CN114712328B - Method for preparing sustained-release propolis saccule based on natural shellac composite wall material - Google Patents

Method for preparing sustained-release propolis saccule based on natural shellac composite wall material Download PDF

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CN114712328B
CN114712328B CN202210319066.1A CN202210319066A CN114712328B CN 114712328 B CN114712328 B CN 114712328B CN 202210319066 A CN202210319066 A CN 202210319066A CN 114712328 B CN114712328 B CN 114712328B
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water
propolis
saccule
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CN114712328A (en
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谌迪
肖朝耿
卢文静
叶沁
张岑
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Zhejiang Academy of Agricultural Sciences
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    • A61K35/644Beeswax; Propolis; Royal jelly; Honey
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5036Polysaccharides, e.g. gums, alginate; Cyclodextrin
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    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/10Vacuum distillation
    • B01D3/106Vacuum distillation with the use of a pump for creating vacuum and for removing the distillate
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract

The invention relates to the technical field of deep processing of propolis raw materials, and particularly discloses a method for preparing a slow-release propolis saccule based on a natural shellac composite wall material, which comprises the steps of extracting raw propolis for the first time with an ethanol solution in water bath, extracting for the second time with water bath ultrasound, and extracting for the third time in water bath to obtain an extracting solution I; filtering the extract I to obtain a concentrate I; concentrate IRemoving water by a water removal device, and adding an absolute ethyl alcohol solution for dissolution to obtain an extract II; filtering the extracting solution II through a water phase microporous filter membrane to obtain extracting solution III; adding shellac into Na 2 CO 3 Obtaining a solution I in the solution; adding sodium alginate into water to obtain a solution II; mixing the solution I and the solution II in equal volume to obtain a solution III; adding the extract III into the solution III, and performing degassing treatment to obtain extract IV; dripping the extracting solution IV into CaCl 2 And (3) performing crosslinking treatment in the solution, filtering out and drying to obtain the slow-release propolis saccule. The invention can meet the demand of the slow release of the propolis and has better health effect.

Description

Method for preparing sustained-release propolis saccule based on natural shellac composite wall material
Technical Field
The invention relates to the technical field of deep processing of propolis raw materials, in particular to a method for preparing a slow-release propolis saccule based on a natural shellac composite wall material.
Background
The China is the first big world for raising bees and is also the world for producing and selling the bee products with the largest global. Propolis is a colloidal solid which is obtained by collecting resin from plant buds and trunks of western bees and mixing with the secretion of the palate gland, beeswax and the like, is a precious and wonderful natural product with natural aromatic smell, has various biological activities and pharmacological functions of resisting virus, resisting bacteria, resisting fungi, reducing blood fat, reducing blood sugar, purifying blood, promoting tissue regeneration, enhancing organism immunity, preventing and treating cardiovascular diseases, diabetes, chronic prostatitis and the like, is known as vascular scavenger, and is a bee product with great development and utilization value. Although the domestic 'propolis heat' is formed, the processing and utilization degree of the propolis is still not high in general, the development technical level of the product is relatively low, the biological activity and the slow release effect of functional factors of the product are difficult to ensure, and the quality of the propolis product is not ideal.
Shellac, also called lac, red gum, shikonin and the like, is a purple natural resin obtained by extracting secretions of lac worms after absorbing sap of host trees, and is mainly distributed in Yunnan province in the production place of China. Shellac has been used as a pharmaceutical matrix and food color for over a thousand years, and in the pharmaceutical industry shellac has the characteristic of plastic film forming property, and is commonly used as a film forming matrix in external preparations. Along with the development of biomedicine and the rising trend of natural therapy, the coating material returns to the nature to become an important development direction, and more attention is paid to the development of green health care food. The traditional propolis product is mainly prepared by dissolving propolis with polyethylene glycol or oil, and potential health risks can be caused to human bodies after long-term consumption, so that the propolis gel beads prepared by the invention mainly contain natural components, and the damage to the health of human bodies caused by excessive intake of solvents such as polyethylene glycol and the like is greatly reduced.
The invention takes propolis as a core material, takes sodium alginate and shellac as wall materials, adopts a sharp hole-coagulation bath method to stabilize the propolis and slowly release functional factors thereof, analyzes the influence of three factors of core wall ratio, shellac concentration and embedding time in the propolis microcapsule on embedding rate and drug loading rate, develops researches on microcapsule swelling degree, propolis release rate and the like under gastrointestinal tract simulation conditions, and the related technology can improve the added value and domestic and foreign market competitiveness of the propolis product, and has important significance for increasing economic benefit of the propolis product processing industry and accelerating deep processing and industrialization process of the propolis resource product.
Disclosure of Invention
The invention aims to solve the technical problems of the prior propolis products, and provides a method for preparing a slow-release propolis saccule based on a natural shellac composite wall material, which has the characteristics of meeting the requirement of slow release of propolis and having better health effect.
The technical scheme of the invention is as follows: a method for preparing a slow-release propolis saccule based on natural shellac composite wall materials, which comprises the following steps,
(a) Soaking raw material propolis in ethanol solution with a certain concentration under water bath for first extraction, performing water bath ultrasonic second extraction, and performing water bath third extraction to obtain extract I;
(b) Filtering the extract I to obtain a concentrate I; removing water from the concentrate I through a water removing device under vacuum decompression, and adding a proper amount of absolute ethyl alcohol solution for dissolution to obtain an extract II;
(c) Filtering the extract II through a water phase microporous filter membrane to obtain extract III, and freezing and preserving the extract III;
(d) Adding a certain amount of shellac into Na with a certain concentration 2 CO 3 Stirring the solution until the solution is completely dissolved to obtain a solution I;
(e) Adding a certain amount of sodium alginate into a certain amount of water, and stirring until the sodium alginate is completely dissolved to obtain a solution II;
(f) Mixing the solution I and the solution II in equal volumes to obtain a solution III;
(g) Rapidly adding the frozen extracting solution III in the step (c) into the solution III in the step (f) according to a specific proportion, standing for a period of time, and then carrying out degassing treatment to obtain extracting solution IV;
(h) Slowly dripping the extracting solution IV into CaCl with a certain concentration 2 And (3) performing crosslinking treatment in the solution, filtering out and drying after crosslinking is finished, and obtaining the slow-release propolis saccule. The propolis is used as a core material, sodium alginate and shellac are used as composite wall materials, the drug loading rate of the propolis saccule prepared by adopting a sharp hole-coagulation bath method can reach 68%, and the embedding rate can reach 90.46%; after the invention is digested in vitro by gastrointestinal tract, the whole propolis saccule keeps relatively complete sphericity, and can meet the requirement of slow release of propolis; the main components of the propolis saccule prepared by the invention are natural components, which are different from the traditional propolis saccule preparation in the market at present, which requires a large amount of solvents such as polyethylene glycol and oil, and can effectively avoid the potential risk of excessive intake of polyethylene glycol and oil to human health; the water removal device introduced by the invention can effectively remove water, reduce the influence on the subsequent process, and obviously improve the quality of the finished product.
