CN110960997B - Device for rapidly producing a stable volume of water-in-oil microemulsion - Google Patents

Device for rapidly producing a stable volume of water-in-oil microemulsion Download PDF

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CN110960997B
CN110960997B CN201911343179.XA CN201911343179A CN110960997B CN 110960997 B CN110960997 B CN 110960997B CN 201911343179 A CN201911343179 A CN 201911343179A CN 110960997 B CN110960997 B CN 110960997B
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pipeline
water phase
microemulsion
water
outlets
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CN110960997A (en
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秦玉岭
吴丽
刘金霞
冀海伟
周晓波
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Nantong University
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Nantong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40Mixing liquids with liquids; Emulsifying
    • B01F23/41Emulsifying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30Micromixers

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  • Chemical Kinetics & Catalysis (AREA)

Abstract

The invention provides a device for quickly generating water-in-oil microemulsion with stable volume, which comprises a water-phase injection port, a microemulsion generation chamber and a circulating pipeline; the circulating pipeline comprises a pipeline inlet and a plurality of pipeline outlets, the pipeline inlet is connected with the water phase sample inlet, the plurality of pipeline outlets are respectively connected with a plurality of water phase sample outlets on the side wall of the microemulsion generating chamber, an oil phase and a stirring device are arranged in the microemulsion generating chamber, the flow direction of the water phase sample outlet water phase is perpendicular to the flow direction of the oil phase, and the water phase flow velocity and the flow of the plurality of water phase sample outlets are the same. The liquid drops generated by the invention are not limited by a pipeline, are directly stored in a large cavity in situ, are particularly suitable for the experiment of the solution with large water phase volume, and solve the problems of long time and high equipment cost of the current high-flux microemulsion generation device.

