CN113304701B - Microcapsule preparation device based on micro-fluidic technology - Google Patents
Microcapsule preparation device based on micro-fluidic technology Download PDFInfo
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- CN113304701B CN113304701B CN202110704128.6A CN202110704128A CN113304701B CN 113304701 B CN113304701 B CN 113304701B CN 202110704128 A CN202110704128 A CN 202110704128A CN 113304701 B CN113304701 B CN 113304701B
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- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
Abstract
The invention relates to the technical field of material preparation devices, and discloses a micro-fluidic technology-based microcapsule preparation device which comprises an inner pipeline, a middle pipeline, an outer pipeline and a lamp tube, wherein the inner pipeline, the middle pipeline and the outer pipeline are sequentially sleeved from inside to outside; the top of the inner pipeline can be connected with an external inner phase liquid input pipe, the bottom of the inner pipeline is closed, a plurality of liquid outlet holes are formed in the inner pipeline, and micro connecting pipes protruding outwards are arranged on the liquid outlet holes; the middle pipeline is provided with a plurality of through holes, the through holes correspond to the micro connecting pipes one by one, the outlets of the micro connecting pipes extend into the through holes, the top of the middle pipeline can be connected with an external middle-phase liquid input pipe, and the bottom of the middle pipeline is closed; the lamp tube is internally provided with an ultraviolet lamp, the lamp tube is made of a material capable of transmitting ultraviolet light, the top of the lamp tube is fixedly connected with the bottom of the middle pipeline, and the lamp tube is also arranged in the outer tube.
Description
Technical Field
The invention relates to the technical field of material preparation devices, in particular to a high-efficiency, simple and convenient microcapsule preparation device based on a microfluidic technology.
Background
The microcapsule has the functions of improving physical properties of substances, improving stability of the substances, controlling release, shielding odor and the like, so that the microcapsule is widely applied to the industrial fields of food, medicines and the like. For example, hollow microspheres with large diameter, thin wall, low surface roughness, uniform spherical shell composition, uniform wall thickness and high sphericity are required to be used as target pellets in an inertial confinement fusion experiment; the food and pharmaceutical industry requires large size capsules that can encapsulate larger doses of core material; the tobacco industry needs to produce brittle explosion beads with larger particle size for flavoring and perfuming. The wide application of the microcapsule promotes the innovation of the microcapsule preparation technology. The preparation methods of the microcapsules are various, such as an encapsulation method (a saturated aqueous solution method), a complex agglomeration method, a spray drying method and the like, but the problems that the encapsulation efficiency is low and the size of the prepared microcapsules cannot be accurately controlled generally exist.
Microfluidics is a science and technology related to a system for processing or manipulating a trace amount of fluid by using a microchannel, has the characteristics of miniaturization, integration and the like, and has the advantages of precision, controllability and the like when an emulsion drop is generated by a microfluidics method, so that the microfluidics is widely applied. The microcapsule prepared by the micro-fluidic method usually takes a core material as an internal phase and a wall material solution as an intermediate phase, wherein the internal phase liquid generates a W/O emulsion under the shearing and extrusion action of the intermediate phase liquid, then flows into an external phase solution to generate a W/O/W double emulsion, and finally the emulsion forms the microcapsule with a core-shell structure under specific conditions (such as ultraviolet light-driven photocrosslinking reaction, interfacial gel reaction and the like). The microcapsule prepared by the micro-fluidic method has the following advantages: the generated microcapsule has an obvious core-shell structure and high encapsulation efficiency, and the size of the microcapsule can be accurately controlled by changing the liquid flow rate, the inner diameter of a microchannel and other methods. Compared with other microcapsule preparation technologies, the microcapsule preparation device has the defects of low production efficiency and incapability of large-scale production, and based on the defect, the patent provides the microcapsule preparation device based on the microfluidic technology.
Disclosure of Invention
The invention aims to solve the problems, and provides an efficient, simple and convenient microcapsule preparation device based on a microfluidic technology, which can generate controllable uniform liquid drops in all directions and all heights simultaneously, and form microcapsules with a core-shell structure under the irradiation of ultraviolet light or other specific conditions, so that the preparation efficiency of the microcapsules is greatly improved, and the problems that the production efficiency of preparing the microcapsules by a microfluidic method is low and large-scale production cannot be carried out are solved.
