phase;

[0021] The fourth step is to prepare a perfluorohexanone-stabilized emulsion;

[0022] Syringe A contains an aqueous solution, and syringe B contains a perfluorohexanone solution. By controlling the flow rates of the perfluorohexanone and aqueous phases, the two phases mix at the Y-shaped tee before entering the main pipeline, where the perfluorohexanone microemulsion is prepared. A one-way filter valve is connected to the Y-shaped tee. The main pipeline connected to the one-way filter valve is filled with solid beads. The one-way filter valve calibrates and standardizes the droplet size, and the solid beads generate controllable shear force and extrusion to initially form droplets. A one-way filter valve is also connected to the outlet of the main pipeline, where high-speed shearing completes the emulsion preparation.

[0023] Furthermore, in the first step, the diameter of the two branches of the Y-shaped structure and the main pipeline is 1.6mm to 3.2mm, and the material is Teflon transparent tubing.

[0024] Furthermore, the solid spheres filling the main pipe have a diameter of 1mm to 5mm, a number of 1000 to 2000, and a main pipe length of 1m to 5m.

[0025] Furthermore, in the second step, the stirring temperature during the preparation of the aqueous phase is 25–35°C, the stirring speed is 300–600 r / min, and the stirring time is 15–25 min.

[0026] Furthermore, in the fourth step, syringes A and B are injection pumps, and the flow rates of the aqueous phase and the perfluorohexanone phase are controlled by the injection pumps connected to them; the injection pump speed of the aqueous phase is 2.5 ml / min to 9.5 ml / min, and the injection pump speed of the perfluorohexanone phase is 1.5 ml / min to 8.5 ml / min; the injection time of the two phases is set to 20 to 30 min.

[0027] Furthermore, in the fourth step, the mixing temperature of the aqueous phase and the perfluorohexanone phase at the tee is -5 to 35°C.

[0028] The beneficial effects of this invention are:

[0029] (1) The perfluorohexanone-stabilized emulsion prepared in this invention is a biodegradable material with an oil-in-water structure. The outer aqueous phase encapsulates the oil phase perfluorohexanone, and the overall emulsion is milky white. Polysorbate series surfactants have high hydrophobic-oleophobic balance values ​​and can provide the main hydrophilic interfacial activity, which has a good effect on reducing the interfacial tension between oil and water. Alkylphenol polyoxyethylene ethers have the functions of emulsification, wetting, and solubilization, and can be compounded with polysorbate series surfactants to form a synergistic effect, jointly reducing interfacial tension and accelerating interfacial coverage. Polyvinyl alcohol can inhibit droplet coalescence and Ostwald ripening by increasing the viscosity of the continuous phase through steric hindrance.

[0030] (2) The perfluorohexanone stabilized emulsion prepared by the present invention continuously absorbs heat when in contact with combustibles, and finally achieves effective cooling. When the ambient temperature rises, water and perfluorohexanone vaporize and expand. The expanded water vapor and perfluorohexanone vapor occupy the combustion zone and weaken the air supply, thereby reducing the local oxygen volume fraction, thus reducing the combustion intensity and finally extinguishing the fire. Attached Figure Description

[0031] Figure 1 This is a 0.1 mm × 0.1 mm field-of-view characterization image of the perfluorohexanone emulsion prepared in Example 3 under an optical microscope. Detailed Implementation

[0032] The perfluorohexanone stabilized emulsion of the present invention has a stable structure and can fully wet the combustible material. Both the aqueous phase and the perfluorohexanone can come into contact with the solid combustible material. During the fire extinguishing process, the water mainly plays a cooling role. The present invention will be described in detail below with reference to specific embodiments.

[0033] Example 1

[0034] In this embodiment, a Teflon transparent tube is used as the microchannel conduit. Injectors are connected to the two ports of the Y-shaped structure. Injector A contains a prepared aqueous solution, and injector B contains a perfluorohexanone solution. By controlling the perfluorohexanone and aqueous solutions in the injectors, the two phases are mixed at the tee of the Y-shaped structure and then enter the main pipeline. A one-way filter valve is simultaneously connected to the pipeline outlet, and high-speed shearing is used to prepare the emulsion.

