CN114307881B - Microcapsule preparation method and microcapsule preparation device - Google Patents
Microcapsule preparation method and microcapsule preparation device Download PDFInfo
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- CN114307881B CN114307881B CN202111435590.7A CN202111435590A CN114307881B CN 114307881 B CN114307881 B CN 114307881B CN 202111435590 A CN202111435590 A CN 202111435590A CN 114307881 B CN114307881 B CN 114307881B
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Abstract
The invention belongs to the technical field of microcapsule preparation, and discloses a microcapsule preparation method and a microcapsule preparation device. The method is characterized in that a hydrophilic solution atomizing nozzle and a lipophilic solution atomizing nozzle of a high-voltage electrostatic spraying system are respectively connected with a high-voltage electrostatic generator, a certain amount of capsule material liquid drops are combined to the outer wall of the core material liquid drops through electrostatic adsorption, when the charges of the capsule material liquid drops adsorbed by the core material liquid drops are equal to the charges of the capsule material liquid drops, uncharged fused liquid drops are formed, and the fused liquid drops are finally separated from the action of an electric field force to form microcapsule particles; in the process of mutual adsorption of the core material liquid drops and the capsule material liquid drops, the particle diameters of the liquid drops are adjusted by controlling the pressure of the nozzle, the charge-to-mass ratio of the core material liquid drops and the capsule material liquid drops is adjusted by controlling the electrostatic high voltage of the high-voltage electrostatic generator, and the particle diameters of the liquid drops, the charge-to-mass ratio of the core material liquid drops and the capsule material liquid drops are set by the method, so that the quantitative control of the particle diameters and the thicknesses of the microcapsules is achieved.
Description
Technical Field
The invention relates to the technical field of microcapsule preparation, in particular to a microcapsule preparation method and a microcapsule preparation device.
Background
Microencapsulation refers to a technique in which a solid, liquid or gas is entrapped in a tiny, sealed capsule, which releases at a controlled rate only under specific conditions. The microcapsule has the functions of covering peculiar smell and color, changing substance form, protecting sensitive components, reducing toxicity, prolonging the storage time of volatile substances, delaying or controlling the release of a capsule core material, mixing immiscible components, isolating immiscible compounds and the like, and is widely applied to the fields of food, medicine, cosmetics, pesticides and the like at present.
The microcapsule preparation method can be roughly divided into three main categories, namely a physical method, a chemical method and a physicochemical method. Specifically, there are spray drying method, spray congealing method, air suspension method, fluidized bed coating method, single agglomeration method, congruence agglomeration method, extrusion method, orifice method, powder bed method, interfacial polymerization method, in situ polymerization method, molecular embedding method, and the like. However, most of the methods have the defects of complex operation steps, high process requirements, unstable finished product quality, incapability of quantitatively controlling the particle size and shell thickness of the microcapsule and the like.
The high-voltage electrostatic spraying microcapsule preparation method is characterized by utilizing a high-voltage electrostatic generator to charge sprayed liquid drops for preparing microcapsules. The general process comprises the following steps: the positive pole of the high voltage generator is connected with the syringe needle, the negative pole is arranged at the bottom of the container filled with the curing liquid, and the syringe needle is suspended at a certain distance above the liquid level of the curing liquid. When the preparation method is used, a power supply is switched on, a high-voltage electric field is generated between the two electrodes, and when the injection pump pushes out the core material solution at a constant speed, the electric field force overcomes the inherent viscous force and surface tension of the core material solution, so that the core material solution is sprayed into the curing liquid in a fog drop form with a certain particle size, and the water-insoluble microcapsule is rapidly cured to form. Many researches show that the microcapsules prepared by the high-voltage electrostatic spraying method have the advantages of good encapsulation performance, uniform size and the like, but the preparation method of the electrostatic spraying capsules still has no method for quantitatively controlling the particle size and the shell thickness of the microcapsules; and the electrostatic spraying microcapsule preparation technology is still basically in the laboratory research stage, generally uses a self-made simple experimental device, and cannot be used for the batch production of the microcapsules.
Patent document CN208049904U discloses a simple high-voltage electrostatic microcapsule generating device, which mainly comprises two spray heads connected with the positive and negative electrodes of a high-voltage electrostatic generator and a sealed reaction container, and can respectively generate core material fog droplets and capsule material fog droplets, and the core material fog droplets and the capsule material fog droplets are combined under the action of high-voltage static electricity to generate microcapsules; however, the device has a simple structure, the injector is used for supplying liquid to the spray head, and the design is not carried out on the continuity required by the batch preparation of the microcapsules and the quality parameter control such as the particle size, the wall thickness and the like of the microcapsules.
In addition, in the current high-voltage electrostatic spray microcapsule preparation technology, a solution jet is mainly charged in a contact charging mode, so that the risks of electric leakage and electric shock exist on one hand, and on the other hand, the solution jet can only be used for spraying hydrophilic conductive solution and cannot be used for spraying lipophilic insulating solution. Most of the lipophilic materials are insulating or low-conductivity materials, and are difficult to be charged by a general contact conduction or induction type charging mode, and conventional corona type charging modes can generate heat effect, ozone, nitrogen oxide and the like, so that the bioactive substances in the capsules can be possibly adversely affected, and the lipophilic materials are not suitable for food or medicine application.