Description

Device for rapidly producing a stable volume of water-in-oil microemulsion
Technical Field
The invention belongs to the field of microemulsion analysis, and particularly relates to a device for quickly generating water-in-oil microemulsion with stable volume.
Background
The water-in-oil microemulsion liquid drop has the advantages of obviously reducing the amount of reaction reagents and the pollution possibility due to small volume, so the water-in-oil microemulsion liquid drop is an important means for digitally researching biological information analysis, such as single cell and single molecule experiments, for many years. It can quickly analyze a large amount of biomedical information, improve analysis flux and greatly reduce analysis cost. In addition, since the aqueous phase droplets separated from the oil phase do not interfere with each other, they have been reported in a great deal of research in the field of nanomaterial preparation.
The T-shaped tubular structure is the most widely applied design for generating microemulsion, and oil phase sample injection is arranged in the direction vertical to the flow of the water phase. The continuous water phase is divided into discontinuous phases by utilizing the shearing force generated by the vertical compression of the oil phase, so that the large-volume water phase is divided into the small-volume microemulsion, and the high-flux analysis of the target is realized.
However, the amount of microemulsion generated by a single T-shaped pipe structure per unit time is small due to the influence of the cross section and the flow rate of the pipeline. For the solution with larger water phase volume, it takes a long time to completely liquefy the microemulsion. Therefore, various microfluidic devices based on this mechanism have been reported, and experiments with multiple parallel channels simultaneously can improve the yield of microemulsion.
Although various structures have been explored beneficially in improving microemulsion flux, these designs suffer from the disadvantages of complex structures, reliance on additional equipment for collecting the microemulsion, complex control systems, and the like.
Disclosure of Invention
Aiming at the problems, the invention designs a device which can rapidly generate a large amount of microemulsion, the generated liquid drops are not limited by a pipeline, and the generated liquid drops are directly stored in a large cavity in situ, so that the device is particularly suitable for the experiment of the solution with large water phase volume, and the problems of long time and high equipment cost of the current high-flux microemulsion generating device are solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the device for quickly producing water-in-oil microemulsion with stable volume comprises an aqueous phase injection port, a microemulsion generation chamber and a flow pipeline; the circulating pipeline comprises a pipeline inlet and a plurality of pipeline outlets, the pipeline inlet is connected with the water phase sample inlet, the plurality of pipeline outlets are respectively connected with a plurality of water phase sample outlets on the side wall of the microemulsion generating chamber, an oil phase and a stirring device are arranged in the microemulsion generating chamber, and the flow direction of the water phase sample outlet water phase is perpendicular to the flow direction of the oil phase.
Preferably, the flow rate and the flow rate of the aqueous phase at the plurality of aqueous phase outlets are the same.
Preferably, the circulation pipeline comprises a primary pipeline, a secondary pipeline and a tertiary pipeline which are sequentially communicated; the center of the first-stage pipeline is connected with a water phase sample inlet, and two halves of the first-stage pipeline are in mirror symmetry; the secondary pipeline is circular, and two points with the same diameter of the circle are respectively connected with two ends of the primary pipeline; the tertiary pipeline has a plurality of, along secondary pipeline circumference evenly distributed, and the tertiary pipeline includes a plurality of grades of subdivision pipelines, and the above one-level subdivision pipeline of each collection subdivision pipeline sets up for symmetry axis symmetry, and the exit linkage aqueous phase of last one-level subdivision pipeline goes out the appearance mouth.
Has the advantages that:
(1) all the water phase pipelines are symmetrically designed at the outlets of the microemulsion generation chamber and the water phase flow pipelines, so that the water phase rates flowing out of the outlets are the same, and the flowing direction is vertical to the flowing direction of the oil phase. The outflow rate of the water phase is the same, and the size of the liquid drops generated by the outlets can be ensured to be the same by the same shearing force, direction and size.
(2) The operation is simple and convenient, and the experiment only relates to an additional stirrer and a water phase sample injection pump;
(3) according to the actual requirements, a sample introduction pipeline can be simply added, the generation rate of the microemulsion is improved, and the method is suitable for large sample experiments such as chemical synthesis and the like;
(4) the volume of the generated microemulsion liquid drop can be regulated and controlled by controlling the oil phase stirring speed and the water phase sample injection speed: the speed of the water phase at the outlet is increased, so that the diameter of generated liquid drops can be increased; reducing the velocity of the aqueous phase at the outlet reduces the diameter of the droplets formed. The stirring speed of the oil phase is improved, and the shearing force of the water phase at the outlet from the vertical direction can be increased, so that the water phase is quickly divided, and the purpose of reducing the size of liquid drops is achieved; conversely, decreasing the rate increases the droplet size.