In order to achieve the purpose, the invention adopts the technical scheme that:
a microcapsule preparation device based on a microfluidic technology comprises an inner pipeline, an intermediate pipeline, an outer pipeline and a lamp tube, wherein the inner pipeline, the intermediate pipeline and the outer pipeline are sequentially sleeved from inside to outside, and gaps are reserved between the inner pipeline and the intermediate pipeline and between the intermediate pipeline and the outer pipeline for allowing an intermediate phase liquid and an outer phase liquid to flow through respectively;
the top of the inner pipeline can be connected with an external inner phase liquid input pipe, the bottom of the inner pipeline is closed, a plurality of liquid outlet holes are formed in the inner pipeline, and micro connecting pipes protruding outwards are arranged on the liquid outlet holes;
the middle pipeline is provided with a plurality of through holes, the through holes correspond to the micro connecting pipes one by one, the outlets of the micro connecting pipes extend into the through holes, the top of the middle pipeline can be connected with an external middle-phase liquid input pipe, and the bottom of the middle pipeline is closed;
the lamp tube is internally provided with an ultraviolet lamp, the lamp tube is made of a material capable of penetrating ultraviolet light, the top of the lamp tube is fixedly connected with the bottom of the middle pipeline, and the lamp tube is also arranged in the outer tube.
Preferably, the device for preparing microcapsules based on the microfluidic technology further comprises an elbow, wherein one end of the elbow is fixedly connected with the bottom of the outer tube, and the other end of the elbow is used for being connected with an external microcapsule collecting device;
the bent pipe is provided with a through hole for inserting the lamp pipe, the top end of the lamp pipe is inserted from the through hole and connected with the bottom of the middle pipeline, and the bottom end of the lamp pipe is exposed outside the bent pipe. The bent pipe is arranged, so that the lamp tube can be conveniently taken out and installed, the lamp tube can be charged or an ultraviolet lamp inside the lamp tube can be replaced, and the outer tube can be conveniently fixed and connected with an external microcapsule collecting device.
Preferably, the liquid outlet holes are uniformly distributed on the inner pipeline from top to bottom, and the liquid outlet holes at the same height are uniformly distributed in a circumferential manner. The number and the size of the liquid outlet holes can be set as required, and microcapsules with uniform sizes can be prepared.
Preferably, the liquid outlet holes in the same height are equal in size, and the liquid outlet holes in different heights are different in size; the liquid outlet holes at different heights are correspondingly arranged from top to bottom and are distributed on the same straight line; so that the processing is convenient and the flow compensation is convenient.
Preferably, the middle pipeline is of a detachable structure and comprises a left half pipe and a right half pipe which are symmetrically arranged; the upper part and the lower part of the middle pipeline are provided with screw holes for connecting the left half pipe and the right half pipe, and the left half pipe and the right half pipe are provided with sealing gaskets. The detachable structure is convenient to install and clean.
Preferably, the lamp tube is made of glass; better transmitting ultraviolet light to irradiate the liquid drop;
the top of the outer pipeline is connected with an outer-phase liquid input pipe, and the bottom of the outer pipeline is connected with a microcapsule collecting device;
the top of the middle pipeline is used for being connected with a middle-phase liquid input pipe, and the bottom of the middle pipeline is used for being fixedly connected with the bottom of the inner pipeline and the top of the lamp tube;
the top of the inner pipeline is used for being connected with an inner phase liquid input pipe, and the bottom of the inner pipeline is used for being fixedly connected with the bottom of the middle pipeline.
Preferably, an inner pipe base is arranged at the bottom of the inner pipe, a positioning pin hole is formed in the inner pipe base, and the inner pipe, the middle pipe and the lamp tube are fixedly connected through a positioning pin. The inner pipeline, the middle pipeline and the lamp tube can be fixed by the same set of positioning pins, the structural design is simple and reasonable, and the lamp tube is convenient to manufacture, install and disassemble.
The invention also provides a preparation method of the microcapsule based on the microfluidic technology, which is prepared by adopting the device of any one of the above steps and comprises the following steps: the top of the outer pipeline is connected with an external phase liquid input pipe, the top of the middle pipeline is connected with a middle phase liquid input pipe, the top of the inner pipeline is connected with an internal phase liquid input pipe, the ultraviolet lamp is turned on, the external device is turned on to simultaneously input external phase, middle phase and internal phase liquid, the internal phase flows out through the micro connecting pipe, double liquid drops with the middle phase wrapping the internal phase are formed at through holes of the middle pipeline, the double liquid drops flow into the external phase in the outer pipeline and are instantly solidified into microcapsules under the irradiation of the ultraviolet lamp.
In the above technical solution, the intermediate phase liquid contains a photoinitiator substance, such as 184 photoinitiator.