Preferably, in the step (a), the feed liquid ratio of the raw material propolis to the ethanol solution is 1:10-20.
Preferably, in the step (a), the feed liquid ratio of the raw material propolis to the ethanol solution is 1:15.
preferably, in the step (a), the concentration of the ethanol solution is 85%.
Preferably, in the step (a), the water bath temperature is 40 to 50 ℃.
Preferably, in the step (a), the first extraction time is 10min to 40min.
Preferably, in the step (a), the second extraction time is 20min to 30min.
Preferably, in the step (a), the third extraction time is 1 to 2 hours.
Preferably, in the step (b), the concentrate I is subjected to vacuum depressurization to remove water by a water removal device at a temperature of not higher than 50 ℃.
Preferably, in the step (b), the absolute ethanol solution is added in a volume which is 1.6 to 2 times of the mass of the raw material propolis.
Preferably, in the step (c), the extract II is dropped onto the aqueous phase microporous membrane by using a needle tube for filtration.
Preferably, in the step (c), the pore size of the aqueous phase microporous filter membrane is 0.4um to 0.6um.
Preferably, in the step (c), the cryopreservation temperature is from-25℃to-15 ℃.
Preferably, in the step (d), shellac is mixed with Na 2 CO 3 The feed liquid ratio of the solution is 1/20-1/2.
Preferably, in the step (d), na 2 CO 3 The concentration of the solution was 0.1mol/mL.
Preferably, in the step (d), the stirring speed is 200r/min to 300r/min.
Preferably, in the step (d), the stirring temperature is 55 to 65 ℃.
Preferably, in the step (e), the feed liquid ratio of sodium alginate to water is 1:35 to 45.
Preferably, in the step (e), the stirring speed is 200r/min to 300r/min.
Preferably, in the step (e), the stirring temperature is 45 to 55 ℃.
Preferably, in the step (g), the ratio of the extract III to the solution III is 1/6 to 1/2.
Preferably, in the step (h), the extracting solution IV is slowly dropped into CaCl with a certain concentration by using a needle tube 2 In solution.
Preferably, in the step (h), caCl 2 The concentration of the solution was 1.5mg/mL.
Preferably, in the step (h), the crosslinking time is 10 to 60 minutes.
Preferably, in the step (h), the drying temperature is 35 to 37 ℃.
Preferably, in the step (h), the drying time is 20 to 24 hours.
Preferably, the water removing device comprises a main body mechanism, a gas control mechanism, a vibration mechanism and a water removing mechanism; the main body mechanism comprises a dewatering bin, a main air pipe, an auxiliary air pipe, a first electromagnetic valve, a second electromagnetic valve, a porous screen plate and an electromagnet; the main tuber pipe is installed in dewatering storehouse top, assist the tuber pipe to install in dewatering storehouse below, first solenoid valve is installed on the main tuber pipe, the second solenoid valve is installed on assisting the tuber pipe, porous otter board is installed in dewatering storehouse inside, the electro-magnet is installed in porous otter board upside. The main body mechanism can realize the selection to the dewatering mode, both can select the mode of hot-blast stoving, also can select the mode of vacuum decompression, can select in a flexible way in order to satisfy different needs, when selecting hot-blast stoving mode, with first solenoid valve, the second solenoid valve is all opened, input hot-blast in to the dewatering storehouse through the second solenoid valve, hot-blast can carry out hot-blast stoving to the material this moment, this is the stoving means of initiative intervention, under the higher circumstances of material moisture content, can accelerate drying effect through the means of hot-blast stoving, when selecting the vacuum decompression mode, close the second solenoid valve, open first solenoid valve and external negative pressure equipment, reach the purpose of decompression through absorbing the gas in the dewatering storehouse, thereby accelerate the escape of moisture, stoving effect is also more degree of depth simultaneously, the technician can select different modes according to different circumstances, also can select simultaneously, firstly reduce moisture fast through hot-blast stoving mode, then deepen drying effect through the vacuum decompression mode.
Preferably, the air control mechanism comprises a gas collecting tube, an upper air expansion cover, a lower air expansion cover and a plurality of splitter plates; the gas collecting tube and the lower expansion hood are respectively and vertically symmetrically connected to the upper end and the lower end of the gas collecting tube, and the flow dividing plates are uniformly distributed in the gas collecting tube; the gas control mechanism is arranged at the lower side of the porous screen plate, and the gas collecting tube is fixedly connected to the lower end of the porous screen plate. The gas collecting tube plays the centralized effect to the air current, can be simultaneously after the concentration of gas collecting tube in the fan housing that expands down fine carry out desorption moisture to dewatering mechanism to after receiving the magnetism of electro-magnet and inhale the effect, can make dewatering mechanism abundant even contact with the raw materials on the porous screen plate under the dispersion effect of flow distribution plate, thereby realize good flip effect, improve the dewatering effect.
Preferably, the vibration mechanism includes a vibration plate, a vibration motor, and a plurality of rebound bags; the vibrating plate is connected with the vibrating end of the vibrating motor, and the rebound bags are uniformly distributed at the upper end of the vibrating plate; the vibrating mechanism is arranged on the lower side of the air control mechanism, the vibrating motor is fixedly arranged on the bottom end in the dewatering bin, and the vibrating plate is positioned on the lower side of the lower expansion hood. The vibrating motor can drive the vibrating plate to generate high-frequency vibration, after the water removing mechanism falls down, the vibrating motor can fully contact with air flow in the lower expansion fan cover to realize desorption under the dispersion and rebound actions of the rebound bag, so that good water absorption performance is kept in the next contact with raw materials.
