CN113952892A - Method for preparing suspended micro-droplets by utilizing negative pressure - Google Patents
Method for preparing suspended micro-droplets by utilizing negative pressure Download PDFInfo
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- CN113952892A CN113952892A CN202111465340.8A CN202111465340A CN113952892A CN 113952892 A CN113952892 A CN 113952892A CN 202111465340 A CN202111465340 A CN 202111465340A CN 113952892 A CN113952892 A CN 113952892A
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
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Abstract
The invention provides a method for preparing suspended micro-droplets by using negative pressure, which comprises the following steps: oily substances are introduced from the bottom of the suspension micro-droplet preparation device as an internal phase, and a water phase is introduced from the side as an external phase; the water phase moves upwards in an external circular ring shape under the action of negative pressure and forms accelerated motion through a conical channel; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the conical channel after passing through the hollow column, and the oily substance forms suspended micro-droplets under the action of the surface tension and the viscous force of the two-phase solution. The particles prepared by the method have high sphericity, are not fused with each other, save cost, are convenient to collect, and can overcome the influence of gravity on particle deformation.
Description
Technical Field
The invention relates to the technical field of liquid drops, in particular to a method for preparing suspended micro-liquid drops by utilizing negative pressure.
Background
The micro-droplet technology has attracted much attention by virtue of its important influence in the scientific research field and special application in the engineering field. Researchers have proposed many methods of forming nearly monodisperse micro-droplets, such as drip bibs, nozzle releases, microfluidic technologies, and the like.
Among these techniques, droplet microfluidics is the most common method, and can be used in food delivery, drug delivery, chemical reactions, health monitoring, and other fields of biological analysis. In general, there are three typical geometries that can be used to generate microdroplets: t-shaped pipeline, flow focusing pipeline and coaxial flow pipeline, wherein the flow focusing pipeline can realize the formation of micro-droplet sequences in a wide volume range.
CN208161617U discloses a controllable micro-droplet generating device, in which a first micro-sampler is connected with a dispersed phase inlet of a micro-fluidic chip through a dispersed phase pipeline, and a second micro-sampler is connected with a continuous phase inlet of the micro-fluidic chip through a continuous phase pipeline; the outlet of the micro-fluidic chip is connected with the collecting bottle through an outlet pipeline; the dispersed phase pipeline is provided with a mechanical vibrator which can enable the pipeline to vibrate, and the vibration frequency and amplitude of the mechanical vibrator are controllable; the first microsyringe is driven by a first syringe pump and the second microsyringe is driven by a second syringe pump.
CN109569344A discloses a method for preparing suspended micro-droplets by using a microfluidic device, which selects any oily substance as an internal phase and a solution containing a surfactant and having shear thinning property as an external phase. At the outlet of the internal phase channel of the microfluidic device, the internal phase solution forms micro-droplets under the combined action of the surface tension and the viscous force of the two-phase solution. Then, a solution for gelling the external phase is introduced at the outlet of the external phase channel of the microfluidic device. The gelled external phase solution has shear thinning properties. In the absence of shear forces, the droplets of the inner phase can remain in a fixed position in three-dimensional space for a long period of time.
However, the droplets prepared in the above devices and systems still have the problems of insufficient droplet uniformity and insufficient circularity, and thus, it is necessary to develop a more excellent method for forming micro droplets.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a method for preparing suspended micro-droplets by using negative pressure, which replaces the traditional pump driving mode, and the negative pressure can overcome the deformation influence of gravity on the droplets by forming the droplets in the vertical direction; but also can avoid the adverse effect that the traditional driving pump leads to the liquid drop to warp in the horizontal direction, and whole liquid drop size is little and even, and the time of depositing is long.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing suspended micro-droplets by using negative pressure, which comprises the following steps:
the water phase moves upwards in an external circular ring shape under the action of negative pressure and forms accelerated motion through a conical channel; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the conical channel after passing through the hollow column, and the oily substance forms suspended micro-droplets under the action of the surface tension and the viscous force of the two-phase solution.