The beneficial effects of the invention are: the device has multiple and adjustable micro-channels, 2 or more than 2 insoluble liquids are prepared into double emulsion, and a proper curing mode is selected for curing according to the characteristics of intermediate phase substances, so that the capsules with uniform particle size, round particles and high encapsulation efficiency are prepared. The device has a simple structure, can quickly generate the microcapsule with uniform and controllable particle size, high encapsulation rate, wide application range of wall material core materials and high capsule preparation efficiency, can well solve the pain point of the existing microcapsule preparation method, and promotes the production and the wide application of the microcapsule.
Drawings
Fig. 1 is a structural sectional view of a microcapsule preparation apparatus based on microfluidic technology according to the present invention.
Fig. 2 is a schematic perspective view of the inner pipe of fig. 1.
Fig. 3 is a cross-sectional view of the innerduct of fig. 1.
Fig. 4 is a perspective view of the intermediate duct of fig. 1.
Fig. 5 is an enlarged view of a connection relationship between the inner pipe and the intermediate pipe in fig. 1.
Fig. 6 is a cross-sectional view of the upper part of the micro-capsule preparing apparatus based on the micro-fluidic technology of fig. 1.
Fig. 7 is an enlarged view of the fixed connection relationship among the inner pipe, the intermediate pipe and the lamp tube.
FIG. 8 is a schematic view of the connection of the elbow to the outer conduit and the lamp tube of the device of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, but the present invention is not limited thereby. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The experimental procedures in the following examples are conventional unless otherwise specified.
Example 1
A microcapsule preparation apparatus based on microfluidic technology, as shown in fig. 1-7, mainly consists of an inner pipe 1, an intermediate pipe 2, an outer pipe 3 and a lamp tube 4. The inner pipeline 1, the middle pipeline 2 and the outer pipeline 3 are sequentially sleeved from inside to outside, and gaps are reserved between the inner pipeline 1 and the middle pipeline 2 and between the middle pipeline 2 and the outer pipeline 3 for the circulation of middle-phase liquid and outer-phase liquid respectively;
the top of the inner pipeline 1 can be connected with an external inner phase liquid input pipe, the bottom of the inner pipeline is closed, a plurality of liquid outlet holes 11 are formed in the inner pipeline 1, and micro connecting pipes 12 protruding outwards are arranged on the liquid outlet holes 11; the micro-connecting tube 12 can be fixedly connected to the liquid outlet hole 11 by welding.
The middle pipeline 2 is provided with a plurality of through holes 21, the through holes 21 correspond to the micro connecting pipes 12 one by one, the outlets of the micro connecting pipes 12 extend into the through holes 21, the top of the middle pipeline 2 can be connected with an external middle-phase liquid input pipe, and the bottom of the middle pipeline is closed;
be provided with ultraviolet lamp 41 in the lamps and lanterns pipe 4, the material of lamps and lanterns pipe 4 is the material that can see through the ultraviolet ray, and the top of lamps and lanterns pipe 4 and the bottom fixed connection of middle pipeline 2, lamps and lanterns pipe 4 also sets up in outer pipeline 3.
In some embodiments, the apparatus for preparing microcapsules based on microfluidic technology of the present invention further comprises an elbow 5, as shown in fig. 8, one end of the elbow 5 is fixedly connected to the bottom of the outer pipe 3, and the other end is used for connecting to an external microcapsule collecting apparatus;
the elbow pipe 5 is provided with a through hole 51 for inserting the lamp tube 4, the top end of the lamp tube 4 is inserted from the through hole 51 and connected with the bottom of the middle pipeline 2, and the bottom end is exposed outside the elbow pipe 5.
In some embodiments, the liquid outlet holes 11 are uniformly distributed on the inner pipe 1 from top to bottom, and the liquid outlet holes 11 at the same height are uniformly distributed circumferentially.
Because of the pressure drop during the flow through the conduit, the flow through the orifices of different heights is different, resulting in different sizes of the droplets produced, and the following compensation mechanisms can be used to make the droplets produced uniform in size, as exemplified below:
firstly, the aperture of liquid outlet holes 11 with different heights of the inner pipeline 1 is adjusted according to the requirement, and the aperture adjustment of through holes 21 of the middle pipeline 2 is consistent with the aperture adjustment of the liquid outlet holes 11 of the inner pipeline 1;
secondly, the wall thickness of the intermediate pipe 2 is adjusted as required, for example, thicker at the higher height through holes 21, to increase the on-way resistance and compensate for the effect of pressure drop.
Thirdly, the compensation is performed in a manner of combining the first and second manners.