Disclosure of Invention
The invention provides a microcapsule preparation method, aiming at solving the technical problems that the quality parameters such as the particle diameter and the wall thickness of a microcapsule can not be quantitatively controlled and the charging mode for preparing the microcapsule by lipophilic materials is insufficient in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a microcapsule preparation method is characterized in that an arranged high-voltage electrostatic spraying system is utilized, a hydrophilic solution atomizing spray head and a lipophilic solution atomizing spray head of the high-voltage electrostatic spraying system are respectively connected with a high-voltage electrostatic generator, the hydrophilic solution atomizing spray head sprays hydrophilic droplets with positive charges, the lipophilic solution atomizing spray head sprays lipophilic droplets with negative charges, electrostatic fields are established in spray chambers below the hydrophilic solution atomizing spray head and the lipophilic solution atomizing spray head, charged droplets with opposite charges generated by the two spray heads move relatively under the action of an electric field force, the hydrophilic droplets with positive charges and the lipophilic droplets with negative charges are respectively used as core material droplets and capsule material droplets, a certain number of capsule material droplets are combined onto the outer walls of the core material droplets through electrostatic adsorption, when the charges of the capsule material droplets adsorbed by the core material droplets are equal to the charges of the capsule material droplets, uncharged fused droplets are formed, and the fused droplets finally break away from the action of the electric field force to form microcapsule particles; in the process of mutual adsorption of the core material liquid drops and the capsule material liquid drops, the particle sizes of the core material liquid drops and the capsule material liquid drops are respectively adjusted by controlling the pressure of a nozzle, the charge-to-mass ratios of the core material liquid drops and the capsule material liquid drops are respectively adjusted by controlling the electrostatic high voltage of a high-voltage electrostatic generator, and the particle sizes of the core material liquid drops and the capsule material liquid drops, and the charge-to-mass ratios of the core material liquid drops and the capsule material liquid drops are set by the method, so that the quantitative control of the particle sizes and the thicknesses of the microcapsules is realized.
Further, hydrophilic solution atomizer adopt the induction charging mode, be provided with annular induction type electrode around the outer wall of shower nozzle spout department, annular induction type electrode is connected with high-voltage electrostatic generator's output, annular induction type electrode with hydrophilic solution atomizer's inside solution uses insulating material one to keep apart, and conductive solution ground connection in the shower nozzle, the electric field that forms between annular induction type electrode and the conductive jet makes hydrophilic solution droplet charge, and the electric charge polarity that the droplet takes is opposite with the induction electrode, finally forms the hydrophilic droplet of taking the positive charge after spouting through the nozzle. In the prior high-voltage electrostatic spraying microcapsule preparation technology, a contact charging mode is mainly adopted to charge solution jet, on one hand, the risks of electric leakage and electric shock exist, on the other hand, the electrostatic spraying microcapsule adopts an electrostatic induction mode to charge, an electrode is not in direct contact with the solution jet, and the electrostatic spraying microcapsule is used for high-voltage electrostatic spraying of a hydrophilic solution conductive material, thereby avoiding the risks of electric leakage and electric shock and improving the operation safety.
Furthermore, lipophilic solution atomizer adopts the contact charging mode, and the shower nozzle center sets up an acute angle electrode of being connected with the output of high-voltage electrostatic generator, sets up a grounded obtuse angle electrode around it, the obtuse angle electrode is installed on the insulating material two of shower nozzle inner wall, and the liquid stream is insulating solution between acute angle electrode and the obtuse angle electrode, and the electron on the acute angle electrode can pour into the liquid stream under the effect of electric field into, and the electron can not freely move in insulating solution, forms the lipophilic fog droplet of taking the negative charge after finally spouting through the nozzle. The invention adopts an improved contact charging mode to charge, utilizes a high-voltage electrostatic field to drive the jet flow of electrons injected into the insulating solution, leads the atomized liquid drops to carry negative charges and realizes the high-voltage electrostatic spraying of the insulating material of the lipophilic solution.
Further, the charged liquid drops or large-particle microcapsules which are not combined or not sufficiently combined are screened and collected by an electric field:
screening and collecting the unbound or insufficiently bound charged liquid drops or large particle microcapsules by an electric field: the liquid drops which are not combined or not fully combined still have electric charges, continue to move towards the opposite electrode plate under the action of the electric field force, are finally collected by the electrode plate, form large liquid drops to fall under the action of gravity after the liquid drops are gathered to a certain amount, and finally flow into a waste collecting tank arranged below along the wall of the container, or large-particle fused liquid drop microcapsules without electric charges flow into the waste collecting tank arranged below under the action of gravity; in the process, the electric field voltage in the spraying chamber can be adjusted to change the electric field intensity so as to adjust the screening intensity of the non-bonded liquid drop or large particle non-charged fused liquid drop microcapsule.
Furthermore, a T-shaped sorting pipeline and a particle collector are arranged below the high-voltage electrostatic spraying system to select the microcapsules with qualified particle size: the pipeline combination department sets up "T" style of calligraphy and selects separately the pipeline, and when the air current that carries dry microcapsule granule got into the collection pipeline from dry pipeline, less granule got into the granule collector along with the air current through the collection pipeline, was equipped with the filter screen at two inside walls of granule collector, and the qualified microcapsule granule that the particle diameter is greater than filter screen mesh diameter is collected, and the granule that the particle diameter is less than filter screen mesh diameter is taken away by the air current.
Further, the hydrophilic droplets are selected from chitosan, starch, maltodextrin, cyclodextrin, cellulose, lignin, pectin, agar, alginate, guar gum, gum arabic, xanthan gum, gellan gum, konjac gum, and beta-glucan polysaccharides; or gelatin, soy protein, whey protein, casein, collagen protein; or water solution composed of vitamin B, vitamin C, surfactant, and emulsifier.
Further, the lipophilic fog drops are selected from soybean oil, olive oil, paraffin, beeswax, paraffin oil and stearic acid; or lipophilic solution composed of vitamin A, vitamin D, coenzyme Q10, surfactant, and emulsifier.
The invention also aims to provide a microcapsule preparation device capable of realizing the microcapsule preparation method, which comprises a high-voltage electrostatic spraying system; wherein, high voltage electrostatic spraying system includes hydrophilic solution atomizer, lipophilic solution atomizer, high voltage electrostatic generator and spray chamber, hydrophilic solution atomizer and lipophilic solution atomizer are installed respectively on the spray chamber, hydrophilic solution atomizer and lipophilic solution atomizer respectively with high voltage electrostatic generator's different output is connected, electrically conductive solution ground connection in the hydrophilic solution atomizer, the spray chamber is equipped with two flat electrodes, and flat electrode connects high voltage electrostatic generator's output, and another flat electrode ground connection establishes the electrostatic field between two electrodes.
Further, hydrophilic solution atomizer is used for hydrophilic conducting solution's electrostatic spraying, hydrophilic solution atomizer adopts the induction charging mode, is provided with annular induction type electrode around the outer wall of shower nozzle department, annular induction type electrode is connected with high-voltage electrostatic generator's output, hydrophilic solution atomizer inner wall is equipped with insulating material one, annular induction type electrode with hydrophilic solution atomizer's inside solution uses insulating material one keeps apart, conducting solution ground connection in the shower nozzle.
