MICROCHANNEL DEVICE, AND HIGH-OIL-LOAD MICROCAPSULE AND METHOD FOR PREPARING THE SAME USING THE MICROCHANNEL DEVICE
20230347348 · 2023-11-02
Inventors
- Yikun LIU (Nanchang, CN)
- Xing CHEN (Nanchang, CN)
- Wei Liu (Nanchang, CN)
- Yuan WANG (Nanchang, CN)
- Liqiang Zou (Nanchang, CN)
Cpc classification
B01J13/203
PERFORMING OPERATIONS; TRANSPORTING
B01L2300/0867
PERFORMING OPERATIONS; TRANSPORTING
B01J13/025
PERFORMING OPERATIONS; TRANSPORTING
B01L2300/1894
PERFORMING OPERATIONS; TRANSPORTING
International classification
B01L3/00
PERFORMING OPERATIONS; TRANSPORTING
B01J13/20
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A microchannel device, including a homogenization chamber, a deceleration-cooling channel, an acidity regulation channel, a microchannel reaction chamber, and an ultrafiltration desalination chamber. A method for preparing high-oil-load microcapsules using the aforementioned microchannel device, including: preparing an aqueous phase and an oil phase; feeding the aqueous phase and the oil phase to the homogenization chamber to form a first emulsion; cooling the first emulsion; adjusting pH of the first emulsion with dilute hydrochloric acid; feeding the first emulsion to the microchannel reaction chamber to form a second emulsion with a core-shell structure; removing Na.sup.+ and Cl.sup.− from the second emulsion; and subjecting the second emulsion to spray drying to obtain the high-oil-load microcapsule powder.
Claims
1. A microchannel device, comprising: a homogenization chamber; and a microchannel reaction chamber; wherein the homogenization chamber comprises an aqueous phase feed pipe, an oil phase feed pipe, a first high-pressure acceleration pipe, a second high-pressure acceleration pipe, and a mixing pipe; an inlet end of the first high-pressure acceleration pipe is connected to the aqueous phase feed pipe, and an outlet end of the first high-pressure acceleration pipe is connected to the mixing pipe; an inlet end of the second high-pressure acceleration pipe is connected to the oil phase feed pipe, and an outlet end of the second high-pressure acceleration pipe is connected to the mixing pipe; an inner diameter of the first high-pressure acceleration pipe is smaller than that of the aqueous phase feed pipe, and an inner diameter of the second high-pressure acceleration pipe is smaller than that of the oil phase feed pipe; and the microchannel reaction chamber comprises at least one reaction flow channel; the at least one reaction flow channel each comprises at least two microchannels communicated in sequence; each of the at least two microchannels comprises an inner tube and an outer tube; and a space between the inner tube and the outer tube is configured for fluid flowing.
2. The microchannel device of claim 1, wherein the first high-pressure acceleration pipe is perpendicularly connected to a sidewall of an outlet end of the aqueous phase feed pipe such that a T-shaped structure is formed by the first high-pressure acceleration pipe and the outlet end of the aqueous phase feed pipe; and the second high-pressure acceleration pipe is perpendicularly connected to a sidewall of an outlet end of the oil phase feed pipe such that a T-shaped structure is formed by the second high-pressure acceleration pipe and the outlet end of the oil phase feed pipe.
3. The microchannel device of claim 2, wherein the aqueous phase feed pipe and the oil phase feed pipe each further comprises an inlet end and a middle section; inlet ends and outlet ends of the aqueous phase feed pipe and the oil phase feed pipe are all arranged along a direction parallel to the mixing pipe; middle sections of the aqueous phase feed pipe and the oil phase feed pipe are both arranged in an outward-inclined manner, such that the aqueous phase feed pipe and the oil phase feed pipe are respectively located at two sides of the mixing pipe, and together form a Y-type structure; and the first high-pressure acceleration pipe and the second high-pressure acceleration pipe are both arranged perpendicular to the mixing pipe.
4. The microchannel device of claim 1, further comprising: a deceleration-cooling channel; a cooling water circulating device; and an acidity regulation channel; wherein the deceleration-cooling channel is arranged between the homogenization chamber and the microchannel reaction chamber; the deceleration-cooling channel is spiral-shaped; an inlet end of the deceleration-cooling channel is connected to the mixing pipe; and an outlet end of the deceleration-cooling channel is connected to the at least one reaction flow channel; the cooling water circulating device is provided with a water inlet and a water outlet; and the deceleration-cooling channel is arranged in the cooling water circulating device; and the acidity regulation channel is arranged between the deceleration-cooling channel and the microchannel reaction chamber; an inlet end of the acidity regulation channel is connected to the deceleration-cooling channel, and an outlet end of the acidity regulation channel is communicated with the microchannel reaction chamber; and a pH detection probe is provided in the acidity regulation channel.
5. The microchannel device of claim 1, further comprising: an ultrafiltration desalination chamber for removing Na.sup.+ and Cl.sup.− from a reaction mixture; wherein the ultrafiltration desalination chamber is connected to an outlet end of the microchannel reaction chamber; and the ultrafiltration desalination chamber comprises a hollow fiber ultrafiltration inner chamber, an inlet, a first outlet for discharge of a filtered reaction mixture, and a second outlet for discharge of a waste liquid, wherein the inlet, the first outlet and the second outlet are connected to the hollow fiber ultrafiltration inner chamber.
