CN102941050B - Method for preparing even and hollow liquid drops based on micro-fluidic technology - Google Patents

Method for preparing even and hollow liquid drops based on micro-fluidic technology Download PDF

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CN102941050B
CN102941050B CN201210479303.7A CN201210479303A CN102941050B CN 102941050 B CN102941050 B CN 102941050B CN 201210479303 A CN201210479303 A CN 201210479303A CN 102941050 B CN102941050 B CN 102941050B
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gas
drop
component
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CN102941050A (en
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骆广生
杨路
王凯
吕阳成
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Tsinghua University
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Abstract

The invention discloses a method for preparing even and hollow liquid drops based on the micro-fluidic technology and belongs to the technical field of chemical engineering. The method combines the micro-fluidic technology and a gas-liquid mass transfer process, and mixed gas formed by steaming component gas to be absorbed and the liquid drops is led into a micro device and form the gas-liquid mass transfer process under the shearing action of continuous phase liquid. Simultaneously, a component for mass transfer in a gas phase is constantly absorbed by the continuous phase liquid, so that the partial pressure of a liquid drop phase steam component is increased till the partial pressure exceeds saturated vapor pressure under the operating condition, the gas phase is converted into a liquid phase, and the liquid is wrapped on the surfaces of air bubbles to form the hollow liquid drops. The average diameter of prepared hollow liquid drops is 50-1000mum, the relative deviation is smaller than 3%, and the liquid membrane thickness is 1-50mum. The method is simple, convenient and reliable, large-scale preparation can be achieved in the micro device with a simple structure, the size and the thickness of the liquid drops are convenient to adjust and control, and the monodispersity is good.