Further, lipophilic solution atomizer is used for lipophilic conductive solution's electrostatic spraying, lipophilic solution atomizer's shower nozzle center is equipped with an acute angle electrode, the acute angle electrode is connected with high-voltage electrostatic generator's output, lipophilic solution atomizer inner wall is provided with insulating material two, two departments of insulating material around the acute angle electrode are inlayed and are had an obtuse angle electrode, obtuse angle electrode ground connection, the acute angle electrode with the liquid stream is insulating solution between the obtuse angle electrode.
Furthermore, the microcapsule preparation device provided by the invention further comprises a liquid supply system, wherein the liquid supply system comprises a hydrophilic solution storage tank and a lipophilic solution storage tank, the hydrophilic solution storage tank is communicated with the hydrophilic solution atomizing spray head through a first infusion pump to provide hydrophilic solution for the hydrophilic solution atomizing spray head, and the lipophilic solution storage tank is communicated with the lipophilic solution atomizing spray head through a second infusion pump to provide lipophilic solution for the lipophilic solution atomizing spray head.
Further, the microcapsule preparation device provided by the invention further comprises a gas control system connected with the high-voltage electrostatic spraying system, wherein the gas control system comprises a gas cylinder and a vacuum pump, the gas cylinder is connected with the high-voltage electrostatic spraying system, a gas flow control valve and a flow rate meter are arranged on a connecting pipeline between the gas cylinder and the high-voltage electrostatic spraying system, and the vacuum pump pumps the gas in the whole device to vacuum and adjusts the gas pressure.
Further, the microcapsule preparation device provided by the invention further comprises a drying system, wherein the drying system comprises a drying pipeline and a heater arranged outside the drying pipeline, and the heater can be preferably an infrared heater; furthermore, a temperature sensor, an air pressure sensor and a humidity sensor are connected to the drying pipeline.
Furthermore, the microcapsule preparation device provided by the invention also comprises a microcapsule grading and collecting system, wherein the microcapsule grading and collecting system comprises a T-shaped sorting pipeline, a waste collecting tank and a particle collector, a vertical pipe of the T-shaped sorting pipeline is communicated with the waste collecting tank, a horizontal pipe of the T-shaped sorting pipeline is communicated with the particle collector, filter screens are arranged on two inner side walls of the particle collector, and the microcapsule collecting tank is arranged below the particle collector.
Further, the filter screen is connected with a vibration motor through a connecting rod; and the waste collecting tank and the microcapsule collecting tank are respectively provided with a connecting piece with a sealing valve.
Compared with the prior art, the method can realize quantitative control on parameters such as the diameter, the wall thickness and the like of the generated microcapsule by adjusting the particle diameter and the charge-to-mass ratio of electrostatic spray droplets, mainly can adjust the particle diameter of the droplets by controlling the pressure of a spray head, adjust the charge-to-mass ratio of the droplets by controlling the electrostatic high voltage, and set the particle diameter of the droplets and the charge-to-mass ratio of the droplets of the core material and the capsule material by the method, thereby achieving quantitative control on the particle diameter and the thickness of the microcapsule.
In addition, two different high-voltage electrostatic spray heads are designed, one of the high-voltage electrostatic spray heads is charged in an electrostatic induction mode, an electrode is not in direct contact with solution jet flow, and the high-voltage electrostatic spray heads are used for high-voltage electrostatic spraying of hydrophilic solution conductive materials, so that electric leakage and electric shock risks are avoided, and the operation safety is improved; and the other method adopts an improved contact charging mode for charging, and utilizes a high-voltage electrostatic field to drive the jet flow of electrons injected into the insulating solution, so that atomized liquid drops are negatively charged, and the high-voltage electrostatic spraying of the lipophilic solution insulating material is realized.
Secondly, in the process of preparing the microcapsule, due to factors such as uneven high-voltage electrostatic atomization, insufficient combination of two kinds of atomized charged liquid drops and the like, or unqualified particles can be generated, or the non-charged fused liquid drop microcapsule with large particles which do not meet the specification can be generated; and microcapsule particles meeting the specification standard are collected through a T-shaped sorting pipeline and a particle collector with a filter screen.
According to the technical scheme, the microcapsule preparation method and the microcapsule preparation device provided by the invention can realize the control of parameters such as the particle size, the wall thickness and the like of the microcapsule, can smoothly realize the high-voltage electrostatic spraying of hydrophilic and lipophilic solution insulating materials, finally prepare the microcapsule by taking the hydrophilic and lipophilic incompatible materials as the core material and the capsule material, and finally collect the microcapsule meeting the specification. The technical scheme can enable the preparation of the electrostatic spraying microcapsule to realize continuous production.
Drawings
FIG. 1 is a schematic diagram of a charged liquid drop combination process in a microcapsule particle preparation process provided by the present invention;
FIG. 2 is a schematic view of a hydrophilic solution atomizer provided in the present invention for electrostatic spraying of a hydrophilic conductive solution;
FIG. 3 is a schematic diagram of a lipophilic solution atomizer according to the present invention for electrostatic spraying of a lipophilic conductive solution;
FIG. 4 is a schematic diagram of a microcapsule screening process provided in the present invention;
FIG. 5 is a schematic structural view of a microcapsule preparation apparatus provided in the present invention;
description of the drawings: 1. a high voltage electrostatic generator; 2. a spray chamber; 3. a hydrophilic solution atomizing spray head; 4. a first flange 5 and a lipophilic solution atomizing nozzle; 6. a second flange; 7. an infrared heating pipe; 8. a drying pipeline; 9. a vibration motor; 10. a particle collector; 11. a filter screen; 12. a third flange; 13. a vacuum pump; 14. a microcapsule collection tank; 15. a second connecting piece; 16. a collection pipe; 17. a waste collector; 18. a first connecting piece; 19. a temperature sensor; 20. an air pressure sensor; 21. a humidity sensor; 22. a hydrophilic solution storage tank; 23. a first infusion pump; 24. a lipophilic solution storage tank; 25. a second infusion pump; 26. a gas cylinder; 27. a flow rate meter; 28. an airflow control valve; 30. a second flat electrode; 31. a first flat electrode; 32. a ring-shaped induction type electrode; 33. insulating material I; 34. an acute angle electrode; 35. an obtuse-angle electrode; 36. and a second insulating material.
