CN114271538A - Device and method for preparing phase-change microcapsules by microfluidics technology - Google Patents

Device and method for preparing phase-change microcapsules by microfluidics technology Download PDF

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Publication number
CN114271538A
CN114271538A CN202111444300.5A CN202111444300A CN114271538A CN 114271538 A CN114271538 A CN 114271538A CN 202111444300 A CN202111444300 A CN 202111444300A CN 114271538 A CN114271538 A CN 114271538A
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needle
injection pump
phase fluid
hose
syringe
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丁党
冯源
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Hefei Zhongke Carbon Micro Technology Co ltd
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Hefei Zhongke Carbon Micro Technology Co ltd
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Abstract

The invention discloses a device and a method for preparing phase-change microcapsules by a microfluidics technology, which belong to the technical field of bead blasting for cigarettes, and comprise an inner needle head 1, an outer needle head 2 cavity 3, an injection pump A4A, an injection pump B4B and an injection pump C4C, wherein the inner needle head 1 is embedded in the outer needle head 2, and the outer needle head 2 is fixed in the cavity 3 through a rubber plug; the injection pump A4A is connected with the inner needle 1 through a hose, the injection pump B4B is connected to a gap between the inner needle 1 and the outer needle 2 through a hose, and the injection pump C4C is connected with the driving outlet small hole through a hose. The invention forms a stable cone-jet structure after being focused by the small holes, and the jet is broken into monodisperse liquid drops due to instability. The prepared microcapsule for cigarettes has the advantages of high production rate, high wrapping rate, uniform and controllable particle size, good balling performance and stable quality. Can solve the problems of high preparation cost, poor quality stability and the like of the essential oil microcapsules for the cigarettes in the prior art.

Description

Device and method for preparing phase-change microcapsules by microfluidics technology
Technical Field
The invention relates to the technical field of bead blasting for cigarettes, in particular to a device and a method for preparing phase-change microcapsules by a microfluid technology.
Background
With the continuous deepening of harm reduction and tar reduction, the partial loss of the aroma quality and the aroma quantity of the cigarettes is inevitably caused, and the smoking taste is influenced. Therefore, the method for improving the taste of the cigarette by directly adding the essence is an effective method for improving the taste of the cigarette. The existing essence adding method mainly comprises the steps of adding essence into tobacco shreds or adding essence-adhered fragrant threads into filter tips, and the two methods have the defects of short essence retention time, uneven essence release and the like. In order to solve the problems caused by directly adding essence, the micro-capsule for tobacco, namely the essence, is an important innovation direction for the tobacco industry at home and abroad. Essence is wrapped in a wall material with extremely high stability, and the diameter of the prepared explosion bead is controlled to be several millimeters to hundreds of micrometers. The microcapsule for cigarette can be added into cigarette tube to improve cigarette quality by slow release of microcapsule for cigarette or added into cigarette filter to release perfume by breaking bead blasting by suction.
The patent application No. CN201810533533.4 discloses a preparation method of the water-containing blasting bead for the cigarette. A plurality of semicircular plastic grooves are formed in a plastic film in a thermoplastic mode, crystal ice balls are placed in the plastic grooves and then covered by the plastic film, the two layers of films are fused together to form plastic sheets containing exploded beads, the plastic sheets are cut, the exploded bead parts are reserved and transferred into an oven, and the inside of the plastic sheets is melted. I.e. to form a water-filled plastic sheet. The water-containing plastic sheet prepared by the patent is complex in cutting, large in cutting, uneven in size and poor in rounding, and the material application range of the method is narrow, so that the method is not suitable for preparing most essential oil microcapsules. The application number CN201910909300.4 patent document discloses a preparation method of coffee flavor type pops for cigarettes, which is to dissolve coffee essence in an oily solvent, then prepare microspheres containing the coffee essence together with a sodium alginate solution and a calcium chloride solution, then place the microspheres in a crosslinking solution (chitosan or potassium persulfate solution is helpful for forming a film on the surfaces of the microspheres) for crosslinking for 20-40min, and then dehydrate and dry the microspheres to obtain the coffee flavor type pops for cigarettes. The caffeine flavor type tobacco microcapsule prepared by the ionic crosslinking method is high in production efficiency and good in product quality stability. But the preparation conditions are complex, the control parameters are more, the particle size cannot be accurately controlled, the monodispersity of the product is poor, agglomeration and other phenomena are easy to occur, and the wrapping rate is low.