Description

A kind of method of preparing even hollow drop based on microflow control technique
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of method of preparing even hollow drop based on microflow control technique.
Technical background
Hollow drop is with its special composition and structure, in chemistry, chemical industry, material, biology, medicine and other fields, be with a wide range of applications, such as for the manufacture of new high-tech products such as lightweight filler, photoelectric display equipment, chemical catalysis material, drug delivery vehicles.The drop with this kind of hollow structure is prepared the monodispersity that difficult point is drop, and the control of size and thickness of liquid film and regulation and control.
The microflow control technique growing up at chemical field in recent years provides effective method for realizing the preparation of single dispersant liquid drop or multiplet drop.Have at present a few studies person to utilize microfluidic device to prepare the hollow drop of internal layer parcel bubble, but the method adopting have the following disadvantages mostly: gas-liquid system is taked multistage or multilayer dispersion, to the structural design of microfluidic device and manufacture, requires higher; The suffered foreign minister's continuous phase of internal layer gas phase shearing force a little less than, the drop size of formation is bigger than normal; In order to make to disperse the multiplet flow pattern forming to stablize, need to take further screening to gas-liquid system, operation and restricted application.
For the problem of above existence, device structure large-scale producing method simple and that have a general applicability becomes the active demand of the preparation of hollow drop and application aspect.On the basis of microflow control technique in conjunction with physical and chemical processes such as gas-liquid interphase mass transfer and inversion of phases, for the preparation of the complicated Gas-Liquid Dispersion flow patterns such as hollow drop provides new ways and means.
Summary of the invention
The invention discloses a kind of method based on the even hollow drop of the extensive preparation of microflow control technique.
A method of preparing even hollow drop based on microflow control technique, the method is the process that microflow control technique combines with gas-liquid mass transfer, comprises the following steps:
(1) take gas phase as decentralized photo, liquid phase is continuous phase, and gas-liquid two-phase is conveyed in microfluidic device, and decentralized photo gas forms uniform and stable single gas column or bubble of disperseing under the shear action of continuous phase liquid; Wherein gas-phase feed temperature is 20 ~ 90 ℃, and gas phase and liquid phase flow-rate ratio are 3 ~ 100, and the passage length of microfluidic device is 10 ~ 200 cm;
Described gas phase is the mist that contains component to be absorbed and approach saturated drop phase steam component; Wherein component to be absorbed is the gas component with continuous phase liquid generation effect of mass transmitting, significantly improves guaranteeing by the dividing potential drop of effect of mass transmitting liquid film phase steam component; Drop phase steam group is divided into the gas component that drop phase liquid volatilizees and forms at gas-phase feed temperature;
The solution containing absorbent of described liquid phase for not dissolving each other mutually with drop or having an effect;
(2) along with single gas column or bubble of disperseing flows in microfluidic device, in gas phase, component to be absorbed constantly and liquid phase generation effect of mass transmitting and then by continuous phase liquid absorption, the dispersion size of gas column or bubble reduces to form uniform microbubble kernel on the one hand, in gas phase, the dividing potential drop of drop phase steam component constantly increases until surpass the saturated vapor pressure under operating condition on the other hand, and then by gas phase conversion be liquid phase coating at bubble core surface, form hollow drop; Hollow drop has composite construction, for internal layer parcel bubble top layer is that thin electrolyte film or internal layer bubble are absorbed formation homogeneous drop completely.
Described component to be absorbed is carbon dioxide or ammonia.
Described drop phase liquid is that saturated vapor pressure is alkanes, ketone, alcohols or the ester class of 5 ~ 100 kPa in gas-phase feed temperature range.
Described absorbent is NaOH, potassium hydroxide, MEA, diethanol amine or acetic acid.
The present invention has the following advantages: the hollow mean drop diameter that the inventive method is prepared is 50 ~ 1000 μ m, relative deviation <3%, thickness of liquid film is 1 ~ 50 μ m, and the hollow drop monodispersity of formation is good, and size and thickness of liquid film are convenient to regulation and control; The method adopting is easy to be reliable, in conventional micro equipment simple in structure, can realize extensive preparation; The system scope of application and opereating specification are wider, have general applicability.
Accompanying drawing explanation
Fig. 1 is hollow drop forming process schematic diagram in microchannel.
The hollow drop (scale 100 μ ms) of Fig. 2 for forming.
The specific embodiment
By example, the present invention is further described below.
Embodiment 1
Decentralized photo gas is the gaseous mixture of carbon dioxide and pentane steam, and flow is 40mL/min, and gas-phase feed temperature is 27 ℃; Continuous phase liquid is 0.1M sodium hydrate aqueous solution (containing 0.05wt% SDS), and flow is 2mL/min, is passed in cross microfluidic device channel water aerodynamic diameter 600 μ m, passage length 27cm by syringe pump.The mode of shearing by symmetrical vertical current and gas-liquid interphase mass transfer process form hollow drop, and as shown in Figure 1, the mean drop diameter that outlet obtains is 50 μ m, and thickness of liquid film is 5 μ m, as shown in Figure 2.
Embodiment 2
Decentralized photo gas is the gaseous mixture of carbon dioxide and n-hexane steam, and flow is 40mL/min, and gas-phase feed temperature is 40 ℃; Continuous phase liquid is 1M sodium hydrate aqueous solution (containing 0.05 wt% SDS), and flow is 800 μ L/min, is passed in T-type microfluidic device channel water aerodynamic diameter 600 μ m, passage length 63cm by syringe pump.The mode of shearing by cross-flow and gas-liquid interphase mass transfer process form micro-drop, as shown in Figure 1.The mean drop diameter that outlet obtains is 98 μ m, internal layer bubble collapse.
Embodiment 3
Decentralized photo gas is the gaseous mixture of carbon dioxide and normal octane steam, and flow is 70mL/min, and gas-phase feed temperature is 80 ℃; Continuous phase liquid is 0.5M sodium hydrate aqueous solution (containing 0.05wt% SDS), and flow is 1mL/min, is passed in coaxial rings cast microfluidic device channel water aerodynamic diameter 600 μ m, passage length 45cm by syringe pump.By mode and gas-liquid interphase mass transfer process that also stream is sheared, form hollow drop, as shown in Figure 1.The mean drop diameter that outlet obtains is 320 μ m, and thickness of liquid film is 36 μ m.
Embodiment 4
Decentralized photo gas is the gaseous mixture of carbon dioxide and n-butanol steam, and flow is 40mL/min, and gas-phase feed temperature is 27 ℃; Continuous phase liquid is the 20wt% MEA aqueous solution (containing 0.05wt% SDS), and flow is 1.5mL/min, is passed in cross microfluidic device channel water aerodynamic diameter 600 μ m, passage length 45cm by syringe pump.The mode of shearing by symmetrical vertical current and gas-liquid interphase mass transfer process form hollow drop, as shown in Figure 1.The mean drop diameter that outlet obtains is 130 μ m, and thickness of liquid film is 1 μ m.
Embodiment 5
Decentralized photo gas is the gaseous mixture of carbon dioxide and 2 pentanone steam, and flow is 40mL/min, and gas-phase feed temperature is 60 ℃; Continuous phase liquid is 0.5M potassium hydroxide aqueous solution (containing 0.05wt% SDS), and flow is 400 μ L/min, is passed in cross microfluidic device channel water aerodynamic diameter 600 μ m, passage length 15cm by syringe pump.The mode of shearing by symmetrical vertical current and gas-liquid interphase mass transfer process form hollow drop, as shown in Figure 1.The mean drop diameter that outlet obtains is 550 μ m, and thickness of liquid film is 17 μ m.
Embodiment 6
Decentralized photo gas is the gaseous mixture of ammonia and n-hexane steam, and flow is 40mL/min, and gas-phase feed temperature is 27 ℃; Continuous phase liquid is 5wt% acetic acid aqueous solution (containing 0.05 wt% SDS), and flow is 400 μ L/min, is passed in cross microfluidic device channel water aerodynamic diameter 600 μ m, passage length 27cm by syringe pump.The mode of shearing by symmetrical vertical current and gas-liquid interphase mass transfer process form hollow drop, as shown in Figure 1.The mean drop diameter that outlet obtains is 770 μ m, and thickness of liquid film is 13 μ m.