Detailed Description
The invention discloses a microcapsule preparation method and a microcapsule preparation device, and can be realized by appropriately improving process parameters by taking the contents of the text as reference. It is specifically noted that all such substitutions and modifications will be apparent to those skilled in the art and are intended to be included within the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations and modifications, or appropriate variations and combinations of the methods and applications described herein may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The following detailed description of the invention refers to specific embodiments thereof for better understanding by those skilled in the art.
The technical problems that the quality parameters such as the particle size and the wall thickness of the microcapsule are not controllable, the spraying of the hydrophilic conductive solution adopts a contact charging mode to charge the solution jet flow, the electric leakage and electric shock risks exist, and the charging mode for preparing the microcapsule by using the lipophilic material is insufficient are solved. The high-voltage electrostatic generator 1 of the invention can provide 3 paths of negative electrode high-voltage output ends: -V 1 、-V 2 、-V 3 Each path of voltage is independently adjustable, and the current range is as follows: 1 μ A-1mA, voltage range: 1kV to 10kV. As shown in figures 1 and 5, the microcapsule preparation method provided by the invention utilizes the high-voltage electrostatic spraying system, and the hydrophilic solution atomizing nozzle 3 and the lipophilic solution atomizing nozzle 5 of the high-voltage electrostatic spraying system are respectively arranged with the-V of the high-voltage electrostatic generator thereof 1 Output port and-V 2 The output ports are connected, the high-voltage electrostatic generator is grounded simultaneously, the hydrophilic solution atomizing nozzle 3 sprays out to form hydrophilic fog drops with positive charges, the lipophilic solution atomizing nozzle 5 sprays out to form lipophilic fog drops with negative charges, electrostatic fields are established in the atomizing chambers below the hydrophilic solution atomizing nozzle 3 and the lipophilic solution atomizing nozzle 5, charged liquid drops with opposite charges generated by the two nozzles move relatively under the action of electric field force, the hydrophilic fog drops with positive charges and the lipophilic fog drops with negative charges are respectively used as core material liquid drops and capsule material liquid drops, a certain amount of capsule material liquid drops can be combined onto the outer wall of the core material liquid drops through electrostatic adsorption, and when the charges of the capsule material liquid drops adsorbed by the core material liquid drops are equal to the charges of the capsule material liquid drops, uncharged hydrophilic fog drops are formedThe fused liquid drops finally form microcapsule particles under the action of the electric field force; in the process of mutual adsorption of the core material liquid drops and the capsule material liquid drops, the particle diameters of the liquid drops are adjusted by controlling the pressure of the nozzle, the charge-to-mass ratios of the core material liquid drops and the capsule material liquid drops are adjusted by controlling the electrostatic high voltage of the high-voltage electrostatic generator, and the particle diameters of the liquid drops and the charge-to-mass ratios of the core material liquid drops and the capsule material liquid drops are set by the method, so that the quantitative control of the particle diameters and the thicknesses of the microcapsules is realized.
In this embodiment, the electrostatic field in the spraying chamber can be established by providing two plate electrodes in the spraying chamber, as shown in fig. 1, one of the plate electrodes is referred to as plate electrode one 31, which is connected to an output terminal-V of the high voltage electrostatic generator 1 3 The other plate may be referred to as the second plate electrode 30, which is grounded and establishes an electrostatic field.
Hydrophilic material solution can be used as core material raw material, and lipophilic material solution can be used as capsule material raw material; the lipophilic material solution can also be used as the raw material of the core material, and the hydrophilic material solution can be used as the raw material of the capsule material.
The method is illustrated by taking a lipophilic material solution as a core material and a hydrophilic material solution as a capsule material as an example:
the following parameters were set: the radius of the microcapsule to be prepared is R, the wall thickness of the microcapsule is d, and the density of the core material is rho 1 The density of the capsule wall material is rho 2 The content of the capsule wall material in the capsule wall material aqueous solution is C%.
Radius R of core material droplet 1 Radius R-wall thickness d of the microcapsules;
charge to mass ratio (q/m) of core droplet 1 May be set to (0.1 mC/kg-1 mC/kg), preferably (0.1 mC/kg-0.3 mC/kg);
radius of capsule material drop R 2 The radius of the core material liquid drop is preferably 1/2-1/10, more preferably 1/3-1/5, and the particle diameter of the capsule material is adjusted by controlling the pressure of the nozzle to meet the radius R of the capsule material liquid drop 2 The size of (a) satisfies the above requirements;
because each fused droplet is formed by combining one core material droplet and a plurality of capsule material droplets, and the core material droplets are carried by the core material dropletsElectric charge Q Core The capsule material liquid drop combined with the electric charge Q Capsule Opposite polarity, equal number of charges, i.e. Q Core ＝Q Capsule According to the charge-to-mass ratio calculation formula,
the following can be obtained: core droplet charge to mass ratio (q/m) 1 X mass of core droplet m 1 = capsule drop charge to mass ratio (q/m) 2 X mass of capsule wall drop M.
So that the charge-to-mass ratio (q/m) of the capsule material liquid drop 2 = core material droplet charge to mass (q/m) 1 X (core mass/outer wall layer mass) = core material drop charge-to-mass ratio (q/m) 1 X mass of microcapsule core material m 1 /(microcapsule wall Material Mass m) 2 C% of capsule material (= core material droplet charge-to-mass ratio (q/m) 1 X (core droplet volume x core density ρ) 1 ) /((microcapsule outer wall volume. Capsule material density. Rho.) 2 ) C% of capsule wall material); finally, a formula I is obtained, and the charge-to-mass ratio and the radius of the core material liquid drop are obtained through the formula I, so that the radius R and the wall thickness d of the generated microcapsule can be obtained.