The method for preparing the suspended micro-droplets by using the negative pressure overcomes the defect of deformation caused by gravity when the suspended micro-droplets are prepared in the horizontal direction by moving from bottom to top by using the negative pressure, and the sphericity and the size of the droplets are difficult to control uniformly by pushing backwards by using the driving pump in the horizontal direction.
The magnitude of the negative pressure is preferably 2 to 20 times the weight of the oily substance, and may be, for example, 2 times, 3 times, 4 times, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, 12 times, 14 times, 15 times, 18 times, or 20 times, but is not limited to the above-mentioned values, and other values not listed in this range are also applicable, and preferably 2 to 10 times.
According to the invention, the weight of the oily substance under the negative pressure is preferably 2-10 times that of the oily substance, so that the formation of small liquid drops under high sphericity can be better realized.
Preferably, the included angle of the tapered channel is 30-45 °, such as 30 °, 32 °, 34 °, 35 °, 37 °, 39 °, 40 °, 42 °, 44 °, or 45 °, but not limited to the listed values, and other values not listed in the range are also applicable.
The invention adopts the conical channel, so that the annular channel is gradually reduced when the water phase moves upwards in an outer annular shape, and the flow speed of the water phase is increased to form accelerated motion, thereby forming shearing force on the inner phase oily substance and obtaining micro-droplets with smaller size; the formation of micro-droplets is preferably facilitated by controlling the included angle of the tapered channel to a specific range.
Preferably, the flow ratio of the oily substance to the aqueous phase is 1:10 to 1:70, and may be, for example, 1:10, 1:15, 1:20, 1:25, 1:30, 1:40, 1:50, 1:55, 1:60, or 1:70, but is not limited to the recited values, and other values not recited in this range are also applicable.
Preferably, the droplet diameter of the suspended micro-droplets is 0.5 to 2mm, and may be, for example, 0.5mm, 0.7mm, 0.9mm, 1mm, 1.2mm, 1.4mm, 1.5mm, 1.7mm, 1.9mm, or 2mm, but is not limited to the values listed, and other values not listed in this range are also applicable.
According to the invention, the microfluid is prepared by conveying the liquid drops from bottom to top under the negative pressure condition, so that micro-liquid drops with the diameter as low as 0.5mm can be prepared, the size is uniform and small, and the application prospect is wider.
Preferably, the aqueous phase comprises water.
When the oily substances comprise the oil phase thickening agent and the oil phase solvent, substances such as a surfactant and the like are not required to be added into the water phase, and the oily substances can be directly used as external phase substances to finally form stable micro-droplets, so that the collection is more convenient, and the cost is lower.
Preferably, the aqueous phase contains additives.
Preferably, the additive comprises a surfactant.
The surfactant used in the present invention is not particularly limited, and any surfactant suitable for the case, which is well known to those skilled in the art, may be used, and may be, for example, an anionic surfactant, a cationic surfactant, or a nonionic surfactant, and may be adjusted according to the actual circumstances.
When the oily substance is any one or the combination of at least two of silk oil, cashmere ester, lavender essential oil or vitamin E, a surfactant needs to be added into the water phase, so that the stability of the particles is improved.
Preferably, the oily substance comprises any one or a combination of at least two of silk oil, cashmere ester, lavender essential oil or vitamin E, wherein typical but non-limiting combinations are the combination of silk oil and cashmere ester, the combination of lavender essential oil and cashmere ester, the combination of silk oil and lavender essential oil, and the combination of vitamin E and cashmere ester.
Preferably, the oily substance comprises an oil phase thickener and an oil phase solvent.
Preferably, the oil phase thickener comprises any one or a combination of at least two of behenyl alcohol, dextrin palmitate, dextrin myristate, castor oil/IPDI copolymer, HDI/trimethylol hexyl lactone crosspolymer, glycerol behenate or eicosadioate, with typical but non-limiting combinations being behenyl alcohol and dextrin palmitate, dextrin myristate and dextrin palmitate, behenyl alcohol and HDI/trimethylol hexyl lactone crosspolymer, HDI/trimethylol hexyl lactone crosspolymer and dextrin palmitate, glycerol behenate and eicosadioate.