Preferably, the water removing mechanism comprises a plurality of water removing components, wherein the water removing components are arranged on the upper side of the vibrating plate, and are lifted to be adsorbed on the lower side of the porous screen plate after the electromagnet is started to apply a magnetic field; the water removal component comprises a top material particle, a limiting hemisphere, a transparent hemisphere, a water absorption fiber bundle, color-changing silica gel particles and magnetic powder; the restriction hemisphere and transparent hemisphere symmetry connect, the roof grain is inlayed and is connected on the restriction hemisphere, the silica gel granule that discolours is filled in transparent hemisphere, the fibre bundle that absorbs water is evenly inlayed on the roof grain, and absorbs water fibre bundle one end extends to the roof grain outside, and the other end extends to the silica gel granule inboard that discolours, the magnetic powder is filled in the roof grain is inboard. The top material particles and the magnetic powder are matched, so that the material can be actively lifted under the magnetic attraction of the electromagnet and extruded and turned, and the water removal effect is improved; the fiber bundles that absorb water extend to the top material outside and can improve the effect of turning over to the raw materials, can stretch into the inside moisture that carries out certain absorption of raw materials simultaneously, and the transmission carries out the characterization to the dewatering degree in the allochroic silica gel granule simultaneously, and the restriction hemisphere then plays the restriction effect, and its diameter is greater than the aperture of porous otter board and can't go on rising, only can turn over the raw materials and absorb water, then naturally falls down and desorbs, helps the repetition implementation of above-mentioned process.
Preferably, in the step, the frozen extracting solution III is quickly added into the solution III in the step through a quick adding mechanism according to a specific proportion; the quick adding mechanism comprises a liquid storage tank, a pressing column, a liquid adding pipe, an electromagnet and a liquid injection pipe; the liquid filling pipe is fixedly arranged on the side wall of the liquid storage tank, the electromagnets are symmetrically arranged at the lower end of the liquid storage tank, the liquid filling pipe is uniformly arranged at the lower end of the liquid storage tank, the liquid filling pipe is positioned between a pair of electromagnets, and the liquid filling pipe is communicated with the liquid storage tank. The extraction liquid III in the liquid storage tank is extruded by the pressing column to accelerate the flow, then is released downwards through the liquid injection pipe and added into the solution III, and the magnetic ring is adsorbed in two directions by intermittently applying magnetic fields through the electromagnets on the left side and the right side, so that the main pipe is driven to shake left and right, and the release of the extraction liquid III can be accelerated.
Preferably, the liquid injection pipe comprises a main pipe, a magnetic ring, a horn mouth, a waterproof sleeve and an electric heating wire; the main pipe, the magnetic ring and the horn mouth are sequentially connected from top to bottom, the main pipe is fixedly connected to the lower end of the liquid storage tank and is communicated with the liquid storage tank, the waterproof sleeve is inserted and arranged at the center in the main pipe, and the electric heating wire is arranged at the inner side of the waterproof sleeve. The solution III can be more widely dispersed and enter the solution III through the horn mouth, and the electric heating wire can heat the extracting solution III to avoid the excessively low temperature; the quick adding mechanism not only can realize quick adding of the extracting solution III, but also can be dispersed into the solution III, and the subsequent standing time can be greatly shortened.
The invention has the following beneficial effects:
(1) The propolis is used as a core material, sodium alginate and shellac are used as composite wall materials, the drug loading rate of the propolis saccule prepared by adopting an orifice-coagulation bath method can reach 68%, and the embedding rate can reach 90.46%;
(2) After in vitro gastrointestinal tract digestion, the whole propolis saccule keeps relatively complete sphericity, and can meet the requirement of slow release of propolis;
(3) The main components of the prepared propolis capsule are natural components, which is different from the traditional propolis capsule preparation in the market at present, which requires a large amount of solvents such as polyethylene glycol and oil, and can effectively avoid the potential risk of excessive intake of polyethylene glycol and oil to human health;
(4) The introduced water removal device can effectively remove water, reduce the influence on the subsequent process, and obviously improve the quality of finished products.
Drawings
FIG. 1 is a schematic diagram of a water removal device according to the present invention;
FIG. 2 is a schematic diagram of the structure of the air control mechanism of the present invention;
FIG. 3 is a schematic view of a vibration mechanism according to the present invention;
FIG. 4 is a schematic diagram of a water removal mechanism according to the present invention;
FIG. 5 is a schematic view of the quick adding mechanism of the present invention;
FIG. 6 is a schematic view of the structure of the liquid injection tube of the present invention;
FIG. 7 is a graph showing the effect of shellac concentration on the embedding rate of propolis flavone in the present invention;
FIG. 8 is a graph showing the effect of shellac concentration on propolis flavone loading of the present invention;
FIG. 9 is a graph showing the effect of core-wall alignment on the embedding rate of propolis according to the present invention;
FIG. 10 is a graph showing the effect of core-wall comparison on propolis drug loading in accordance with the present invention;
FIG. 11 is a graph showing the effect of core wall comparison on the cumulative release rate of propolis flavonoids;
FIG. 12 is a graph showing the effect of core wall ratios on microcapsule swelling capacity in accordance with the present invention;
FIG. 13 is a graph showing the effect of time of encapsulation on the encapsulation efficiency of microcapsules according to the present invention;
FIG. 14 is a graph showing the effect of embedding time on the drug loading of microcapsules according to the present invention;
FIG. 15 is a graph showing the effect of embedding time on the swelling ratio of microcapsules according to the present invention.
The marks in the drawings are: 1-a body mechanism; 101-a dewatering bin; 102-a main air pipe; 103-auxiliary air pipes; 104-a first solenoid valve; 105-a second solenoid valve; 106-a porous screen; 107-an electromagnet; 2-an air control mechanism; 201-gas collecting pipes; 202-an upper expansion hood; 203-a lower expansion hood; 204-a diverter plate; 3-a vibration mechanism; 301-a vibrating plate; 302-a vibration motor; 303-rebound package; 4-a water removal mechanism; 401-top pellet; 402-limit hemisphere; 403-transparent hemispheres; 404-bundles of water-absorbing fibers; 405-color-changing silica gel particles; 406-magnetic powder; 5-a quick adding mechanism; 501-a liquid storage tank; 502-pressing down a column; 503-a liquid adding pipe; 504-an electromagnet; 505-liquid injection pipe; 5051—a main pipe; 5052-a magnetic ring; 5053-flare; 5054-a waterproof jacket; 5055-an electric heating wire.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments, and that all other embodiments obtained by persons of ordinary skill in the art without making creative efforts based on the embodiments in the present invention are within the protection scope of the present invention.