In this example, the method for adjusting the particle size and the charge-to-mass ratio of the electrostatic spray droplets was as follows: under the condition of selecting the spray head and the working solution, the particle size and the charge-to-mass ratio of spray liquid drops can be adjusted by changing the pressure of the spray head and the electrostatic high voltage. Specifically, the particle size of the liquid drops is reduced along with the increase of the pressure of the spray head, the electrostatic high voltage is beneficial to the superfine atomization of the liquid drops, but the influence degree is smaller, so the particle size of the liquid drops is determined by the pressure of the spray head, the pressure of the spray head can be changed by adjusting a liquid transfer pump connected with the spray head and the like, and the radius R of the core material can be set in advance according to the actual production requirement through the pressure of the spray head 1 (ii) a The charge-to-mass ratio of the liquid drops is increased along with the increase of the electrostatic high voltage, but in the induction type charging mode, the electrostatic high voltage is increased to a certain value, a corona phenomenon occurs, the charge-to-mass ratio is reduced, and the electrostatic high voltage can be changed by adjusting the output of the high-voltage electrostatic generator; therefore, under the condition of certain pressure of the spray head, the height can be adjusted and adjusted through the actual conditionElectrostatic high voltage of piezoelectric generator sets charge-to-mass ratio (q/m) of core material and capsule material 1 And (q/m) 2 Finally, the radius R and the wall thickness d of the microcapsule are obtained according to the formula.
The hydrophilic solution atomizer 3 is used for electrostatic spraying of a hydrophilic electroconductive solution. As shown in figure 2, the hydrophilic solution atomizing nozzle 3 adopts an induction charging mode, an annular induction type electrode 32 is arranged around the outer wall of the nozzle opening of the nozzle, and the annular induction type electrode 32 and the-V of the high-voltage electrostatic generator 2 The output end is connected, the annular induction type electrode 32 and the internal solution of the hydrophilic solution atomizing nozzle 3 are isolated by using an insulating material I33, the conductive solution in the nozzle is grounded, an electric field formed between the annular induction type electrode 32 and the conductive jet flow enables hydrophilic solution droplets to be charged, the polarity of charges carried by the droplets is opposite to that of the induction electrode, and finally the hydrophilic droplets with positive charges are formed after the hydrophilic solution droplets are sprayed out through the spray nozzle, and the polarity of charges carried by the droplets is opposite to that of the induction electrode and is positively charged. Compared with the commonly used contact charging mode in the field at present, the electrode of the induction type charging mode is not in direct contact with the solution jet, the electric field between the electrode and the solution jet is utilized to charge the fog drops, the liquid is grounded, the liquid storage tank and the conveying pipeline are not required to be insulated, the required charging voltage is lower, the electric leakage and electric shock risks frequently existing in the commonly used contact charging mode are avoided, and the operation safety is improved.
In this embodiment, the hydrophilic droplets are selected from the group consisting of chitosan, starch, maltodextrin, cyclodextrin, cellulose, lignin, pectin, agar, alginate, guar gum, gum arabic, xanthan gum, gellan gum, konjac gum, and β -glucan polysaccharides; or gelatin, soy protein, whey protein, casein, collagen protein; or water solution composed of vitamin B, vitamin C, surfactant, and emulsifier.
The lipophilic solution atomizer head 5 is used for electrostatic spraying of lipophilic solutions, i.e. spraying of non- (low) conducting solutions. Common materials for preparing core materials of the microcapsules comprise edible oil and lipophilic vitamins (vitamin E, vitamin D and the like), common materials for capsule materials comprise stearic acid, beeswax and the like which are insulating or low-conductivity materials, common contact conduction or induction charging modes are difficult to charge, and corona charging modes commonly used in the electrostatic spraying industry probably have adverse effects on bioactive substances in the microcapsules due to the generation of heat effect, ozone, nitrogen oxide and the like.
The invention adopts a special contact charging mode, as shown in figure 3, the lipophilic solution atomizing nozzle 5 adopts a contact charging mode, and the center of the nozzle is provided with a-V connected with the high-voltage electrostatic generator 1 1 The sharp-angle electrode 34 is connected with the output end, the grounded blunt-angle electrode 35 is arranged around the sharp-angle electrode 34, the blunt-angle electrode 35 is installed on the second insulating material 36 on the inner wall of the spray head, liquid flow between the sharp-angle electrode 34 and the blunt-angle electrode 35 is insulating solution, electrons on the sharp-angle electrode 34 can be injected into the liquid flow under the action of an electric field, the electrons cannot move freely in the insulating solution, and finally lipophilic fog drops with negative charges are formed after being sprayed out through the spray nozzle. The charging mode of the electrostatic spray head for the lipophilic solution provided by the invention is improved contact charging, because the lipophilic solution is generally an electric insulating solution, the lipophilic solution is effectively charged by the charging mode provided by the invention, the improved contact charging mode is used for charging, the high-voltage electrostatic field is used for driving the jet flow of electrons injected into the insulating solution, so that atomized liquid drops are negatively charged, the lipophilic solution insulating material is effectively charged, ozone or superoxide radical is not generated, and active row components in the solution are not damaged.
In this example, the lipophilic droplet is selected from the group consisting of soybean oil, olive oil, paraffin, beeswax, paraffin oil, stearic acid; or lipophilic solution composed of vitamin A, vitamin D, coenzyme Q10, surfactant, and emulsifier.
As shown in fig. 1 and 4, the electric field provided by the present invention can realize the screening collection of large particle capsules of unbound or insufficiently bound charged droplets and neutral confluent droplets: two flat electrodes are arranged below the atomizing nozzles on two sides of the atomizing chamber 2, and a first flat electrode 31 is connected with the output end-V of the high-voltage electrostatic generator 1 3 The second plate electrode 30 is grounded, as shown in FIG. 4, and is constructed between the two electrodes during operationAnd (3) standing an electrostatic field to enable the charged liquid drops generated by the two nozzles to move relatively under the action of an electric field force, combining the liquid drops with the same amount of heterogeneous charges in a middle combining area, restoring the electric neutrality (no charge) of the combined liquid drops, separating the action of the electric field force, entering a heating drying area under the action of gravity and air flow, and dehydrating the outer capsule layer to form dried microcapsule particles. The liquid drops which are not or fully combined still have electric charges, continue to move towards the opposite electrode plate under the action of the electric field force, are finally collected by the electrode plates, form large liquid drops under the action of gravity after being gathered to a certain amount, and then flow into a waste material collecting tank below along the wall of the container; large particle capsules that are out of specification for neutral coalesced droplets will also enter the waste collection tank by gravity; in the process, the electric field voltage in the spraying chamber can be adjusted to change the electric field intensity so as to adjust the screening intensity of the non-bonded liquid drop or large particle non-charged fused liquid drop microcapsule.