Claims (4)

1. based on microflow control technique, prepare a method for even hollow drop, it is characterized in that: the method is the process that microflow control technique combines with gas-liquid mass transfer, comprises the following steps:
(1) take gas phase as decentralized photo, liquid phase is continuous phase, and gas-liquid two-phase is conveyed in microfluidic device, and decentralized photo gas forms uniform and stable single gas column or bubble of disperseing under the shear action of continuous phase liquid; Wherein gas-phase feed temperature is 20~90 ℃, and gas phase and liquid phase flow-rate ratio are 3~100, and the passage length of microfluidic device is 10~200cm;
Described gas phase is the mist that contains component to be absorbed and approach saturated drop phase steam component; Wherein component to be absorbed is the gas component with continuous phase liquid generation effect of mass transmitting, significantly improves guaranteeing by the dividing potential drop of effect of mass transmitting liquid film phase steam component; Drop phase steam group is divided into the gas component that drop phase liquid volatilizees and forms at gas-phase feed temperature;
The solution containing absorbent of described liquid phase for not dissolving each other mutually with drop or having an effect;
(2) along with single gas column or bubble of disperseing flows in microfluidic device, in gas phase, component to be absorbed constantly and liquid phase generation effect of mass transmitting and then by continuous phase liquid absorption, the dispersion size of gas column or bubble reduces to form uniform microbubble kernel on the one hand, in gas phase, the dividing potential drop of drop phase steam component constantly increases until surpass the saturated vapor pressure under operating condition on the other hand, and then by gas phase conversion be liquid phase coating at bubble core surface, form hollow drop; Hollow drop has composite construction, for internal layer parcel bubble top layer is that thin electrolyte film or internal layer bubble are absorbed formation homogeneous drop completely.
2. method according to claim 1, is characterized in that: described component to be absorbed is carbon dioxide or ammonia.
3. method according to claim 1, is characterized in that: described drop phase liquid is alkanes, ketone, alcohols or the ester class that saturated vapor pressure is 5~100kPa in gas-phase feed temperature range.
4. method according to claim 1, is characterized in that: described absorbent is NaOH, potassium hydroxide, MEA, diethanol amine or acetic acid.
CN201210479303.7A 2012-11-22 2012-11-22 Method for preparing even and hollow liquid drops based on micro-fluidic technology Active CN102941050B (en)

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