[0035] In this embodiment, a one-way filter valve is connected to the tee, and the main pipe connected after the one-way filter valve is filled with solid beads. The main pipe has a diameter of 1.6 mm, a length of 1 m, and 1000 solid beads with a diameter of 1 mm.

[0036] In this embodiment, the aqueous phase is composed of 3.55% polysorbate surfactant, 0.45% alkylphenol polyoxyethylene ether, 0.05% polyvinyl alcohol, 83.40% deionized water, and 12.55% glycerol, with the sum of the mass percentages of all components being 100%. All components are stirred thoroughly to obtain the aqueous phase. The perfluorohexanone phase is a 99.9% pure perfluorohexanone solution. In this embodiment, the flow rate of the aqueous phase is controlled by an injection pump, with a pump speed of 2.5 ml / min. The flow rate of the perfluorohexanone phase is also controlled by an injection pump, with a pump speed of 1.5 ml / min. The propulsion time for both phases is set to 20 min. The polysorbate surfactant is polysorbate 20.

[0037] In this embodiment, the mixing temperature of the aqueous phase and the perfluorohexanone phase is -5°C;

[0038] In this embodiment, the stirring temperature for preparing the aqueous phase is 25°C, the stirring speed is 300 r / min, and the stirring time is 15 min.

[0039] Example 2

[0040] In this embodiment, a Teflon transparent tube is used as the microchannel conduit. Injectors are connected to the two ports of the Y-shaped structure. Injector A contains a prepared aqueous solution, and injector B contains a perfluorohexanone solution. By controlling the perfluorohexanone and aqueous solutions in the injectors, the two phases are mixed at the tee of the Y-shaped structure and then enter the main pipeline. A one-way filter valve is simultaneously connected to the pipeline outlet, and high-speed shearing is used to prepare the emulsion.

[0041] In this embodiment, a one-way filter valve is connected to the tee, and the main pipe connected after the one-way filter valve is filled with solid beads. The main pipe has a diameter of 3.2 mm, a length of 1.5 m, and 1200 solid beads with a diameter of 1.2 mm.

[0042] In this embodiment, the aqueous phase consists of 6.23% polysorbate surfactant, 3.17% alkylphenol polyoxyethylene ether, 3.55% polyvinyl alcohol, 67.49% deionized water, and 19.56% glycerol, with the sum of the mass percentages of all components being 100%. All components are stirred thoroughly to obtain the aqueous phase. The perfluorohexanone phase is a 99.9% pure perfluorohexanone solution. In this embodiment, the flow rate of the aqueous phase is controlled by an injection pump at a speed of 9.5 ml / min; the flow rate of the perfluorohexanone phase is also controlled by an injection pump at a speed of 8.5 ml / min; the propulsion time for both phases is set to 30 min; the polysorbate surfactant is polysorbate 120.

[0043] In this embodiment, the mixing temperature of the aqueous phase and the perfluorohexanone phase is 35°C;

[0044] In this embodiment, the stirring temperature when preparing the aqueous phase is 35°C, the stirring speed is 600 r / min, and the stirring time is 25 min.

[0045] Example 3

[0046] In this embodiment, a Teflon transparent tube is used as the microchannel conduit. Injectors are connected to the two ports of the Y-shaped structure. Injector A contains a prepared aqueous solution, and injector B contains a perfluorohexanone solution. By controlling the perfluorohexanone and aqueous solutions in the injectors, the two phases are mixed at the tee of the Y-shaped structure and then enter the main pipeline. A one-way filter valve is simultaneously connected to the pipeline outlet, and high-speed shearing is used to prepare the emulsion.