As shown in fig. 4 and 5, a method for collecting microcapsules with the particle size meeting the specification by arranging a T-shaped sorting pipeline and a particle collector 10 is as follows: the T-shaped sorting pipeline is arranged at the joint of the pipelines, when the air flow carrying the dry microcapsule particles enters the collecting pipeline 16 from the drying pipeline 8, the smaller particles enter the particle collector 10 along with the air flow through the collecting pipeline, the filter screens 11 are arranged on the two inner side walls of the particle collector 10, the qualified microcapsule particles with the particle size larger than the mesh diameter of the filter screens in the smaller particles are collected, and the particles with the particle size smaller than the mesh diameter of the filter screens 11 are taken away by the air flow. The invention adjusts the air pressure and the air flow in the pipeline through the vacuum pump 12 to adjust the upper limit of the diameter range of the screened microcapsule particles, and the diameter of the meshes can be selected to control the lower limit of the diameter range of the collected microcapsule particles.
As shown in FIG. 5, the present invention shows the connection relationship and structural features of a microcapsule preparation apparatus, which comprises a high voltage electrostatic spraying system in this embodiment; wherein, high-voltage electrostatic spraying system includes hydrophilic solution atomizer 3, lipophilic solution atomizer 5, high-voltage electrostatic generator 1 and spray chamber 2, hydrophilic solution atomizer 3 and lipophilic solution atomizer 5 are installed respectively on spray chamber 2, hydrophilic solution atomizer 3 and lipophilic solution atomizer 5 respectively with high-voltage electrostatic generator 1's different output is connected, the conducting solution ground connection in the hydrophilic solution atomizer 3, be equipped with two flat plate electrodes in the spray chamber 2, a flat plate electrode is called flat plate electrode one 31, and its output of connecting high-voltage electrostatic generator 1, another ground connection flat plate is called flat plate electrode two 30, establishes the electrostatic field between two electrodes.
In the embodiment shown in fig. 2, the hydrophilic solution atomizer 3 is used for electrostatic spraying of hydrophilic conductive solution, the hydrophilic solution atomizer 3 adopts an induction charging mode, an annular induction electrode 32 is arranged around the outer wall of the nozzle of the hydrophilic solution atomizer, and the annular induction electrode 32 and the-V of the high voltage electrostatic generator 1 are connected in parallel 2 The output is connected, hydrophilic solution atomizer 3 inner wall is equipped with insulating material 33, annular induction type electrode 32 with hydrophilic solution atomizer 3's inside solution uses insulating material 33 keeps apart, and electrically conductive solution ground connection in the shower nozzle. By adopting the electrostatic induction charging mode, the electrode is not in direct contact with the solution jet flow, and the electrostatic spraying device is used for high-voltage electrostatic spraying of hydrophilic solution conductive materials, thereby avoiding electric leakage and electric shock risks and improving the operation safety.
In the embodiment shown in fig. 3, the lipophilic solution atomizing nozzle 5 is used for electrostatic spraying of lipophilic conductive solution, the nozzle center of the lipophilic solution atomizing nozzle 5 is provided with an acute angle electrode 34, and the acute angle electrode 34 is connected with-V of the high voltage electrostatic generator 1 1 The output is connected, 5 inner walls of lipophilic solution atomizer are provided with two 36 of insulating material, two 36 departments of insulating material around the acute angle electrode 34 are inlayed and are had an obtuse angle electrode 35, obtuse angle electrode 35 ground connection, acute angle electrode 34 with the liquid stream is insulating solution between the obtuse angle electrode 35, adopts the contact charging mode of improvement to charge, utilizes the high-voltage electrostatic field drive electron to pour into insulating solution's efflux into, makes the liquid droplet of atomizing negative charge, has realized the high-voltage electrostatic spraying to lipophilic solution insulating material.
In the embodiment shown in fig. 5, the microcapsule preparation apparatus provided by the present invention further includes a liquid supply system, the liquid supply system includes a hydrophilic solution storage tank 22 and a lipophilic solution storage tank 24, the hydrophilic solution storage tank 22 is communicated with the hydrophilic solution atomizer 3 through a first infusion pump 23 to supply hydrophilic solution to the hydrophilic solution atomizer 3, and the lipophilic solution storage tank 24 is communicated with the lipophilic solution atomizer 5 through a second infusion pump 25 to supply lipophilic solution to the lipophilic solution atomizer 5. The hydrophilic solution storage tank 22 is used for storing water-soluble material solution, and the lipophilic solution storage tank 24 is used for storing fat-soluble material solution; the first infusion pump 23 is used for conveying the hydrophilic solution to the atomizing nozzle at an adjustable flow rate, and the second infusion pump 25 is used for conveying the lipophilic solution to the atomizing nozzle at an adjustable flow rate.
In this embodiment, the microcapsule preparation apparatus provided by the present invention further includes a drying system, where the drying system includes a drying duct 8 and a heater, preferably an infrared heater, installed outside the drying duct 8, and in a preferred embodiment, a temperature sensor 19, an air pressure sensor 20, and a humidity sensor 21 may be connected to the drying duct 8.
In the embodiment shown in fig. 5, the microcapsule preparation apparatus provided by the present invention further includes a gas control system connected to the high-voltage electrostatic spraying system, the gas control system includes a gas cylinder 26 and a vacuum pump 13, the gas cylinder 26 is connected to the high-voltage electrostatic spraying system, a gas flow control valve 28 and a flow meter 27 are disposed on a connecting pipeline between the gas cylinder 26 and the high-voltage electrostatic spraying system, and the vacuum pump 13 pumps the gas in the entire apparatus to vacuum and adjust the gas pressure.