Preferably, the oil phase solvent comprises any one of or a combination of at least two of hydrogenated polyisobutene, hydrogenated polyparactene, isononyl isononanoate, glycerol tri (ethyl hexanoate), caprylic/capric triglyceride, caprylic/capric/succinic triglyceride, sunflower seed oil or meadowfoam seed oil, wherein typical but non-limiting combinations are a combination of hydrogenated polyisobutene and hydrogenated polyparactene, a combination of isononyl isononanoate and hydrogenated polyparactene, a combination of hydrogenated polyisobutene and caprylic/capric triglyceride, a combination of sunflower seed oil and hydrogenated polyparactene.
Preferably, when the oily substance comprises an oil phase thickener and an oil phase solvent, the temperature of the water phase is lower than the freezing point of the oily substance.
Preferably, the oily substance is at a temperature such that it is in a fluid state.
When the oily substance contains the oil phase thickener and the oil phase solvent, the oily substance needs to be heated and then enters the suspension micro-droplet preparation device to be in a fluid state.
Preferably, when the oily substance comprises an oily phase thickener and an oily phase solvent, the temperature of the aqueous phase is 5 to 30 ℃ lower than the freezing point of the oily substance, and may be, for example, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃ or 30 ℃, but not limited to the recited values, and other values not recited in the range are also applicable. Further preferably, the above range is advantageous in that instantaneous solidification of the oily substance in the case of containing the oil phase thickener and the oil phase solvent is achieved by utilizing the temperature difference, and solid round particles having a high sphericity are obtained.
Preferably, the formed suspended micro-droplets are conveyed in the vertical channel from bottom to top under the action of negative pressure to form solid round particles.
Preferably, the suspended micro-droplets in the vertical channels continue to be cooled by the aqueous phase.
As a preferred technical solution of the present invention, the method comprises:
oily substances in a fluid state are introduced from the bottom of the suspended micro-droplet preparation device as an internal phase, and an aqueous phase is introduced from the side as an external phase. The flow ratio of the oily substance to the water phase is 1: 10-1: 70; the temperature of the aqueous phase is lower than the temperature of the oily substance;
the water phase moves upwards in an outer ring shape under the action of negative pressure and forms accelerated motion through a conical channel with an included angle of 30-45 degrees; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the tapered channel after passing through the hollow column, and the oily substance forms suspended micro-droplets with the diameter of 0.5-2 mm under the action of the surface tension and the viscous force of the two-phase solution;
the formed suspended micro-droplets are conveyed from bottom to top in the vertical channel under the action of negative pressure, and are continuously cooled by a water phase to form solid round particles;
the negative pressure is 2-20 times of the gravity of the oily substance.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the method for preparing the suspended micro-droplets by using the negative pressure overcomes the problem that two particles are easy to collide and fuse in the prior art, the particles are uniform, the particle size range is 0.5-2.0 mm, the particles can be controlled to be 0.5-1.0 mm under the optimal condition, the problem that the oil phase is pushed by a peristaltic pump to cause fluctuation in the joining process and the particles are easy to have different sizes is solved, and compared with a precision rotor pump with high cost, one negative pressure device can drive a plurality of forming channels, so that the cost is obviously reduced;
(2) the method for preparing the suspended micro-droplets by using the negative pressure avoids the situation that particles form ellipses when oily substances are cooled due to the influence of gravity, and the average maximum diameter difference of the obtained suspended micro-droplets is less than or equal to 0.02mm, and can be less than or equal to 0.002mm under the optimal condition;
(3) according to the method for preparing the suspended micro-droplets by using the negative pressure, when the oil phase thickener and the oil phase solvent are adopted, the water phase can be directly adopted as the external phase, other substances are not required to be added, and the purification and collection are simple.