Therefore, the preparation method of the tobacco microcapsule with high wrapping rate, good monodispersity, controllable particle size, good circularity and stable quality has great attention on the preparation scheme of the tobacco microcapsule with simple and easy operation of the preparation device, low production cost, high production efficiency and wide material adaptability.
Disclosure of Invention
In view of the problems in the prior art, the present invention is to provide a device and a method for preparing phase-change microcapsules by microfluidics technology, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a phase-change microcapsule preparation device adopting microfluidics technology comprises an inner needle, an outer needle cavity chamber, an injection pump A, an injection pump B and an injection pump C, wherein the inner needle is embedded in the outer needle, the inner needle and the outer needle are coaxially arranged, and the outer needle is fixed in the cavity chamber through a rubber plug; the hollow chamber is provided with a driving outlet small hole and a hose connecting small hole;
the injection pump A is connected with the inner needle through a hose to provide an inner phase fluid; the injection pump B is connected to the gap between the inner needle head and the outer needle head through a hose to provide an external phase fluid; syringe pump C is connected to the drive outlet orifice by a flexible tube to provide the drive phase fluid.
The invention provides a tobacco tar microcapsule preparation method based on a flow focusing technology, which comprises the following steps:
(1) the inner needle is embedded in the outer needle to form a coaxial needle which is fixed in the cavity chamber through the rubber plug;
(2) the injection pump A is connected with the inner needle head through a hose, the injection pump B is connected to a gap between the inner needle head and the outer needle head through a hose, the injection pump C is connected with a small driving outlet hole through a hose, firstly, the driving phase fluid is regulated through the injection pump C, so that the driving phase fluid fills a cavity chamber, secondly, the injection pump A is regulated, so that the internal phase fluid is injected into the inner needle head, the injection pump B is regulated to inject the external phase fluid between the inner needle head and the outer needle head, and when stable cone-jet flow is formed, a sample starts to be collected;
(3) regulating the rotating speeds of three injection pumps, namely an injection pump A, an injection pump B and an injection pump C, regulating the flow rate of the injection pump A to be 10-30ml/h, regulating the flow rate of the injection pump B to be 10-30ml/h, and regulating the flow rate of the injection pump C to be 400-500 ml/h;
(4) the culture dish is used for collecting double emulsion drops, is placed below the cavity chamber and is opposite to the small hole of the driving phase outlet;
(5) placing the culture dish containing double emulsion droplets on a shaking table, adjusting the rotation speed of the shaking table to 20-80r/min, and irradiating with an ultraviolet lamp arranged above one side of the shaking table 7 after 1 min;
(6) after the wall materials are completely solidified, washing the wall materials with clear water for three times, and naturally drying the wall materials at room temperature;
(7) the sample was collected.
As a further scheme of the invention: the inner phase fluid is tobacco tar 6672, the outer phase fluid is ETPTA, and the driving phase fluid is PVA
As a further scheme of the invention: the ETPTA preparation needs to add ethanol with the same volume and a photoinitiator (2-hydroxy-2-methyl-1-phenyl-1-acetone) accounting for 1 percent of the total volume, and the concentration of the polyvinyl alcohol is 1 to 3 percent.