(5) The device can be used repeatedly many times after wasing, avoids extravagant.
Drawings
FIG. 1 is a top view of the apparatus, A sample inlet; b, a device main body; c, generating and storing a microemulsion; d, a circulation pipeline; e is a primary pipeline; f is a secondary pipeline; g is a three-stage pipeline; h is a subdivided pipeline.
Fig. 2 is a side view of the device.
FIG. 3 is a simulated plot of microemulsion droplet generation with the oil phase flow rate 10 times the water phase flow rate.
FIG. 4 is a simulated plot of microemulsion droplet production with the oil phase flow rate being 40 times the water phase flow rate.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
The invention comprises the following steps: a sample inlet, a circulation pipeline, a microemulsion generation chamber and a storage chamber.
1) The sample inlet mainly performs inflow of the aqueous phase liquid sample.
2) The circulation pipeline is connected with the sample inlet and the water phase sample outlet, and the water phase flowing in from the sample inlet is uniformly dispersed and conveyed to the sample outlet. In this embodiment, the circulation pipeline includes a primary pipeline, a secondary pipeline and a tertiary pipeline which are sequentially communicated; the center of the first-stage pipeline is connected with a water phase sample inlet, and two halves of the first-stage pipeline are in mirror symmetry; the secondary pipeline is circular, and two points with the same diameter of the circle are respectively connected with two ends of the primary pipeline; the tertiary pipeline has a plurality of, along secondary pipeline circumference evenly distributed, and the tertiary pipeline includes a plurality of grades of subdivision pipelines, and the above one-level subdivision pipeline of each collection subdivision pipeline sets up for symmetry axis symmetry, and the exit linkage aqueous phase of last one-level subdivision pipeline goes out the appearance mouth. The structure of the circulation pipeline is not limited to the structure given in this embodiment, as long as the flow rate and the flow rate of the aqueous phase at the aqueous phase sample outlet are the same.
3) The microemulsion generation chamber and the storage chamber are integral. The space of the stirring device is reserved, and magnetic stirring or mechanical stirring can be carried out. Under the action of the stirrer, the oil phase rotates fast to produce shearing force in the direction perpendicular to the water phase sample introduction direction and to isolate the water phase. The resulting microemulsion can be stored in situ until the end of the stirring.
The operation method of the invention is as follows:
1) firstly, the surfaces contacted by all liquid in the chip are subjected to hydrophobic treatment, and for plastic materials, the surfaces originally have hydrophobic characteristics, so that additional treatment is not needed; if the chip is made of polydimethylsiloxane and glass materials and bonded by applying the plasma cleaning technology, the chip can be subjected to heat preservation treatment for 24 hours by using an oven at the temperature of 100-120 ℃.
2) And (5) opening the stirring device, and setting the speed according to the requirement.
3) From the sample inlet, the injection pump injects water into the microemulsion generating chamber at a constant speed. The water phase flowing out from the sample outlet generates microemulsion under the shearing force generated by the oil phase rotating at high speed, and the oil-water interfacial tension can maintain the stable existence of the microemulsion.
4) And (5) after the sample introduction is finished, closing the injection pump, stopping stirring, and taking out the microemulsion.
As shown in fig. 1, the number of sampling channels can be increased or decreased depending on the microemulsion demand flux. The two opposite sample introduction pipelines connected with the sample outlet are mirror-symmetrical, and the subdivision pipeline behind the sample introduction pipeline is centrosymmetrical with the outlet connected with the reaction chamber, so that the partial pressure of the liquid at the parallel position in the pipeline is ensured to be the same, the flow rate of the liquid at the outlet in the pipeline is ensured to be the same, and the size of the generated liquid drops is ensured to be the same.
As shown in fig. 2, the sample inlet a is connected to a syringe pump. The C storage chamber is a non-closed space, so that the increase of the injection pressure of the injection pump is avoided, and the flow velocity of the sample outlet is not uniform.
Figures 3 and 4 show the relationship between droplet generation and flow rate simulated by fluid simulation software, with an inlet size of 20-100 microns and, after partial enlargement, the curved wall of the circular stirrer is approximately planar. When the flow rate ratio of the oil phase and the aqueous phase is larger, the smaller the size of the droplets produced, that is, when the oil phase agitation speed is higher, the aqueous phase outflow speed is lower, the smaller the size of the droplets is more easily produced; the larger the size of the droplets produced when the flow rate ratio of the oil phase and the aqueous phase is smaller, that is, the larger the outflow rate of the aqueous phase when the stirring speed of the oil phase is lower, the larger the size of the droplets produced more easily.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.