[0047] In this embodiment, a one-way filter valve is connected to the tee, and the main pipe connected after the one-way filter valve is filled with solid beads. The main pipe has a diameter of 2.0 mm, a length of 2.0 m, and 1400 solid beads with a diameter of 2.0 mm.

[0048] In this embodiment, the aqueous phase consists of 8.91% polysorbate surfactant, 5.89% alkylphenol polyoxyethylene ether, 3.55% polyvinyl alcohol, 62.09% deionized water, and 19.56% glycerol, with the sum of the mass percentages of all components being 100%. All components are stirred thoroughly to obtain the aqueous phase. The perfluorohexanone phase is a 99.9% pure perfluorohexanone solution. In this embodiment, the flow rate of the aqueous phase is controlled by an injection pump, with a pump speed of 6 ml / min. The flow rate of the perfluorohexanone phase is also controlled by an injection pump, with a pump speed of 5 ml / min. The propulsion time for both phases is set to 25 min. The polysorbate surfactant is polysorbate 80.

[0049] In this embodiment, the mixing temperature of the aqueous phase and the perfluorohexanone phase is 20°C.

[0050] In this embodiment, the stirring temperature for preparing the aqueous phase is 20°C, the stirring speed is 600 r / min, and the stirring time is 20 min.

[0051] Example 4

[0052] In this embodiment, a Teflon transparent tube is used as the microchannel conduit. Injectors are connected to the two ports of the Y-shaped structure. Injector A contains a prepared aqueous solution, and injector B contains a perfluorohexanone solution. By controlling the perfluorohexanone and aqueous solutions in the injectors, the two phases are mixed at the tee of the Y-shaped structure and then enter the main pipeline. A one-way filter valve is simultaneously connected to the pipeline outlet, and high-speed shearing is used to prepare the emulsion.

[0053] In this embodiment, a one-way filter valve is connected to the tee, and the main pipe connected after the one-way filter valve is filled with solid beads. The main pipe has a diameter of 2.5 mm, a length of 2.5 m, and 1600 solid beads with a diameter of 2.5 mm.

[0054] In this embodiment, the aqueous phase is composed of 7.55% polysorbate surfactant, 4.67% alkylphenol polyoxyethylene ether, 2.55% polyvinyl alcohol, 69.58% deionized water, and 15.65% propylene glycol, with the sum of the mass percentages of all components being 100%. All components are stirred thoroughly to obtain the aqueous phase. The perfluorohexanone phase is a 99.9% pure perfluorohexanone solution. In this embodiment, the flow rate of the aqueous phase is controlled by an injection pump, with a pump speed of 5.5 ml / min. The flow rate of the perfluorohexanone phase is also controlled by an injection pump, with a pump speed of 4.5 ml / min. The propulsion time for both phases is set to 28 min. The polysorbate surfactant is polysorbate 85.

[0055] In this embodiment, the mixing temperature of the aqueous phase and the perfluorohexanone phase is 0°C.

[0056] In this embodiment, the stirring temperature for preparing the aqueous phase is 18°C, the stirring speed is 550 r / min, and the stirring time is 18 min.

[0057] Example 5

[0058] In this embodiment, a Teflon transparent tube is used as the microchannel conduit. Injectors are connected to the two ports of the Y-shaped structure. Injector A contains a prepared aqueous solution, and injector B contains a perfluorohexanone solution. By controlling the perfluorohexanone and aqueous solutions in the injectors, the two phases are mixed at the tee of the Y-shaped structure and then enter the main pipeline. A one-way filter valve is simultaneously connected to the pipeline outlet, and high-speed shearing is used to prepare the emulsion.

[0059] In this embodiment, a one-way filter valve is connected to the tee, and the main pipe connected after the one-way filter valve is filled with solid beads. The main pipe has a diameter of 3.0 mm, a length of 5.0 m, and 2000 solid beads with a diameter of 3.0 mm.