Therefore, in some embodiments, the sizes of the liquid outlet holes 11 located at the same height on the inner pipe 1 are equal, and the sizes of the liquid outlet holes 11 located at different heights are different; the liquid outlet holes 11 at different heights are correspondingly arranged from top to bottom and distributed on the same straight line. Therefore, the pipeline can be conveniently processed and manufactured and the flow compensation is convenient.
In some embodiments, the intermediate pipe 2 is a detachable structure, comprising a left half pipe and a right half pipe which are symmetrically arranged;
the upper part and the lower part of the middle pipeline 2 are provided with screw holes 22 for connecting the left half pipe and the right half pipe, and the left half pipe and the right half pipe are provided with sealing gaskets.
Preferably, the lamp tube 4 is made of glass;
the top of the outer pipeline 3 is used for being connected with an outer phase liquid input pipe, and the bottom of the outer pipeline is used for being connected with a microcapsule collecting device;
the top of the middle pipeline 2 is used for being connected with a middle-phase liquid input pipe, and the bottom of the middle pipeline is used for being fixedly connected with the bottom of the inner pipeline 1 and the top of the lamp tube 4;
the top of the inner pipe 1 is used for connecting with an inner phase liquid input pipe, and the bottom is used for fixedly connecting with the bottom of the middle pipe 2.
In some embodiments, the bottom of the inner pipe 1 is provided with an inner pipe base 13, the inner pipe base 13 is provided with a positioning pin hole, and the inner pipe 1, the middle pipe 2 and the lamp tube 4 are fixedly connected through a positioning pin 6.
The device of the invention prepares 2 or more than 2 insoluble liquids into double emulsion based on the microfluidic technology, and selects a proper curing mode to cure according to the characteristics of mesophase substances, thereby preparing the microcapsule with uniform grain diameter, round grains and high encapsulation efficiency.
Example 2 preparation method of microcapsule based on microfluidic technology
The micro-capsule preparation device based on the micro-fluidic technology in example 1 is used for preparing micro-capsules based on the micro-fluidic technology, and the operation is carried out according to the following steps:
the top of the outer pipeline 3 is connected with an external phase liquid input pipe, the top of the middle pipeline 2 is connected with a middle phase liquid input pipe, the top of the inner pipeline 1 is connected with an internal phase liquid input pipe, the ultraviolet lamp 41 is turned on, the external device is turned on to input external phase, middle phase and internal phase liquid at the same time, the internal phase flows out through the micro connecting pipe 12, double liquid drops of which the middle phase wraps the internal phase are formed at the through hole 21 of the middle pipeline 2, the double liquid drops flow into the external phase in the outer pipeline 3 and are instantly cured into microcapsules under the irradiation of the ultraviolet lamp 41. The intermediate phase liquid contains a photoinitiator substance.
The method can be used for producing water-in-oil-in-water (W/O/W) double emulsion.
The inner phase liquid flows through the micro connecting pipe 12 through the liquid outlet hole 11, and at the outlet of the micro connecting pipe 12, namely at the through hole 21 of the middle pipeline 2, due to the flowing shearing force and the gravity, double liquid drops of the inner phase liquid are wrapped by the middle phase liquid and flow into the outer phase liquid in the outer pipeline 3. As the intermediate phase liquid contains photoinitiator substances, under the irradiation of ultraviolet light, the intermediate phase epoxy acrylate generates a rapid polymerization reaction under the action of the photoinitiator, the capsule shell layer can be cured to form microcapsules within a few seconds, and the formed microcapsules flow out through the outer pipeline 3 and finally enter the microcapsule collection device.