In the description of the present invention, it should be noted that the positional or positional relationship indicated by the terms such as "upper", "lower", "inner", "outer", "top/bottom", etc. are based on the positional or positional relationship shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "configured to," "engaged with," "connected to," and the like are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
A method for preparing a slow-release propolis saccule based on natural shellac composite wall materials, which comprises the following steps,
(a) Soaking raw material propolis in ethanol solution with a certain concentration under water bath for first extraction, performing water bath ultrasonic second extraction, and performing water bath third extraction to obtain extract I; the feed liquid ratio of the raw material propolis to the ethanol solution is 1:10-20. Better, the feed liquid ratio of raw material propolis to ethanol solution is 1:15. the ethanol solution concentration was 85%. The water bath temperature is 40-50 ℃. The first extraction time is 10 min-40 min. The second extraction time is 20 min-30 min. The third extraction time is 1-2 h.
(b) Filtering the extract I to obtain a concentrate I; removing water from the concentrate I through a water removing device under vacuum decompression, and adding a proper amount of absolute ethyl alcohol solution for dissolution to obtain an extract II; the concentrate I is subjected to vacuum depressurization to remove water by a water removal device at a temperature of not higher than 50 ℃. The added volume of the absolute ethyl alcohol solution is 1.6-2 times of the mass of the raw material propolis.
(c) Filtering the extract II through a water phase microporous filter membrane to obtain extract III, and freezing and preserving the extract III; and (3) dripping the extract II onto a water phase microporous filter membrane by using a needle tube, and filtering. The aperture of the water phase microporous filter membrane is 0.4 um-0.6 um. The freezing preservation temperature is minus 25 ℃ to minus 15 ℃.
(d) Adding a certain amount of shellac into Na with a certain concentration 2 CO 3 Stirring the solution until the solution is completely dissolved to obtain a solution I; na (Na) 2 CO 3 The concentration of the solution was 0.1mol/mL. Shellac and Na 2 CO 3 The feed liquid ratio of the solution is 1/20-1/2. The stirring speed is 200 r/min-300 r/min. The stirring temperature is 55-65 ℃.
(e) Adding a certain amount of sodium alginate into a certain amount of water, and stirring until the sodium alginate is completely dissolved to obtain a solution II; the feed liquid ratio of sodium alginate to water is 1:35 to 45. The stirring speed is 200 r/min-300 r/min. The stirring temperature is 45-55 ℃.
(f) Mixing the solution I and the solution II in equal volumes to obtain a solution III;
(g) Rapidly adding the frozen extracting solution III in the step (c) into the solution III in the step (f) according to a specific proportion, standing for a period of time, and then carrying out degassing treatment to obtain extracting solution IV; the ratio of the extracting solution III to the solution III is 1/6-1/2.
(h) Slowly dripping the extracting solution IV into CaCl with a certain concentration 2 And (3) performing crosslinking treatment in the solution, filtering out and drying after crosslinking is finished, and obtaining the slow-release propolis saccule. Slowly dripping the extracting solution IV into CaCl with a certain concentration by using a needle tube 2 In solution. CaCl (CaCl) 2 The concentration of the solution was 1.5mg/mL. The crosslinking time is 10 min-60 min. The drying temperature is 35-37 ℃. The drying time is 20-24 hours.
The water removal device shown in fig. 1 comprises a main body mechanism 1, a gas control mechanism 2, a vibration mechanism 3 and a water removal mechanism 4; the main body mechanism comprises a dewatering bin 101, a main air pipe 102, an auxiliary air pipe 103, a first electromagnetic valve 104, a second electromagnetic valve 105, a porous screen 106 and an electromagnet 107; the main air pipe 102 is arranged above the dewatering bin 101, the auxiliary air pipe 103 is arranged below the dewatering bin 101, the first electromagnetic valve 104 is arranged on the main air pipe 102, the second electromagnetic valve 105 is arranged on the auxiliary air pipe 103, the porous screen plate 106 is arranged inside the dewatering bin 101, and the electromagnet 107 is arranged on the upper side of the porous screen plate 106.
The gas control mechanism 2 comprises a gas collecting tube 201, an upper expansion hood 202, a lower expansion hood 203 and a plurality of flow dividing plates 204 as shown in fig. 2; the gas collecting tube 201 and the lower expansion hood 203 are respectively and vertically symmetrically connected to the upper end and the lower end of the gas collecting tube 201, and the splitter plates 204 are uniformly distributed in the gas collecting tube 201; the gas control mechanism 2 is arranged at the lower side of the porous screen plate 106, and the gas collecting tube 201 is fixedly connected to the lower end of the porous screen plate 106.
The vibration mechanism 3 includes a vibration plate 301, a vibration motor 302, and a plurality of rebound bags 303 as shown in fig. 3; the vibrating plate 301 is connected with the vibrating end of the vibrating motor 302, and the rebound bags 303 are uniformly distributed at the upper end of the vibrating plate 301; the vibration mechanism 3 is installed at the lower side of the air control mechanism 2, the vibration motor 302 is fixedly installed at the inner bottom end of the dewatering bin 101, and the vibration plate 301 is positioned at the lower side of the lower expansion hood 203.
The water removing mechanism 4 comprises a plurality of water removing components, the water removing components are placed on the upper side of the vibrating plate 301, and the water removing components are lifted to be adsorbed on the lower side of the porous screen plate 106 after the electromagnet 107 is started to apply a magnetic field; the water removal assembly comprises a top pellet 401, a limiting hemisphere 402, a transparent hemisphere 403, a water absorbing fiber bundle 404, color changing silica gel particles 405 and magnetic powder 406 as shown in fig. 4; the limiting hemisphere 402 and the transparent hemisphere 403 are symmetrically connected, the top material particle 401 is inlaid and connected on the limiting hemisphere 402, the allochroic silica gel particles 405 are filled in the transparent hemisphere 403, the water-absorbing fiber bundles 404 are uniformly inlaid on the top material particle 401, one end of each water-absorbing fiber bundle 404 extends to the outer side of the top material particle 401, the other end extends to the inner side of the allochroic silica gel particles 405, and the magnetic powder 406 is filled in the inner side of the top material particle 401.
In the step (g), the frozen extracting solution III is rapidly added into the solution III in the step (f) according to a specific proportion through a rapid adding mechanism 5 shown in fig. 5; the quick adding mechanism 5 comprises a liquid storage tank 501, a pressing post 502, a liquid adding pipe 503, an electromagnet 504 and a liquid injecting pipe 505; the lower pressure column 502 is slidably mounted on the upper side of the liquid storage tank 501, the liquid filling pipe 503 is fixedly mounted on the side wall of the liquid storage tank 501, the electromagnets 504 are symmetrically mounted on the lower end of the liquid storage tank 501, the liquid filling pipe 505 is uniformly mounted on the lower end of the liquid storage tank 501, the liquid filling pipe 505 is located between the electromagnets 504, and the liquid filling pipe 505 is communicated with the liquid storage tank 501.