Claims (1)

1. The device for rapidly generating the water-in-oil microemulsion with stable volume is characterized by comprising an aqueous phase injection port, a microemulsion generation chamber and a circulating pipeline; the circulating pipeline comprises a pipeline inlet and a plurality of pipeline outlets, the pipeline inlet is connected with the water phase sample inlet, the pipeline outlets are respectively connected with the water phase sample outlets on the side wall of the microemulsion generating chamber, the microemulsion generating chamber is internally provided with an oil phase and a stirring device, and the flow direction of the water phase sample outlet water phase is vertical to the flow direction of the oil phase;
the flow velocity and the flow of the water phase at the plurality of water phase sample outlets are the same;
the circulating pipeline comprises a primary pipeline, a secondary pipeline and a tertiary pipeline which are sequentially communicated; the center of the first-stage pipeline is connected with a water phase sample inlet, and two halves of the first-stage pipeline are in mirror symmetry; the secondary pipeline is circular, and two points with the same diameter of the circle are respectively connected with two ends of the primary pipeline; the tertiary pipeline has a plurality of, along secondary pipeline circumference evenly distributed, and the tertiary pipeline includes a plurality of grades of subdivision pipelines, and the above one-level subdivision pipeline of each grade subdivision pipeline sets up for symmetry axis symmetry, and the exit linkage aqueous phase appearance mouth of last one-level subdivision pipeline.
CN201911343179.XA 2019-12-24 2019-12-24 Device for rapidly producing a stable volume of water-in-oil microemulsion Active CN110960997B (en)

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CN101268574A (en) * 2005-09-16 2008-09-17 雷诺股份公司 Plate for fuel cell
CN101683592A (en) * 2008-09-28 2010-03-31 中国科学院过程工程研究所 Membrane emulsifier and method of preparing emulsion
CN103025417A (en) * 2010-07-23 2013-04-03 日东电工株式会社 Device for forming droplets and method for forming droplets
CN104069757A (en) * 2014-07-07 2014-10-01 东南大学 Dual-microemulsion rapid preparation device
CN105597582A (en) * 2016-03-24 2016-05-25 华东理工大学 Mechanically-stirring type continuous emulsifier and emulsifying method
CN106140340A (en) * 2016-08-19 2016-11-23 北京工业大学 Micro-fluidic chip based on flow focusing type microchannel synthesis microemulsion drop
CN108273576A (en) * 2018-03-12 2018-07-13 苏州锐讯生物科技有限公司 The micro-fluidic chip system that adjustable lotion is formed
CN109012251A (en) * 2017-06-09 2018-12-18 淡江大学 Rotary emulsifying device structure
CN109351217A (en) * 2018-11-22 2019-02-19 然晟(上海)实业发展有限公司 A kind of phaco device preparing pesticide micro capsule

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EP3068526B1 (en) * 2013-11-11 2021-05-05 King Abdullah University Of Science And Technology Microfluidic device for high-volume production and processing of monodisperse emulsions and method
CN105797791B (en) * 2016-03-16 2017-11-03 清华大学深圳研究生院 A kind of microfluid ion source chip and preparation method thereof
GB2572403B (en) * 2018-03-29 2023-05-17 Univ Heriot Watt Microfluidic device

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1867394A (en) * 2003-10-16 2006-11-22 巴塞尔聚烯烃意大利有限责任公司 Process for the continuous production of emulsions
CN101268574A (en) * 2005-09-16 2008-09-17 雷诺股份公司 Plate for fuel cell
CN101683592A (en) * 2008-09-28 2010-03-31 中国科学院过程工程研究所 Membrane emulsifier and method of preparing emulsion
CN103025417A (en) * 2010-07-23 2013-04-03 日东电工株式会社 Device for forming droplets and method for forming droplets
CN104069757A (en) * 2014-07-07 2014-10-01 东南大学 Dual-microemulsion rapid preparation device
CN105597582A (en) * 2016-03-24 2016-05-25 华东理工大学 Mechanically-stirring type continuous emulsifier and emulsifying method
CN106140340A (en) * 2016-08-19 2016-11-23 北京工业大学 Micro-fluidic chip based on flow focusing type microchannel synthesis microemulsion drop
CN109012251A (en) * 2017-06-09 2018-12-18 淡江大学 Rotary emulsifying device structure
CN108273576A (en) * 2018-03-12 2018-07-13 苏州锐讯生物科技有限公司 The micro-fluidic chip system that adjustable lotion is formed
CN109351217A (en) * 2018-11-22 2019-02-19 然晟(上海)实业发展有限公司 A kind of phaco device preparing pesticide micro capsule

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