Compared with the prior art; the invention has the beneficial effects that: the invention solves the problem that the particle size can not be accurately controlled by an emulsification method, an in-situ polymerization method and the like, and the preparation of the microcapsule products for cigarettes with different particle sizes (the particle size range is hundreds of microns-millimeters) can be realized only by adjusting the three-phase flow; the micro-droplet is formed because the disturbance is continuously increased and the fluid interface is finally cut off, and the surface tension and other acting forces are almost in the same magnitude in the process, so that the micro-droplet with good monodispersity can be obtained; the driving phase fluid provides shearing acting force, so that two interfaces (three layers of fluid form two layers of interfaces) are coaxially stretched, the outer layer of fluid wraps the inner layer of fluid and moves in the same direction to form coaxial jet flow, and double-emulsion micro-droplets with high wrapping rate can be obtained theoretically; the frequency of generation of double emulsion micro-droplets was calculated to be 106-108HZ, high production efficiency and suitability for industrial production; theoretically, as long as the inner phase fluid and the outer phase fluid are not mutually soluble, micro-packaging can be realized, so that the micro-packaging material can be used for micro-packaging of different tobacco essence materials, and the material adaptability is wide.
Drawings
FIG. 1 is a schematic structural diagram of a phase-change microcapsule preparation device by microfluidics.
FIG. 2 is a microscope photograph of the present invention using a coaxial capillary to make a double emulsion droplet of tobacco tar 6672;
in the figure: 1. an inner needle head; 2. an outer needle; 3. a hollow chamber; 4A, an injection pump A; 4B, an injection pump B; 4C, an injection pump C; 5A, an internal phase fluid; 5B, external phase fluid; 5C, driving phase fluid; 6. a culture dish; 7. shaking table; 8. ultraviolet lamp.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; rather than all embodiments. According to the embodiment of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "provided," "connected," and "connected" are to be construed broadly; for example, the two elements may be fixedly connected, detachably connected, or integrally connected, mechanically connected, electrically connected, directly connected, indirectly connected through an intermediate medium, or communicated with each other. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1-2, a phase-change microcapsule preparation apparatus using microfluidics comprises an inner needle 1, an outer needle 2, a hollow chamber 3, a syringe pump A4A, a syringe pump B4B, a syringe pump C4C, an inner phase fluid 5A, an outer phase fluid 5B, a driving phase fluid 5C, a petri dish 6, a shaker 7 and a purple light 8, wherein the inner needle 1 is embedded in the outer needle 2 and keeps a good coaxiality, and the outer needle 2 is fixed in the hollow chamber 3 through a rubber plug; the cavity chamber 3 is provided with a driving outlet small hole and a hose connecting small hole, and except the driving outlet small hole and the hose connecting small hole, the sealing performance of other positions is good;
the syringe pump A4A is connected with the inner needle 1 through a hose to provide an inner phase fluid 5A; a syringe pump B4B is connected to the space between the inner needle 1 and the outer needle 2 through a hose to provide an outer phase fluid 5B; syringe pump C4C is connected to the drive outlet orifice by a hose to provide drive phase fluid 5C;
the inner phase fluid 5A is tobacco tar 6672 (one of tobacco essence), is not limited to the essence material, and can be used as the inner core essence material as long as the inner phase fluid 5A and the outer phase fluid 5B are insoluble with each other theoretically; the external phase fluid 5B is ETPTA (one kind of light-cured adhesive), is not limited to the material of the outer shell, and theoretically can be used as the material of the wall as long as the external phase fluid 5B and the internal phase fluid 5A are immiscible with each other; the driving phase fluid 5C is PVA (polyvinyl alcohol), the concentration is 1% -3%, on one hand, the effect of stabilizing the cone shape is achieved, on the other hand, the shearing force is provided, so that two interfaces (three layers of fluid form two layers of interfaces) are coaxially stretched, the outer layer fluid wraps the inner layer fluid to move in the same direction to form coaxial jet flow, then disturbance is transmitted, according to the instability theory, the disturbance with large growth rate leads the flow field along with the increase of the disturbance transmission, the fluid interface is finally cut off along with the continuous increase of the disturbance, and the discretized small-scale double-emulsion micro-droplets are formed; the culture dish is positioned right below the driving phase outlet small hole and is used for receiving the double-emulsion micro-droplets; the shaking table is used for providing centrifugal force to avoid the eccentricity of the inner core; the ultraviolet lamp is positioned above the shaking table and excites ETPTA to crosslink so as to solidify into a shell.