The pour tube 505 includes a main tube 5051, a magnetic ring 5052, a flare 5053, a waterproof jacket 5054, and an electric heating wire 5055 as shown in fig. 6; the main pipe 5051, the magnetic ring 5052 and the flare 5053 are sequentially connected from top to bottom, the main pipe 5051 is fixedly connected to the lower end of the liquid storage tank 501 and is communicated with the liquid storage tank 501, the waterproof sleeve 5054 is inserted and installed at the center in the main pipe 5051, and the electric heating wire 5055 is installed on the inner side of the waterproof sleeve 5054.
A method for preparing a slow-release propolis saccule based on natural shellac composite wall materials, which comprises the following steps,
soaking and extracting propolis in ethanol with a certain concentration in water bath, performing water bath ultrasonic extraction, and extracting in water bath for 2 hr to obtain extractive solution I.
Carrying out suction filtration on the extract I to obtain a concentrate I, carrying out vacuum decompression on the concentrate I through a water removal device to remove water, and adding a proper amount of absolute ethyl alcohol solution for dissolution to obtain an extract II;
filtering the extracting solution II by using a 1mL needle tube and combining a water phase microporous filter membrane with the diameter of 0.4-0.6 microns, and then freezing and preserving at the temperature of minus 20 ℃ for standby, namely extracting solution III;
adding a certain amount of shellac into Na with a certain concentration 2 CO 3 Magnetically stirring the solution until the solution is completely dissolved to obtain a solution I; adding a certain amount of sodium alginate into a certain amount of water, and magnetically stirring until the sodium alginate is completely dissolved to obtain a solution II;
Uniformly mixing the solution I and the solution II in equal volume to obtain a solution III; adding the extracting solution III into the solution III according to a specific proportion, wherein the proportion of the extracting solution III to the solution III is 1: 6-3: and 6, standing for a period of time, and then carrying out degassing treatment to obtain an extract IV.
Slowly dripping the extracting solution IV into CaCl with a certain concentration by a needle tube 2 And (3) performing crosslinking treatment in the solution, and filtering out and drying after crosslinking is finished to obtain the slow-release propolis saccule.
The feed liquid ratio of the raw material propolis to the ethanol solution is 1:15, the concentration of the ethanol solution is 85%, the water bath temperature is 40-50 ℃, the ultrasonic extraction time is 20-30 min, and the soaking is continued in the water bath at 40-50 ℃ for 1-2 h after the ultrasonic treatment is finished.
The concentrate I is decompressed and removed with water at the temperature of not higher than 50 ℃, and the addition amount of the absolute ethyl alcohol solution is 1.6-2 (v: m) times of that of the raw material propolis.
Shellac and Na 2 CO 3 The feed liquid ratio of the solution is 1: 20-1:2, na 2 CO 3 The concentration of the solution is 0.1moL/mL, and the solution is stirred magnetically at 60 ℃ for 200-300 r/min until the solution is completely dissolved to obtain solution I; the feed liquid ratio of sodium alginate to water is 1:40, at 50 ℃ using a magnetic stirrer at 200-300 r/minStirring until dissolved under the stirring to obtain solution II.
CaCl 2 The concentration of the solution is 1.5mg/mL, and the extracting solution IV and CaCl 2 The cross-linking time of the solution is 10-60 min; and (3) drying the embedded microcapsule in an oven with the temperature lower than 37 ℃ for 20-24 hours.
The water removing device comprises a main body mechanism 1, an air control mechanism 2, a vibration mechanism 3 and a water removing mechanism 4, wherein the main body mechanism comprises a water removing bin 101, a main air pipe 102, an auxiliary air pipe 103, a first electromagnetic valve 104, a second electromagnetic valve 105, a porous screen 106 and an electromagnet 107, the main air pipe 102 is arranged above the water removing bin 101, the auxiliary air pipe 103 is arranged below the water removing bin 101, the first electromagnetic valve 104 is arranged on the main air pipe 102, the second electromagnetic valve 105 is arranged on the auxiliary air pipe 103, the porous screen 106 is arranged inside the water removing bin 101, the electromagnet 107 is arranged on the upper side of the porous screen 106, the main body mechanism 1 can realize the selection of a water removing mode, can select a hot air drying mode, can also select a vacuum decompression mode, can flexibly select to meet different requirements, when the hot air drying mode is selected, the first electromagnetic valve 104 and the second electromagnetic valve 105 are both opened, hot air is input into the dewatering bin 101 through the second electromagnetic valve 105, at the moment, the hot air can dry materials through hot air, the drying method is an active intervention drying method, under the condition that the water content of the materials is high, the drying effect can be accelerated through the hot air drying method, when the vacuum decompression mode is selected, the second electromagnetic valve 105 is closed, the first electromagnetic valve 104 is opened, negative pressure equipment is externally connected, the purpose of decompressing is achieved through absorbing the gas in the dewatering bin 101, so that the escape of moisture is accelerated, meanwhile, the drying effect is deeper, technicians can select different modes according to different conditions, the drying effect can be selected simultaneously, namely, the moisture is quickly reduced through the hot air drying mode, and then the drying effect is deepened through the vacuum decompression mode.
The gas control mechanism 2 comprises a gas collecting tube 201, an upper gas expansion cover 202, a lower gas expansion cover 203 and a plurality of flow dividing plates 204, wherein the gas collecting tube 201 and the lower gas expansion cover 203 are respectively and vertically symmetrically connected to the upper end and the lower end of the gas collecting tube 201, the flow dividing plates 204 are uniformly distributed in the gas collecting tube 201, the gas control mechanism 2 is arranged on the lower side of the porous screen plate 106, the gas collecting tube 201 is fixedly connected to the lower end of the porous screen plate 106, the gas collecting tube 201 plays a role in concentrating air flow, and meanwhile, after the concentration of the gas collecting tube 201, moisture can be well desorbed from the water removing mechanism 4 in the lower gas expansion cover 203, and after the magnetic attraction of the electromagnet 107 is received, the water removing mechanism 4 can be fully and uniformly contacted with raw materials on the porous screen plate 106 under the dispersing action of the flow dividing plates 204, so that good turning action is realized, and the water removing effect is improved.