The gas control system is used to control the gas composition, gas pressure and gas flow strength inside the sealed container. When the spraying device works, firstly, the vacuum pump 13 pumps the air in the container to a certain vacuum, then the airflow control valve 28 is opened to enable inert gas or air with a certain flow rate to enter the container through the air inlet at the upper part of the spraying chamber 2, and the air pressure and the airflow speed in the container and the vacuum degree of the whole system can be adjusted by adjusting the air pumping speed of the vacuum pump 13 and the air inlet speed of the air inlet. Controlling gas components: protective gases such as nitrogen and helium are used for some microcapsule materials which are easy to oxidize, and air is used for materials which are not easy to oxidize. And (3) air pressure control: the evaporation speed of the water or volatile components in the liquid drops can be controlled by adjusting the air pressure in the container, and the method is suitable for the preparation requirements of different microcapsules.
In the implementation shown in fig. 5, the microcapsule preparation apparatus provided by the present invention further comprises a microcapsule grading and collecting system, the microcapsule grading and collecting system comprises a t-shaped sorting pipeline, a waste collecting tank 17 and a particle collector 10, a vertical pipe of the t-shaped sorting pipeline is communicated with the waste collecting tank 17, a horizontal pipe of the t-shaped sorting pipeline, that is, a collecting pipeline 16 is communicated with the particle collector 10, filtering nets 11 are installed on two inner side walls of the particle collector 10, and a microcapsule collecting tank 14 is installed below the particle collector 10. As shown in figure 4, the air flow carrying the dry particles enters the particle collector 10 through the collecting pipeline 16 under the action of the vacuum pump 13, the waste or large particle microcapsules in the air flow are separated from the air flow and enter the waste collecting tank 14 under the action of gravity, as shown in figure 5, the smaller particles enter the particle collector 10 along with the air flow, the microcapsules in accordance with the specification are collected by the filter screen 11, preferably, the filter screen 11 is connected with the vibrating motor 9 through a connecting rod, the collected microcapsule particles in accordance with the specification enter the microcapsule collecting tank 14 through timing vibration, and the smaller particles in accordance with the specification are carried away along with the air flow. The upper limit of the diameter range of the screened microcapsule particles can be adjusted by adjusting the air pressure and the air flow strength in the pipeline, and the diameters of the microcapsule particles screened in a grading way are controlled. The lower limit of the diameter range of the collected microcapsule particles can be controlled by selecting the mesh diameter, and the smaller capsule particles entering the particle collector 10 are classified and screened.
In a preferred embodiment, as shown in fig. 5, the connection parts of the waste collecting tank 17 and the microcapsule collecting tank 14 and the sealed container are respectively provided with a first connecting part 18 and a second connecting part 15 with sealed valves, when the collecting tank needs to be replaced, the sealed valves on the connecting mechanisms are closed, then the collecting tank is taken down, and after a new collecting tank is installed, the sealed valves are opened, so that the collecting tank can be replaced without destroying the tightness of the container.
In a specific embodiment, as shown in fig. 5, the present invention mounts flanges one 4, two 6 and three 12 at the corresponding locations of the apparatus, corresponding to the connection between the pipe ends, or the connection between two systems.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (11)
1. A microcapsule preparation method is characterized in that a high-voltage electrostatic spraying system is utilized, a hydrophilic solution atomizing nozzle and a lipophilic solution atomizing nozzle of the high-voltage electrostatic spraying system are respectively connected with a high-voltage electrostatic generator of the high-voltage electrostatic spraying system, the hydrophilic solution atomizing nozzle sprays hydrophilic fog drops with positive charges, the lipophilic solution atomizing nozzle sprays lipophilic fog drops with negative charges, electrostatic fields are established in spraying chambers below the hydrophilic solution atomizing nozzle and the lipophilic solution atomizing nozzle, charged drops with opposite charges generated by the two nozzles move relatively under the action of an electric field force, the hydrophilic fog drops with positive charges and the lipophilic fog drops with negative charges are respectively used as core material drops and capsule material drops, a certain number of capsule material drops can be combined onto the outer wall of the core material drops through electrostatic adsorption, when the charges of the capsule material drops adsorbed by the core material drops are equal to the charges of the capsule material drops, uncharged fused drops are formed, and the fused drops finally separate from the action of the electric field force to form microcapsule particles; in the process of mutual adsorption of the core material liquid drops and the capsule material liquid drops, the particle sizes of the core material liquid drops and the capsule material liquid drops are respectively adjusted by controlling the pressure of a nozzle, the charge-to-mass ratios of the core material liquid drops and the capsule material liquid drops are respectively adjusted by controlling the electrostatic high voltage of a high-voltage electrostatic generator, and the particle sizes of the liquid drops, the charge-to-mass ratios of the core material liquid drops and the capsule material liquid drops are set by the method, so that the quantitative control of the particle sizes and the thicknesses of the microcapsules is realized; the lipophilic solution atomizing spray head adopts a contact charging mode, an acute angle electrode connected with the output end of the high-voltage electrostatic generator is arranged in the center of the spray head, a grounded obtuse angle electrode is arranged around the acute angle electrode, the obtuse angle electrode is arranged on an insulating material II on the inner wall of the spray head, liquid flow between the acute angle electrode and the obtuse angle electrode is insulating solution, electrons on the acute angle electrode can be injected into the liquid flow under the action of an electric field, the electrons cannot move freely in the insulating solution, and finally lipophilic fog drops with negative charges are formed after being sprayed out through a spray nozzle; the radius R and wall thickness d of the resulting microcapsules are controlled by formula (i):
wherein, (q/m) 1 As core material the charge-to-mass ratio of the droplets, (q/m) 2 Is the charge-to-mass ratio of the capsule material drop, R 1 Radius of the droplet as core material, p 2 Is the density of the capsule material, p 1 The density of the core material is C% of the content of the capsule material in the capsule material water solution, and R is the radius of the microcapsule; and the radius R of the core material liquid drop 1 Radius R of the microcapsules-wall thickness d.