The invention provides a tobacco tar microcapsule preparation method based on a flow focusing technology, which comprises the following steps:
(1) the inner needle head 1 is embedded into the outer needle head 2 to form a coaxial needle head which is fixed in the cavity chamber 3 through a rubber plug;
(2) syringe pump A4A is connected to inner needle 1 by a hose, syringe pump B4B is connected to the space between inner needle 1 and outer needle 2 by a hose, syringe pump C4C is connected to the drive outlet orifice by a hose, first drive phase fluid 5C is regulated by syringe pump C4C to fill empty chamber 3 with drive phase fluid, second inner phase fluid 5A is injected into inner needle 1 by syringe pump A4A, outer phase fluid 5B is injected between inner needle 1 and outer needle 2 by syringe pump B4B, and when a stable cone-jet is formed, collection of sample is started;
(3) the rotational speeds of three injection pumps, namely an injection pump A4A, an injection pump B4B and an injection pump C4C are adjusted, the flow rate of the injection pump A4A is adjusted to be 10-30ml/h, the flow rate of the injection pump B4B is adjusted to be 10-30ml/h, and the flow rate of the injection pump C4C is adjusted to be 400-500 ml/h;
(4) the culture dish 6 is used for collecting double emulsion drops, is placed below the hollow chamber 3 and is opposite to the small driving phase outlet hole;
(5) placing the culture dish 6 containing double emulsion droplets on a shaking table 7, adjusting the rotation speed of the shaking table 7 to 20-80r/min, and irradiating for 1min by using an ultraviolet lamp 8 arranged above one side of the shaking table 7;
(6) after the wall materials are completely solidified, washing the wall materials with clear water for three times, and naturally drying the wall materials at room temperature;
(7) the sample was collected.
When inside and outside syringe needle inlay, interior syringe needle will surpass outer syringe needle 0.2mm for inlayer liquid is in more steady outer fluid, guarantees simultaneously that inside and outside syringe needle possesses good axiality. The bottom of the coaxial needle is opposite to the small hole of the driving phase outlet and is spaced by about 1 mm.
The three-phase flow is regulated by firstly regulating the driving phase fluid 5C to make the driving liquid fill the cavity chamber 3, secondly regulating the inner phase fluid 5A and the outer phase fluid 5B, and when a stable cone-jet flow is formed, starting to collect a sample.
The diameter range of the driving outlet small hole is 350-550 mu m, the edge of the hole is smooth, and no burr is generated.
Wall material cure time is related to the shell thickness of the double emulsion droplets, and in general, cure time can increase trimethylolpropane ethoxylate triacrylate crosslink density. When the wall thickness of two emulsion drops was 30um, curing time was 6 seconds, and when the wall thickness was 50um, curing time was 12 seconds.
The ETPTA preparation needs to add ethanol with the same volume and a photoinitiator (2-hydroxy-2-methyl-1-phenyl-1-acetone) accounting for 1 percent of the total volume, and the concentration of the polyvinyl alcohol is 1 to 3 percent.
Compared with the prior art, the method solves the problem that the particle size cannot be accurately controlled by an emulsification method, an in-situ polymerization method and the like, and can realize the preparation of the microcapsule products for cigarettes with different particle sizes (the particle size range is hundreds of microns-millimeters) only by adjusting the three-phase flow; the micro-droplet is formed because the disturbance is continuously increased and the fluid interface is finally cut off, and the surface tension and other acting forces are almost in the same magnitude in the process, so that the micro-droplet with good monodispersity can be obtained; the driving phase fluid provides shearing acting force, so that two interfaces (three layers of fluid form two layers of interfaces) are coaxially stretched, the outer layer of fluid wraps the inner layer of fluid and moves in the same direction to form coaxial jet flow, and double-emulsion micro-droplets with high wrapping rate can be obtained theoretically; the frequency of double emulsion microdroplet generation was calculated to be 106-108HZ, high production efficiency and suitability for industrial production; theoretically, as long as the requirement that the inner phase fluid and the outer phase fluid are not mutually soluble is met, micro-packaging can be realized, so that the micro-packaging material can be used for micro-packaging of different tobacco essence materials, and the material adaptability is wide.