The vibration mechanism 3 comprises a vibration plate 301, a vibration motor 302 and a plurality of rebound bags 303, the vibration plate 301 is connected with the vibration end of the vibration motor 302, the rebound bags 303 are uniformly distributed at the upper end of the vibration plate 301, the vibration mechanism 3 is arranged at the lower side of the air control mechanism 2, the vibration motor 302 is fixedly arranged at the inner bottom end of the dewatering bin 101, the vibration plate 301 is arranged at the lower side of the lower expansion hood 203, the vibration motor 302 can drive the vibration plate 301 to generate a high-frequency vibration phenomenon, after the dewatering mechanism 4 falls down, due to the vibration effect, and under the dispersion and rebound effect of the rebound bags 303, the vibration bags 303 can fully contact with air flow in the lower expansion hood 203 to realize desorption, so that the good water absorption performance is kept in the next contact with raw materials.
The dewatering mechanism 4 includes a plurality of dewatering subassemblies, dewatering subassembly is placed in vibrating plate 301 upside, after the magnetic field is applyed in electro-magnet 107 start-up, rising adsorption to porous otter board 106 downside, dewatering subassembly includes the top grain 401, restriction hemisphere 402, transparent hemisphere 403, water absorption fiber bundle 404, allochroic silica gel granule 405 and magnetic powder 406, restriction hemisphere 402 and transparent hemisphere 403 symmetrical connection, the top grain 401 inlay and connect on restriction hemisphere 402, water absorption fiber bundle 404 evenly inlay on top grain 401 in transparent hemisphere 403 is filled to allochroic silica gel granule 405, and water absorption fiber bundle 404 one end extends to top grain 401 outside, the other end extends to allochroic silica gel granule 405 inboard, magnetic powder 406 is filled in top grain 401 inboard, top grain 401 and magnetic powder 406 cooperation, both can initiatively rise and extrude the stirring to the raw materials under the magnetic absorption effect of electro-magnet 107, thereby improve the dewatering effect, water absorption fiber bundle 404 extends to the top grain 401 outside and can stretch into the inside of raw materials and absorb the moisture to a certain extent, simultaneously in transparent hemisphere 405 carries out the characteristic that water absorption is carried out, and then can's the diameter is repeated in the porous otter board is carried out to the porous to the water absorption fiber bundle 401, and then can't be carried out the diameter is repeated in the porous limiting process is carried out under the porous otter board's of the porous particle 401.
The extracting solution III is added fast through a fast adding mechanism 5, the fast adding mechanism 5 comprises a liquid storage tank 501, a lower pressing column 502, a liquid adding pipe 503, electromagnets 504 and a liquid injecting pipe 505, the lower pressing column 502 is slidingly arranged on the upper side of the liquid storage tank 501, the liquid adding pipe 503 is fixedly arranged on the side wall of the liquid storage tank 501, the electromagnets 504 are symmetrically arranged at the lower end of the liquid storage tank 501, the liquid injecting pipe 505 is uniformly arranged at the lower end of the liquid storage tank 501 and between a pair of electromagnets 504, the liquid injecting pipe 505 is communicated with the liquid storage tank 501, the liquid injecting pipe 505 comprises a main pipe 5051, a magnetic ring 5052, a horn 5053, a waterproof sleeve 5054 and an electric heating wire 5055, the main pipe 5051, the magnetic ring 5052 and the horn 5053 are sequentially connected from top to bottom, and the main pipe 5051 is fixedly connected to the lower end of the liquid storage tank 501 and is communicated with the liquid storage tank 501, waterproof jacket 5054 inserts and installs in the interior center department of being responsible for 5051, electric heating wire 5055 installs in waterproof jacket 5054 inboard, through pushing down the extrusion of post 502 to extract III in the liquid reserve tank 501 and accelerate the flow, then release down through annotate liquid pipe 505 and add in solution III, intermittently apply the magnetic field to carry out the absorption of two directions to magnetic ring 5052 through the electro-magnet 504 of left and right sides, make it drive the main pipe 5051 and rock about, not only can accelerate the release of extract III, can more disperse wide entering into solution III simultaneously through horn 5053, and electric heating wire 5055 can heat the extract III and avoid the temperature too low, quick adding mechanism 5 not only can realize the quick joining to extract III, simultaneously can be more dispersed entering into solution III, also can shorten subsequent time of standing greatly.
Example 1:
a method for preparing a slow-release propolis saccule based on natural shellac composite wall materials, which comprises the following steps,
(a) Soaking raw material propolis in ethanol solution with a certain concentration under water bath for first extraction, performing water bath ultrasonic second extraction, and performing water bath third extraction to obtain extract I; the feed liquid ratio of the raw material propolis to the ethanol solution is 1:15; the concentration of the ethanol solution is 85%; the water bath temperature is 45 ℃; the first extraction time is 25min; the second extraction time is 25min; the third extraction time is 1.5h;
(b) Filtering the extract I to obtain a concentrate I; removing water from the concentrate I through a water removing device under vacuum decompression, and adding a proper amount of absolute ethyl alcohol solution for dissolution to obtain an extract II; vacuum decompressing the concentrate I by a water removing device at the temperature of not higher than 50 ℃ to remove water; the added volume of the absolute ethyl alcohol solution is 1.8 times of the mass of the raw material propolis;
(c) Filtering the extract II through a water phase microporous filter membrane to obtain extract III, and freezing and preserving the extract III; dripping the extracting solution II onto a water phase microporous filter membrane by using a needle tube for filtering; the aperture of the water phase microporous filter membrane is 0.5um; the cryopreservation temperature was-20 ℃.
(d) Adding a certain amount of shellac into Na with a certain concentration 2 CO 3 Stirring the solution until the solution is completely dissolved to obtain a solution I; na (Na) 2 CO 3 The concentration of the solution is 0.1mol/mL; shellac and Na 2 CO 3 The feed liquid ratio of the solution is 1/10; the stirring speed is 250r/min; the stirring temperature was 60 ℃.
(e) Adding a certain amount of sodium alginate into a certain amount of water, and stirring until the sodium alginate is completely dissolved to obtain a solution II; the feed liquid ratio of sodium alginate to water is 1:40, a step of performing a; the stirring speed is 250r/min; the stirring temperature was 50 ℃.
(f) Mixing the solution I and the solution II in equal volumes to obtain a solution III;
(g) Rapidly adding the frozen extracting solution III in the step (c) into the solution III in the step (f) according to a specific proportion, standing for a period of time, and then carrying out degassing treatment to obtain extracting solution IV; the ratio of the extract III to the solution III is 1/3.