Drawings
Fig. 1 is a schematic flow chart of an apparatus for preparing suspended micro-droplets by using negative pressure according to embodiment 1 of the present invention.
FIG. 2 is a schematic representation of suspended micro-droplets produced in example 1 of the present invention.
Figure 3 is a schematic of the suspended micro-droplets prepared in comparative example 1.
In the figure: 1-a hollow column; 2-tapered channel.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be taken as limiting the present invention.
It should be understood by those skilled in the art that the present invention necessarily includes necessary piping and conventional valves for achieving the complete process, but the above contents do not belong to the main inventive points of the present invention, and those skilled in the art can select the layout of the additional devices based on the process flow and the structure of the equipment, and the present invention is not particularly limited to this.
Example 1
The present embodiment provides a method for preparing suspended micro-droplets by using negative pressure, as shown in fig. 1, the method comprising:
oily substances in a fluid state (HDI/trimethylol hexyl lactone crosslinked polymer and hydrogenated polyisobutene) are introduced from the bottom of the suspended micro-droplet preparation apparatus as an internal phase, and an aqueous phase is introduced from the side as an external phase; the flow ratio of the oily substance to the water phase is 1: 60; the temperature of the aqueous phase was 10 ℃;
the water phase moves upwards in an external circular ring shape under the action of negative pressure and forms accelerated motion through a conical channel 2 with an included angle of 35 degrees; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water converged from the conical channel 2 after passing through the hollow column 1, and the oily substance forms suspended micro-droplets with the diameter of 0.5-0.8 mm under the action of the surface tension and the viscous force of the two-phase solution;
the formed suspended micro-droplets are conveyed from bottom to top in the vertical channel under the action of negative pressure, and are continuously cooled by a water phase to form solid round particles;
the negative pressure is 15 times of the weight of the oily substances.
The suspended micro-droplets prepared in this embodiment are shown in fig. 2, and it can be seen from fig. 2 that the suspended micro-droplets prepared in this embodiment are all spherical and have particle sizes uniformly distributed between 0.5mm and 0.8 mm.
Example 2
The present embodiment provides a method for preparing suspended micro-droplets by using negative pressure, the method comprising:
the lavender essential oil in a fluid state is taken as an internal phase and introduced from the bottom of the suspension micro-droplet preparation device, and the water phase is taken as an external phase and introduced from the side; the flow ratio of the oily substance to the water phase is 1: 10;
the water phase (0.8 wt% of sodium dodecyl sulfate is added in the water phase) moves upwards in an external circular ring shape under the action of negative pressure, and forms accelerated motion through a conical channel with an included angle of 45 degrees; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the tapered channel after passing through the hollow column, and the oily substance forms suspended micro-droplets with the diameter of 0.6-0.8 mm under the action of the surface tension and the viscous force of the two-phase solution;
the formed suspended micro-droplets are conveyed from bottom to top in the vertical channel under the action of negative pressure, and are continuously cooled by a water phase to form solid round particles;
the negative pressure is 20 times of the weight of the oily substances.
Example 3
The present embodiment provides a method for preparing suspended micro-droplets by using negative pressure, the method comprising:
oily substances (white chinaroot oil and dextrin myristate) in fluid state are introduced from the bottom of the suspension droplet preparation device as internal phase, and water phase is introduced from side as external phase; the flow ratio of the oily substance to the water phase is 1: 70; the temperature of the aqueous phase is 5 ℃;
the water phase moves upwards in an external circular ring shape under the action of negative pressure and forms accelerated motion through a conical channel with an included angle of 30 degrees; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the tapered channel after passing through the hollow column, and the oily substance forms suspended micro-droplets with the diameter of 1.0-1.5 mm under the action of the surface tension and the viscous force of the two-phase solution;
the formed suspended micro-droplets are conveyed from bottom to top in the vertical channel under the action of negative pressure, and are continuously cooled by a water phase to form solid round particles;
the negative pressure is 2 times of the weight of the oily substance.