To those skilled in the art; it is obvious that the invention is not restricted to the details of the above-described exemplary embodiments; and without departing from the spirit or essential characteristics of the invention; the invention can be embodied in other specific forms. Thus; from whatever point; the embodiments should be considered as exemplary; and is not limiting; the scope of the invention is indicated by the appended claims rather than by the foregoing description; all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore; it should be understood that; although the present description has been described in terms of embodiments; but not every embodiment contains only a single solution; this manner of description is by way of clarity only; the person skilled in the art will consider the description as a whole; the technical schemes in the embodiments can also be combined appropriately; forming other embodiments that will be understood by those skilled in the art.

Claims (4)

1. A microfluidics phase-change microcapsule preparation device and method, including inner syringe needle (1), outer syringe needle (2) cavity (3), syringe pump A (4A), syringe pump B (4B) and syringe pump C (4C), characterized by that, the said inner syringe needle (1) imbeds and sets up in the outer syringe needle (2), inner syringe needle (1) and outer syringe needle (2) are coaxial to set up, the outer syringe needle (2) is fixed in cavity (3) through the rubber plug;
the hollow chamber (3) is provided with a driving outlet small hole and a hose connecting small hole;
the injection pump A (4A) is connected with the inner needle (1) through a hose to provide an inner phase fluid (5A); the injection pump B (4B) is connected to the gap between the inner needle (1) and the outer needle (2) through a hose to provide an outer phase fluid (5B); the syringe pump C (4C) is connected to the drive outlet orifice by a hose to provide a drive phase fluid (5C).
2. A method for preparing phase-change microcapsules by a microfluidics technology is characterized by comprising the following steps:
s1, embedding the inner needle (1) into the outer needle (2) to form a coaxial needle which is fixed in the cavity chamber (3) through the rubber plug;
s2, connecting a syringe pump A (4A) with an inner needle (1) through a hose, connecting a syringe pump B (4B) with a gap between the inner needle (1) and an outer needle (2) through a hose, connecting a syringe pump C (4C) with a driving outlet small hole through a hose, firstly adjusting a driving phase fluid (5C) through the syringe pump C (4C) to fill a cavity chamber (3) with the driving phase fluid (5C), secondly adjusting the syringe pump A (4A) to inject an inner phase fluid (5A) into the inner needle (1), adjusting the syringe pump B (4B) to inject an outer phase fluid (5B) between the inner needle (1) and the outer needle (2), and starting to collect a sample when a stable cone-jet flow is formed;
s3, adjusting the rotating speeds of three injection pumps, namely an injection pump A (4A), an injection pump B (4B) and an injection pump C (4C), adjusting the flow rate of the injection pump A (4A) to be 10-30ml/h, the flow rate of the injection pump B (4B) to be 10-30ml/h and the flow rate of the injection pump C (4C) to be 400-500 ml/h;
s4, placing the culture dish (6) used for collecting the double emulsion drops below the empty chamber (3) and opposite to the small hole of the driving phase outlet;
s5, placing the culture dish (6) with the double-emulsion drops on a shaking table (7), adjusting the rotating speed of the shaking table (7) to be 20-80r/min, and irradiating the culture dish with an ultraviolet lamp (8) arranged above one side of the shaking table (7) after 1 min;
s6, after the wall material is completely solidified, washing the wall material with clean water for three times, and naturally drying the wall material at room temperature;
s7, collecting the sample.
3. The method for preparing phase-change microcapsules according to claim 2, wherein the internal phase fluid (5A) is tobacco tar 6672, the external phase fluid (5B) is ETPTA, and the driving phase fluid (5C) is PVA.
4. The method for preparing phase-change microcapsules by microfluidics technology according to claim 3, wherein the ETPTA formulation requires the addition of the same volume of ethanol and 1% of photoinitiator (2-hydroxy-2-methyl-1-phenyl-1-propanone) based on the total volume, and the concentration of polyvinyl alcohol is 1-3%.
CN202111444300.5A 2021-11-30 2021-11-30 Device and method for preparing phase-change microcapsules by microfluidics technology Pending CN114271538A (en)

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