(h) Slowly dripping the extracting solution IV into CaCl with a certain concentration 2 Crosslinking treatment is carried out in the solution, and after crosslinking is finished, filtering out and drying are carried out, thus obtaining the slow-release propolis saccule; slowly dripping the extracting solution IV into CaCl with a certain concentration by using a needle tube 2 In solution; caCl (CaCl) 2 The concentration of the solution was 1.5mg/mL. The crosslinking time is 30min; the drying temperature is 36 ℃; the drying time was 22h.
And (3) experimental verification:
1. influence of shellac concentration on embedding rate and drug loading rate
As shown in fig. 7 and 8, as the concentration of propolis increases, both the embedding rate and the drug loading rate show a tendency to rise and then fall. When the concentration of the shellac is too low, the strength of the whole gel bead is reduced, so that the bearing effect of the prepared gel bead medicine is weakened, and the embedding rate is too low due to incomplete embedding of the propolis flavone; as the concentration of the shellac increases, the embedding rate and the drug loading rate are gradually increased, and when the concentration of the shellac reaches 1.5g/mL, the embedding rate and the drug loading rate reach optimal values, namely 70.46% and 47.38% respectively; however, when the concentration of shellac is further increased, the embedding rate and the drug loading rate are gradually reduced, because the combination of the excessive shellac and sodium alginate makes the integral structure of the microcapsule more compact, the surface aperture of the gel beads is reduced, more flavone molecules are retained on the surfaces of the gel beads, and the embedding amount is reduced. Thus 1.5g/mL was chosen as the optimum concentration of shellac.
2. Influence of core-wall ratio on embedding rate, drug-loading rate and swelling degree of propolis
As shown in fig. 9 and 10, the effect of the core-wall ratio on the beading of the propolis flavone gel beads was evaluated by using the embedding rate and the drug loading as main indexes, and the embedding rate and the drug loading all showed a continuous trend of increasing with the increase of the core-wall ratio, but the optimal core-wall ratio was 3:6 because the wall material was excessively diluted and could not be encapsulated when the core-wall ratio was greater than 3:6 (g/g). When the core wall ratio is 3: and 6, the embedding rate and the drug loading rate of the microcapsule reach the highest.
As shown in fig. 11 and 12, by accumulating the release rate and the swelling ratio, the release conditions of the propolis flavone in the simulated digestive system are observed, which shows that the time swelling degree of the intestinal simulated digestion for only 2 hours is 26.58 times, the accumulated release rate is nearly complete, the whole digestive juice is pasty, the digestive juice is completely digested, the slow release is not met, and the core-wall ratio is 2.5: the embedding rate and drug loading rate of the group 6 are close to those of the group 3:6, the swelling degree of the group 2h is smaller and is 22.45 times, the whole body of the group 6 is kept in a relatively complete spherical shape after being digested by intestinal juice, the group 6 can be further released, and the requirement of slow release is met. Thus, core wall ratio was chosen to be 2.5:6 (g/g) is most suitable.
3. Influence of embedding time on propolis microencapsulation effect
As shown in fig. 13, 14 and 15, the effect of embedding time on the microencapsulation effect of propolis flavone was judged using the embedding rate, drug loading rate and swelling ratio as main indexes. The embedding rate was relatively high in the range of 20-50 min, while the drug loading was slowly reduced from the embedding time of 10min, but without significant differences (p>0.05). The embedding rate and the drug loading rate are reduced when the embedding time reaches 60 min. The swelling ratio of the group with embedding time of 10min reaches 30.72 times, and the whole sample is gelatinized and is close to complete digestion. This is caused by too short an embedding time, cl in the crosslinking solution - Ions are incompletely combined with sodium alginate, and no perfect structure is formed, so that the ions are rapidly decomposed during digestion. The embedding rate and drug loading rate of the group with the embedding time of 30min are similar to those of other groups, the swelling ratio is the lowest, and the requirement of the propolis microcapsule on slow release in vivo is met. Considering comprehensively, the embedding time is preferably 30 min.
4. Orthogonal optimization experiment
The core-wall ratio and the embedding time in the influencing factors have obvious influence on the embedding rate of the propolis flavone microcapsules, and the concentration of shellac has smaller influence on the embedding rate of the propolis flavone microcapsules. The primary and secondary relationships of the 3 factors are respectively: core-to-wall ratio > embedding time > shellac concentration. The orthogonal results show that the optimal conditions of the wall ratio, the embedding time and the shellac concentration in the orthogonal experiments are 2:6 (g/g), 30min and 1.5g/mL respectively.
The invention can realize that the propolis is used as a core material, the sodium alginate and the shellac are used as composite wall materials, the drug loading rate of the propolis gel beads prepared by adopting a sharp hole-coagulation bath method can reach 68 percent, and the embedding rate can reach 90.46 percent; the gel beads are relatively complete and spherical in whole after in-vitro gastrointestinal digestion, the requirement of slow release of propolis can be met, and meanwhile, main components such as the propolis gel beads are mostly natural components, which is different from the fact that a large amount of solvents such as polyethylene glycol and oil are needed for preparing traditional propolis capsules in the market at present, the potential risks to human health caused by excessive ingestion of polyethylene glycol and oil can be effectively avoided, and a water removal device introduced after concentration can effectively remove water, so that the influence on the subsequent process is reduced, and the quality of finished products is obviously improved.
The above description is only of the preferred embodiments of the present invention; the scope of the invention is not limited in this respect. Any person skilled in the art, within the technical scope of the present disclosure, may apply to the present invention, and the technical solution and the improvement thereof are all covered by the protection scope of the present invention.