Claims (6)
1. A microcapsule preparation device based on a microfluidic technology is characterized in that: the lamp comprises an inner pipeline (1), a middle pipeline (2), an outer pipeline (3), a lamp tube (4) and a bent tube (5), wherein the inner pipeline (1), the middle pipeline (2) and the outer pipeline (3) are sequentially sleeved from inside to outside, and gaps are reserved between the inner pipeline (1) and the middle pipeline (2) and between the middle pipeline (2) and the outer pipeline (3) respectively for circulation of middle-phase liquid and outer-phase liquid;
the top of the outer pipeline (3) is used for being connected with an outer-phase liquid input pipe; the top of the middle pipeline (2) is connected with a middle-phase liquid input pipe, and the bottom of the middle pipeline is fixedly connected with the bottom of the inner pipeline (1) and the top of the lamp tube (4); the top of the inner pipeline (1) is used for being connected with an inner phase liquid input pipe, and the bottom of the inner pipeline is used for being fixedly connected with the bottom of the middle pipeline (2);
the bottom of the inner pipeline (1) is closed, a plurality of liquid outlet holes (11) are formed in the inner pipeline (1), the liquid outlet holes (11) are uniformly distributed in the inner pipeline (1) from top to bottom, and micro connecting pipes (12) protruding outwards are arranged on the liquid outlet holes (11); the liquid outlet holes (11) at the same height on the inner pipeline (1) are uniformly distributed in a circumferential manner, the liquid outlet holes (11) at the same height are equal in size, and the liquid outlet holes (11) at different heights are different in size; the liquid outlet holes (11) at different heights are correspondingly arranged from top to bottom and are distributed on the same straight line;
the middle pipeline (2) is provided with a plurality of through holes (21), the through holes (21) correspond to the micro connecting pipes (12) one by one, the outlets of the micro connecting pipes (12) extend into the through holes (21), the top of the middle pipeline (2) can be connected with an external middle-phase liquid input pipe, and the bottom of the middle pipeline is closed; the wall thickness of the intermediate pipe (2) is thicker at the through hole (21) with higher height;
an ultraviolet lamp (41) is arranged in the lamp tube (4), the lamp tube (4) is made of a material capable of transmitting ultraviolet light, the top of the lamp tube (4) is fixedly connected with the bottom of the middle pipeline (2), and the lamp tube (4) is also arranged in the outer pipeline (3);
one end of the bent pipe (5) is fixedly connected with the bottom of the outer pipeline (3), and the other end of the bent pipe is used for being connected with an external microcapsule collecting device; the bent pipe (5) is provided with a through hole (51) for inserting the lamp tube (4), the top end of the lamp tube (4) is inserted from the through hole (51) and connected with the bottom of the middle pipeline (2), and the bottom end of the lamp tube is exposed out of the bent pipe (5).
2. The microfluidic-technology-based microcapsule preparation apparatus according to claim 1, wherein: the middle pipeline (2) is of a detachable structure and comprises a left half pipe and a right half pipe which are symmetrically arranged;
the upper part and the lower part of the middle pipeline (2) are provided with positioning screw holes (22) for connecting the left half pipe and the right half pipe, and the left half pipe and the right half pipe are provided with sealing gaskets.
3. Microfluidic technology based microcapsule preparation apparatus according to claim 1, characterized in that:
the lamp tube (4) is made of glass.
4. Microfluidic technology based microcapsule preparation apparatus according to claim 1, characterized in that: an inner pipeline base (13) is arranged at the bottom of the inner pipeline (1), a positioning pin hole is formed in the inner pipeline base (13), and the inner pipeline (1), the middle pipeline (2) and the lamp tube (4) are fixedly connected through a positioning pin (6).
5. A method for preparing microcapsules based on a microfluidic technology is characterized by comprising the following steps: prepared using the device of any one of claims 1 to 4, comprising the steps of: the top of an outer pipeline (3) is connected with an external phase liquid input pipe, the top of an intermediate pipeline (2) is connected with an intermediate phase liquid input pipe, the top of an inner pipeline (1) is connected with an internal phase liquid input pipe, an ultraviolet lamp (41) is turned on, an external device is turned on to simultaneously input external phase, intermediate phase and internal phase liquid, the internal phase flows out through a micro connecting pipe (12), double liquid drops of which the intermediate phase wraps the internal phase are formed at a through hole (21) of the intermediate pipeline (2), the double liquid drops flow into the external phase in the outer pipeline (3), and are instantly cured into microcapsules under the irradiation of the ultraviolet lamp (41).
6. The method of claim 5, wherein: the intermediate phase liquid contains a photoinitiator substance.
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| CN102794119B (en) * | 2011-05-26 | 2014-08-20 | 北京化工大学 | Method for preparing monodisperse emulsion |
| CN103721655B (en) * | 2014-01-06 | 2015-12-09 | 武汉理工大学 | A kind of size uniformity and the preparation method of the controlled chitosan microcapsules of size |
| CN106040115B (en) * | 2016-07-05 | 2018-10-09 | 中国工程物理研究院激光聚变研究中心 | A kind of dual milk particle generating means of three hole coaxial-types |
| CN109201130B (en) * | 2018-08-31 | 2020-06-02 | 广东工业大学 | Double-emulsification glass capillary micro-fluidic chip and phase-change microcapsule prepared by same |
| CN112371065B (en) * | 2020-11-19 | 2021-11-09 | 西安交通大学 | Method for generating magnetic core-shell microcapsules based on surface acoustic wave microfluidic device |
| CN112593302A (en) * | 2020-12-28 | 2021-04-02 | 南京鼓楼医院 | Microfluidic spinning device, spiral core-shell structure conductive fiber, and preparation method and application thereof |
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