Example 4
The present embodiment provides a method for preparing suspended micro-droplets by using negative pressure, the method comprising:
oily substances (isononyl isononanoate and glyceryl behenate) in a fluid state are introduced from the bottom of the suspension micro-droplet preparation device as an internal phase, and a water phase is introduced from the side as an external phase; the flow ratio of the oily substance to the water phase is 1: 30; the temperature of the water phase is 25 ℃ at normal temperature;
the water phase moves upwards in an external circular ring shape under the action of negative pressure and forms accelerated motion through a conical channel with an included angle of 45 degrees; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the tapered channel after passing through the hollow column, and the oily substance forms suspended micro-droplets with the diameter of 0.5-0.9 mm under the action of the surface tension and the viscous force of the two-phase solution;
the formed suspended micro-droplets are conveyed from bottom to top in the vertical channel under the action of negative pressure, and are continuously cooled by a water phase to form solid round particles;
the negative pressure is 10 times of the weight of the oily substance.
Example 5
This example provides a method for preparing suspended micro-droplets using negative pressure, which is the same as example 1 except that the magnitude of the negative pressure is 1 time of the weight of the oily substance.
Example 6
This example provides a method for preparing suspended micro-droplets using negative pressure, which is the same as example 1 except that the magnitude of the negative pressure is 25 times the magnitude of the gravity of the oily substance.
Example 7
This example provides a method for preparing suspended micro-droplets using negative pressure, which is the same as example 1 except that accelerated motion is formed through a tapered channel with an included angle of 25 °.
Example 8
This example provides a method for preparing suspended micro-droplets using negative pressure, which is the same as example 1 except that accelerated motion is formed through a tapered channel with an included angle of 60 °.
Comparative example 1
This comparative example provides a method of preparing suspended micro-droplets using the method provided in example 1 of CN 109569344B.
The suspended micro-droplets produced by this comparative example are shown in fig. 3, and as can be seen by comparing fig. 3 with fig. 2, the circularity of the droplets in fig. 3 is significantly lower than that in fig. 2, and the particles having an elliptical shape in fig. 3 are more abundant.
Comparative example 2
This comparative example provides a method for preparing suspended micro-droplets, which is the same as example 1 except that the negative pressure in example 1 was replaced with a syringe pump (peristaltic pump) for injecting oily substances (HDI/trimethylol hexyl lactone crosslinked polymer and hydrogenated polyisobutene) in a fluid state, and a syringe pump (peristaltic pump) for injecting an aqueous phase.
The suspended micro-droplets prepared in the above examples and comparative examples were left to stand for two weeks, respectively, and the results are shown in table 1.
The particle size of the prepared suspended micro-droplets was counted, and the average maximum diameter difference of the suspended micro-droplets (i.e., the average of the maximum difference of the diameters of a plurality of the obtained droplet balls) was calculated by taking 10 different points, and the sphericity was the highest when the number of the points was 0, as shown in table 1.
TABLE 1
From table 1, the following points can be seen:
(1) it can be seen from the comprehensive examples 1 to 8 that the micro-droplets prepared by the method for preparing suspended micro-droplets by using negative pressure provided by the invention have more uniform particle size, the average maximum diameter difference is within 0.02mm, the particle size range can be controlled between 0.5 and 2.0mm, the particle size range can be controlled between 0.5 and 1.0mm in the preferred range, the particle size span is low, the particle size distribution is uniform, and the floating phenomenon does not occur after standing for two weeks;
(2) it can be seen from the combination of example 1 and comparative example 2 that the negative pressure mode is adopted in example 1 to achieve the transportation from bottom to top, compared with the injection pump mode adopted in comparative example 2, the particle size range in example 1 is 0.5-0.8 mm, the average maximum diameter difference is only 0.001mm, and the particle size range in comparative example 2 is 0.7-3.0 mm, and the average maximum diameter difference is as high as 0.04mm, thereby showing that the method for preparing suspended micro-droplets by using negative pressure provided by the invention significantly improves the circularity and uniformity of particle size through the negative pressure transportation from bottom to top.