Claims (8)

1. A method for preparing a slow-release propolis saccule based on natural shellac composite wall materials is characterized by comprising the following steps: comprises the steps of,
(a) Soaking raw material propolis in ethanol solution with a certain concentration under water bath for first extraction, performing water bath ultrasonic second extraction, and performing water bath third extraction to obtain extract I;
(b) Filtering the extract I to obtain a concentrate I; removing water from the concentrate I through a water removing device under vacuum decompression, and adding a proper amount of absolute ethyl alcohol solution for dissolution to obtain an extract II;
(c) Filtering the extract II through a water phase microporous filter membrane to obtain extract III, and freezing and preserving the extract III;
(d) Adding a certain amount of shellac with the concentration of 1 g/mL-2 g/mL into Na with a certain concentration 2 CO 3 Stirring the solution until the solution is completely dissolved to obtain a solution I;
(e) Adding a certain amount of sodium alginate into a certain amount of water, and stirring until the sodium alginate is completely dissolved to obtain a solution II;
(f) Mixing the solution I and the solution II in equal volumes to obtain a solution III;
(g) Rapidly adding the frozen extracting solution III in the step (c) into the solution III in the step (f) according to a specific proportion, standing for a period of time, and then carrying out degassing treatment to obtain extracting solution IV;
(h) Slowly dripping the extracting solution IV into CaCl with a certain concentration 2 Crosslinking treatment is carried out in the solution, and after crosslinking is finished, filtering out and drying are carried out, thus obtaining the slow-release propolis saccule;
in the step (a), the feed liquid ratio of the raw material propolis to the ethanol solution is 1:10-20; the water bath temperature is 40-50 ℃; the first extraction time is 10 min-40 min; the second extraction time is 20 min-30 min; the third extraction time is 1-2 h;
in the step (b), the concentrate I is subjected to vacuum decompression to remove water through a water removing device under the condition of not higher than 50 ℃; the added volume of the absolute ethyl alcohol solution is 1.6-2 times of the mass of the raw material propolis;
in the step (c), the aperture of the water phase microporous filter membrane is 0.4 um-0.6 um; the freezing preservation temperature is minus 25 ℃ to minus 15 ℃;
in the step (g), the ratio of the extracting solution III to the solution III is 1/3-1/2;
in the step (h), the crosslinking time is 10-60 min; the drying temperature is 35-37 ℃; the drying time is 20-24 hours.
2. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material, which is characterized in that:
in the step (d), shellac and Na 2 CO 3 The feed liquid ratio of the solution is 1/20-1/2; the stirring speed is 200 r/min-300 r/min; stirring temperature is 55-65 ℃;
in the step (e), the feed liquid ratio of sodium alginate to water is 1: 35-45; the stirring speed is 200 r/min-300 r/min; the stirring temperature is 45-55 ℃.
3. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material, which is characterized in that: the water removing device comprises a main body mechanism (1), a gas control mechanism (2), a vibration mechanism (3) and a water removing mechanism (4); the main body mechanism comprises a dewatering bin (101), a main air pipe (102), an auxiliary air pipe (103), a first electromagnetic valve (104), a second electromagnetic valve (105), a porous screen plate (106) and an electromagnet (107); the main air pipe (102) is arranged above the water removal bin (101), the auxiliary air pipe (103) is arranged below the water removal bin (101), the first electromagnetic valve (104) is arranged on the main air pipe (102), the second electromagnetic valve (105) is arranged on the auxiliary air pipe (103), the porous screen plate (106) is arranged inside the water removal bin (101), and the electromagnet (107) is arranged on the upper side of the porous screen plate (106).
4. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material of claim 3, which is characterized in that: the air control mechanism (2) comprises a gas collecting tube (201), an upper expansion fan cover (202), a lower expansion fan cover (203) and a plurality of flow dividing plates (204); the gas collecting tube (201) and the lower expansion hood (203) are respectively and vertically symmetrically connected to the upper end and the lower end of the gas collecting tube (201), and the flow dividing plates (204) are uniformly distributed in the gas collecting tube (201); the gas control mechanism (2) is arranged at the lower side of the porous screen plate (106), and the gas collecting tube (201) is fixedly connected to the lower end of the porous screen plate (106).
5. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material of claim 4, which is characterized in that: the vibration mechanism (3) comprises a vibration plate (301), a vibration motor (302) and a plurality of rebound bags (303); the vibrating plate (301) is connected with the vibrating end of the vibrating motor (302), and the rebound bags (303) are uniformly distributed at the upper end of the vibrating plate (301); the vibrating mechanism (3) is arranged at the lower side of the air control mechanism (2), the vibrating motor (302) is fixedly arranged at the inner bottom end of the dewatering bin (101), and the vibrating plate (301) is arranged at the lower side of the lower expansion hood (203).
6. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material of claim 5, which is characterized in that: the water removing mechanism (4) comprises a plurality of water removing components, the water removing components are arranged on the upper side of the vibrating plate (301), and the water removing components are lifted to be adsorbed on the lower side of the porous screen plate (106) after the electromagnet (107) is started to apply a magnetic field; the water removal assembly comprises a top material particle (401), a limiting hemisphere (402), a transparent hemisphere (403), a water absorption fiber bundle (404), color-changing silica gel particles (405) and magnetic powder (406); the restriction hemisphere (402) and transparent hemisphere (403) symmetrical connection, roof grain (401) are inlayed and are connected on restriction hemisphere (402), allochroic silica gel granule (405) are filled in transparent hemisphere (403), water absorbing fiber bundle (404) are evenly inlayed on roof grain (401), and water absorbing fiber bundle (404) one end extends to roof grain (401) outside, and the other end extends to allochroic silica gel granule (405) inboard, magnetic powder (406) are filled in roof grain (401) inboard.
7. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material, which is characterized in that: in the step (g), the frozen extracting solution III is quickly added into the solution III in the step (f) through a quick adding mechanism (5) according to a specific proportion; the quick adding mechanism (5) comprises a liquid storage tank (501), a pressing column (502), a liquid adding pipe (503), an electromagnet (504) and a liquid injection pipe (505); the liquid filling device is characterized in that the pressing column (502) is slidably mounted on the upper side of the liquid storage tank (501), the liquid filling pipe (503) is fixedly mounted on the side wall of the liquid storage tank (501), the electromagnets (504) are symmetrically mounted at the lower end of the liquid storage tank (501), the liquid filling pipe (505) is uniformly mounted at the lower end of the liquid storage tank (501), the liquid filling pipe (505) is located between the electromagnets (504), and the liquid filling pipe (505) is communicated with the liquid storage tank (501).
8. The method for preparing the sustained-release propolis saccule based on the natural shellac composite wall material, which is characterized in that: the liquid injection pipe (505) comprises a main pipe (5051), a magnetic ring (5052), a bell mouth (5053), a waterproof sleeve (5054) and an electric heating wire (5055); the main pipe (5051), the magnetic ring (5052) and the bell mouth (5053) are sequentially connected from top to bottom, the main pipe (5051) is fixedly connected to the lower end of the liquid storage tank (501) and is communicated with the liquid storage tank (501), the waterproof jacket (5054) is inserted and installed at the center of the main pipe (5051), and the electric heating wire (5055) is installed at the inner side of the waterproof jacket (5054).
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Publication number Priority date Publication date Assignee Title
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CN113662191A (en) * 2021-08-24 2021-11-19 安徽农业大学 Preparation method of lecithin propolis alcohol extract double-wall nano-scale vegetable oil microcapsule
CN114042054A (en) * 2021-12-14 2022-02-15 陈永斌 Method for preparing Chinese herbal medicine extract microcapsule

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