2. The method for preparing microcapsules of claim 1, wherein the hydrophilic solution atomizing nozzle adopts an induction charging mode, an annular induction electrode is arranged around the outer wall of the nozzle opening of the nozzle, the annular induction electrode is connected with the output end of the high-voltage electrostatic generator, the annular induction electrode is isolated from the inner solution of the hydrophilic solution atomizing nozzle by using an insulating material, the conductive solution in the nozzle is grounded, an electric field formed between the annular induction electrode and the conductive jet flow charges hydrophilic solution droplets, the polarity of the charges of the droplets is opposite to that of the induction electrode, and the hydrophilic droplets with positive charges are finally formed after being sprayed out through the nozzle.
3. The method of claim 1, wherein the unbound or inadequately bound charged liquid droplet or large particle microcapsules are subjected to a screening collection by an electric field: the liquid drops which are not or not fully combined still have electric charges, continue to move towards the opposite electrode plate under the action of the electric field force, are collected by the electrode plate, form large liquid drops to fall under the action of gravity after the liquid drops are gathered to a certain amount, and finally flow into a waste collecting tank arranged below along the wall of the container, or large-particle non-charged fused liquid drop microcapsules flow into the waste collecting tank arranged below under the action of gravity; in the process, the electric field voltage in the spray chamber can be adjusted to change the electric field intensity so as to adjust the screening intensity of the non-charged fused liquid drop microcapsules without liquid drops or large particles.
4. The microcapsule preparation method according to claim 1, wherein a "t" shaped sorting pipe and a particle collector are provided below the high-voltage electrostatic spraying system to select microcapsules of acceptable particle size: the pipeline combination department sets up "T" style of calligraphy and selects separately the pipeline, and when the air current that carries dry microcapsule granule got into the collection pipeline from dry pipeline, less granule got into the granule collector along with the air current through the collection pipeline, was equipped with the filter screen at two inside walls of granule collector, and the qualified microcapsule granule that the particle diameter is greater than filter screen mesh diameter is collected, and the granule that the particle diameter is less than filter screen mesh diameter is taken away by the air current.
5. A microcapsule preparation apparatus for carrying out the microcapsule preparation process according to any one of claims 1 to 4, comprising a high-pressure electrostatic spray system; wherein, high voltage electrostatic spraying system includes hydrophilic solution atomizer, lipophilic solution atomizer, high voltage electrostatic generator and spray chamber, hydrophilic solution atomizer and lipophilic solution atomizer are installed respectively on the spray chamber, hydrophilic solution atomizer and lipophilic solution atomizer respectively with high voltage electrostatic generator's different output is connected, electrically conductive solution ground connection in the hydrophilic solution atomizer, the spray chamber is equipped with two flat electrodes, and flat electrode connects high voltage electrostatic generator's output, and another flat electrode ground connection establishes the electrostatic field between two electrodes.
6. The apparatus for preparing microcapsules of claim 5, wherein the hydrophilic solution atomizer is used for electrostatic spraying of hydrophilic conductive solution, the hydrophilic solution atomizer adopts an induction charging mode, an annular induction electrode is arranged around the outer wall of the nozzle opening of the atomizer, the annular induction electrode is connected with the output end of the high voltage electrostatic generator, the inner wall of the hydrophilic solution atomizer is provided with a first insulating material, the annular induction electrode is isolated from the inner solution of the hydrophilic solution atomizer by the first insulating material, and the conductive solution in the atomizer is grounded.
7. The microcapsule preparation apparatus according to claim 5, wherein the lipophilic solution atomizing nozzle is used for electrostatic spraying of the lipophilic conductive solution, the lipophilic solution atomizing nozzle is provided with an acute angle electrode at the nozzle center, the acute angle electrode is connected with the output end of the high voltage electrostatic generator, the lipophilic solution atomizing nozzle is provided with a second insulating material on the inner wall, a blunt angle electrode is embedded in the second insulating material around the acute angle electrode, the blunt angle electrode is grounded, and the insulating solution flows between the acute angle electrode and the blunt angle electrode.
8. The microcapsule preparation apparatus as recited in claim 5, further comprising a liquid supply system comprising a hydrophilic solution reservoir and a lipophilic solution reservoir, the hydrophilic solution reservoir being in communication with the hydrophilic solution atomizer via a first infusion pump for supplying hydrophilic solution to the hydrophilic solution atomizer, and the lipophilic solution reservoir being in communication with the lipophilic solution atomizer via a second infusion pump for supplying lipophilic solution to the lipophilic solution atomizer.
9. The microcapsule preparation apparatus according to claim 5, further comprising a gas control system, wherein the gas control system comprises a gas cylinder and a vacuum pump, the gas cylinder is connected with the high-voltage electrostatic spraying system, a gas flow control valve and a flow rate meter are arranged on a connecting pipeline between the gas cylinder and the high-voltage electrostatic spraying system, and the vacuum pump controls the gas in the whole apparatus to be pumped to vacuum and regulate the gas pressure.
10. The microcapsule preparation apparatus according to claim 5, further comprising a drying system comprising a drying duct connected below the spray chamber and a heater installed outside the drying duct.
11. The apparatus for preparing microcapsules of claim 10, further comprising a microcapsule classifying and collecting system connected to the drying system, wherein the microcapsule classifying and collecting system comprises a t-shaped sorting pipe, a waste collecting tank, and a particle collector, wherein a vertical pipe of the t-shaped sorting pipe is communicated with the waste collecting tank, a horizontal pipe of the t-shaped sorting pipe is communicated with the particle collector, two inner side walls of the particle collector are provided with filter screens, and a microcapsule collecting tank is arranged below the particle collector.
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| CN100488618C (en) * | 2006-09-25 | 2009-05-20 | 上海理工大学 | Method for producing liquid core microcapsule by electrostatic spraying |
| CN102407088A (en) * | 2010-09-21 | 2012-04-11 | 中国科学院化学研究所 | Preparation method for phase-change energy-storage microcapsule and phase-change energy-storage microcapsule |
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| CN103933908B (en) * | 2014-04-25 | 2016-04-06 | 江苏大学 | The Apparatus for () and method therefor of microcapsules is prepared in a kind of liquid liquid electrostatic microjet atomization |
| CN208049904U (en) * | 2018-02-26 | 2018-11-06 | 上海理工大学 | A kind of simple high-voltage electrostatic microcapsules generating means |
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