[0060] In this embodiment, the aqueous phase is composed of 4.78% polysorbate surfactant, 5.15% alkylphenol polyoxyethylene ether, 2.65% polyvinyl alcohol, 69.87% deionized water, and 17.55% glycerol, with the sum of the mass percentages of all components being 100%. All components are stirred thoroughly to obtain the aqueous phase. The perfluorohexanone phase is a 99.9% pure perfluorohexanone solution. In this embodiment, the flow rate of the aqueous phase is controlled by an injection pump at a speed of 4.5 ml / min; the flow rate of the perfluorohexanone phase is also controlled by an injection pump at a speed of 3.5 ml / min; the propulsion time for both phases is set to 22 min; the polysorbate surfactant is polysorbate 40.

[0061] In this embodiment, the mixing temperature of the aqueous phase and the perfluorohexanone phase is 5°C. The stirring temperature for preparing the aqueous phase is 31°C, the stirring speed is 450 r / min, and the stirring time is 18 min.

[0062] Verification of the effectiveness of this invention:

[0063] The perfluorohexanone emulsion prepared in Example 3 was characterized under an optical microscope at a field of view of 0.1 mm × 0.1 mm as follows: Figure 1 As shown, from Figure 1 As can be seen, the prepared emulsion is uniformly mixed and presents a highly regular monodisperse array.

[0064] Table 1: Comparison of the fire extinguishing effects of the perfluorohexanone stabilized emulsion of the present invention with water and liquid perfluorohexanone

[0065]

[0066] As shown in Table 1, the fire extinguishing time of the perfluorohexanone stabilized emulsion prepared by the present invention is shorter than that of liquid perfluorohexanone, that is, the fire extinguishing effect of the perfluorohexanone stabilized emulsion prepared by the present invention is better than the existing fire extinguishing efficiency.

[0067] Table 2 shows the reagent screening results of this invention, examining the effects of adding different reagents on the properties of perfluorohexanone-stabilized emulsions. The results in Table 2 indicate that polysorbate surfactants have high hydrophobic-oleophobic balance values, providing the main hydrophilic interfacial activity and effectively reducing oil-water interfacial tension. Alkylphenol polyoxyethylene ethers have emulsifying, wetting, and solubilizing effects, and can synergistically combine with polysorbate surfactants to reduce interfacial tension and accelerate interfacial coverage. Polyvinyl alcohol can inhibit droplet coalescence and Ostwald ripening by increasing the viscosity of the continuous phase through steric hindrance. Glycerol contains three hydrophilic hydroxyl groups, which can form strong hydrogen bonds with water molecules, significantly lowering the freezing point of the emulsion. The combined addition of polysorbate, alkylphenol polyoxyethylene ether, polyvinyl alcohol, and glycerol significantly enhances the storage and usage stability of the emulsion; the effects achieved by reagents such as sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, and hexadecyltrimethylammonium bromide cannot be achieved with the above reagents.

[0068] Table 2: Reagent Screening Results

[0069]

[0070] Perfluorohexanone, as a new generation of clean chemical fire extinguishing agent, possesses highly efficient fire extinguishing performance, but it is highly volatile at room temperature. Existing technologies mostly focus on dry powder formulations and matching fire extinguishing devices. This invention employs a microchannel device for emulsification, improving the storage and use stability of perfluorohexanone. It combines multiple emulsifiers and preferentially selects surfactants that significantly enhance emulsification stability, ensuring the system remains stable at room temperature and is easy to store and transport. During fire extinguishing, this stable emulsion continuously absorbs heat upon contact with combustibles and rapidly removes heat from the flame zone. Simultaneously, the vapor it generates dilutes the air in the combustion zone, reducing combustion intensity and improving fire extinguishing efficiency.

[0071] The above embodiments are merely illustrative of the implementation methods of the present invention, but should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the protection scope of the present invention.