In conclusion, the micro-droplets prepared by the method for preparing the suspended micro-droplets by utilizing negative pressure provided by the invention have uniform particle size, smaller size and higher circularity, and have wide application prospect.
The applicant states that the present invention is illustrated by the detailed steps of the above embodiments, but the present invention is not limited to the detailed steps, i.e. it is not meant that the present invention must rely on the detailed steps to be implemented. It will be apparent to those skilled in the art that any modifications to the invention, equivalents of selected steps and materials, additions of additional steps, selection of particular means, etc., are within the scope and disclosure of the invention.
Claims (10)
1. A method for producing suspended micro-droplets using negative pressure, the method comprising:
the water phase moves upwards in an external circular ring shape under the action of negative pressure and forms accelerated motion through a conical channel; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the conical channel after passing through the hollow column, and the oily substance forms suspended micro-droplets under the action of the surface tension and the viscous force of the two-phase solution.
2. The method according to claim 1, wherein the negative pressure is 2 to 20 times, preferably 2 to 10 times, the weight of the oily substance.
3. A method according to claim 1 or 2, wherein the included angle of the tapered channel is 30-45 °.
4. A process according to any one of claims 1 to 3, wherein the flow ratio of the oily substance to the aqueous phase is from 1:10 to 1: 70.
5. The method according to any one of claims 1 to 4, wherein the suspended micro-droplets have a droplet diameter of 0.5 to 2 mm.
6. The method according to any one of claims 1 to 5, wherein the aqueous phase comprises water;
preferably, the aqueous phase contains additives;
preferably, the additive comprises a surfactant.
7. The method according to any one of claims 1 to 6, wherein the oily substance comprises any one of silk oil, cashmere ester, lavender essential oil or vitamin E or a combination of at least two of the above;
preferably, the oily substance comprises an oil phase thickener and an oil phase solvent;
preferably, the oil phase thickener comprises any one or a combination of at least two of behenyl alcohol, dextrin palmitate, dextrin myristate, castor oil/IPDI copolymer, HDI/trimethylol hexyl lactone crosspolymer, glyceryl behenate or eicosanedioate;
preferably, the oil phase solvent comprises any one of hydrogenated polyisobutene, hydrogenated polyparacene, isononyl isononanoate, triglyceride (ethyl hexanoate), caprylic/capric triglyceride, caprylic/capric/succinic triglyceride, sunflower seed oil or meadowfoam seed oil or a combination of at least two thereof.
8. The method according to any one of claims 1 to 7, wherein when the oily substance comprises an oil phase thickener and an oil phase solvent, the temperature of the water phase is lower than the freezing point of the oily substance;
preferably, the oily substance is at a temperature such that it is in a fluid state.
9. The method according to any one of claims 1 to 8, wherein the formed suspended micro-droplets are conveyed in the vertical channel from bottom to top under the action of negative pressure to form solid round particles.
10. The method according to any one of claims 1 to 9, characterized in that it comprises:
oily substances in a fluid state are taken as an internal phase and introduced from the bottom of the suspension micro-droplet preparation device, and a water phase is taken as an external phase and introduced from the side; the flow ratio of the oily substance to the water phase is 1: 10-1: 70;
the water phase moves upwards in an outer ring shape under the action of negative pressure and forms accelerated motion through a conical channel with an included angle of 30-45 degrees; the oily substance moves from bottom to top in the internal channel under the action of negative pressure, and contacts with the water gathered from the tapered channel after passing through the hollow column, and the oily substance forms suspended micro-droplets with the diameter of 0.5-2 mm under the action of the surface tension and the viscous force of the two-phase solution;
the formed suspended micro-droplets are conveyed from bottom to top in the vertical channel under the action of negative pressure, and are continuously cooled by a water phase to form solid round particles;
the negative pressure is 2-20 times of the gravity of the oily substance.
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