Claims

1. A microchannel-based perfluorohexanone-stabilized emulsion, characterized in that, The perfluorohexanone stabilized emulsion is an oil-in-water emulsion, with an outer aqueous phase encapsulating an oil phase, the oil phase being the perfluorohexanone phase. The preparation and control of the perfluorohexanone stabilized emulsion are achieved by adjusting the injection pump rates of the aqueous phase and the perfluorohexanone phase. The aqueous phase comprises polysorbate surfactant, alkylphenol polyoxyethylene ether, polyvinyl alcohol, deionized water, and glycerol. The perfluorohexanone phase is a perfluorohexanone solution.

2. The microchannel-based perfluorohexanone stabilized emulsion according to claim 1, characterized in that, The mass percentage of each component in the aqueous phase is as follows: The aqueous phase consists of 3.55%–8.91% polysorbate surfactant, 0.45%–5.89% alkylphenol polyoxyethylene ether, 0.05%–3.55% polyvinyl alcohol, 62.09%–83.40% deionized water, and 12.55%–19.56% glycerol. The sum of the mass percentages of the above components is 100%. All components are stirred evenly to obtain an aqueous phase.

3. The microchannel-based perfluorohexanone stabilized emulsion according to claim 1, characterized in that, The perfluorohexanone phase is a perfluorohexanone solution with a purity of 99.9%.

4. The microchannel-based perfluorohexanone stabilized emulsion according to claim 1, characterized in that, Furthermore, the glycerol in the aqueous phase can be replaced with propylene glycol.

5. A method for preparing a microchannel-based perfluorohexanone-stabilized emulsion according to any one of claims 1-4, characterized in that, Includes the following steps: The first step is to prepare microchannels; The microchannel described is a Y-shaped structure, comprising two branches and a main channel; The interfaces of the two branches of the Y-shaped structure are respectively connected to syringe A and syringe B; The second step is to mix the components of the aqueous phase and stir until homogeneous. The third step is to prepare the perfluorohexanone phase; The fourth step is to prepare a perfluorohexanone-stabilized emulsion; The syringe A contains an aqueous solution, and the syringe B contains a perfluorohexanone solution. By controlling the flow rates of the perfluorohexanone phase and the aqueous phase, the two phases are mixed at the tee of the Y-shaped structure and then enter the main pipe, where the preparation of the perfluorohexanone microemulsion is completed. A one-way filter valve is connected to the tee of the Y-shaped structure. The main pipe connected after the one-way filter valve is filled with solid beads. The outlet of the main pipe is connected to a one-way filter valve. The emulsion is prepared by high-speed shearing.

6. The method for preparing a microchannel-based perfluorohexanone stabilized emulsion according to claim 5, characterized in that, The diameter of the two branches and the main pipeline of the Y-shaped structure is 1.6mm to 3.2mm, and the material is Teflon transparent tubing.

7. The method for preparing a microchannel-based perfluorohexanone stabilized emulsion according to claim 5, characterized in that, The solid spheres filling the main pipe have a diameter of 1mm to 5mm, a number of 1000 to 2000, and a length of 1m to 5m.

8. The method for preparing a microchannel-based perfluorohexanone stabilized emulsion according to claim 5, characterized in that, The stirring temperature for configuring the aqueous phase is 25–35°C, the stirring speed is 300–600 r / min, and the stirring time is 15–25 min.

9. The method for preparing a microchannel-based perfluorohexanone stabilized emulsion according to claim 5, characterized in that, In the fourth step, syringes A and B are injection pumps, and the flow rates of the aqueous phase and the perfluorohexanone phase are controlled by the injection pumps connected to them; the injection pump speed of the aqueous phase is 2.5 ml / min to 9.5 ml / min, and the injection pump speed of the perfluorohexanone phase is 1.5 ml / min to 8.5 ml / min; the injection time of the two phases is set to 20 to 30 min.

10. The method for preparing a microchannel-based perfluorohexanone stabilized emulsion according to claim 5, characterized in that, The mixing temperature of the aqueous phase and the perfluorohexanone phase at the tee is -5 to 35°C.

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