6. A method of preparing an oil-loading microcapsule using the microchannel device of claim 1, comprising: (S1) mixing an alcohol-soluble protein and a hydrocolloid followed by dispersion, alkalinity regulation, and centrifugal filtration to obtain an aqueous phase mixture; and preparing an oil phase; (S2) feeding the aqueous phase mixture into the homogenization chamber through the aqueous phase feed pipe, and feeding the oil phase into the homogenization chamber through the oil phase feed pipe; dispersing the aqueous phase mixture through the first high-pressure acceleration pipe, and dispersing the oil phase through the second high-pressure acceleration pipe and mixing the aqueous phase mixture and the oil phase in the mixing pipe to form a first emulsion; (S3) cooling the first emulsion; (S4) adjusting the first emulsion to pH 6.5-7.5 with dilute hydrochloric acid; allowing the first emulsion to flow into the microchannel reaction chamber to undergo dispersion and mixing such that the alcohol-soluble protein in the aqueous phase mixture undergoes interfacial coacervation to embed the oil phase, thereby obtaining a second emulsion with a core-shell structure; (S5) removing Na.sup.+ and Cl.sup.− from the second emulsion; and (S6) drying the second emulsion to obtain the oil-loading microcapsule in a powder form.
7. The method of claim 6, wherein in step (S1), the alcohol-soluble protein is selected from the group consisting of gliadin, zein, kafirin, and a combination thereof; the hydrocolloid is selected from the group consisting of gum arabic, carrageenan, guar gum, maltodextrin, alpha-cyclodextrin, beta-cyclodextrin, octenyl succinic anhydride-modified (OSA)-modified starch, and a combination thereof; the oil phase is selected from the group consisting of camellia oil, linseed oil, peony seed oil, grape seed oil, and a combination thereof; the alkalinity regulation is performed to adjust a mixture of the alcohol-soluble protein and the hydrocolloid to pH 10.5-12; and the centrifugal filtration is performed at 3000-6000 rpm for 5-20 min.
8. The method of claim 6, wherein in step (S3), the first emulsion is cooled through steps of: feeding the first emulsion to a deceleration-cooling channel, and feeding cooling water into a cooling water circulating device, wherein the deceleration-cooling channel is configured as spiral-shaped to cool the first emulsion and reduce a flow rate of the first emulsion; in step (S4), the dilute hydrochloric acid is continuously fed through an acidity regulation channel, and a pH of the first emulsion is monitored and fed back through a pH detection probe; in step (S5), the Na.sup.+ and Cl.sup.− are removed from the second emulsion through steps of: feeding the second emulsion to an ultrafiltration desalination chamber equipped with a hollow fiber ultrafiltration inner chamber such that the second emulsion passes through the hollow fiber ultrafiltration inner chamber to remove the Na.sup.+ and Cl.sup.−; and in step (S6), the drying is performed in a spray dryer.
9. The method of claim 6, wherein an inner diameter of each of the at least two microchannels is 0.4-1 mm; in step (S4), the dilute hydrochloric acid has a concentration of 2 mol/L; and in step (S6), a particle size of the oil-loading microcapsule is 4-40 μm.
10. An oil-loading microcapsule prepared by using the method of claim 6, comprising: a wall material; and a core material; wherein the wall material consists of the aqueous phase mixture; the core material is the oil phase; the wall material is 20-25% by weight of the oil-loading microcapsule; and the core material is 75-80% by weight of the oil-loading microcapsule.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0052] The patent or application file contains at least one drawing executed in color. Copies of this patent or patent application publication with color drawing(s) will be provided by the Office upon request and payment of the necessary fee.
[0053]
[0054]
[0055]
[0056]
[0057] In the drawings, 1, high-pressure homogenization chamber; 11, aqueous phase feed pipe; 12, oil phase feed pipe; 13, first high-pressure acceleration pipe; 14, second high-pressure acceleration pipe; 15, mixing pipe; 2, deceleration-cooling channel; 3, acidity regulation channel; 31, pH detection probe; 4, microchannel reaction chamber; 41, reaction flow channel; 42, microchannel; 5, ultrafiltration desalination chamber; 6, spray dryer; and 7, cooling water circulating device.
DETAILED DESCRIPTION OF EMBODIMENTS
[0058] As shown in
[0059] The high-pressure homogenization chamber 1 includes an aqueous phase feed pipe 11, an oil phase feed pipe 12, a first high-pressure acceleration pipe 13, a second high-pressure acceleration pipe 14, and a mixing pipe 15. An inlet end of the first high-pressure acceleration pipe 13 is connected to the aqueous phase feed pipe 11, and an outlet end of the first high-pressure acceleration pipe 13 is connected to the mixing pipe 15. An inlet end of the second high-pressure acceleration pipe 14 is connected to the oil phase feed pipe 12, and an outlet end of the second high-pressure acceleration pipe 14 is connected to the mixing pipe 15. An inner diameter of the first high-pressure acceleration pipe 13 is smaller than that of the aqueous phase feed pipe 11, and an inner diameter of the second high-pressure acceleration pipe 14 is smaller than that of the oil phase feed pipe 12. Specifically, the first high-pressure acceleration pipe 13 is perpendicularly connected to a sidewall of an outlet end of the aqueous phase feed pipe 11 such that a T-shape structure is formed by the first high-pressure acceleration pipe 13 and the outlet end of the aqueous phase feed pipe 11. The second high-pressure acceleration pipe 14 is vertically connected to a sidewall of an outlet end of the oil phase feed pipe 12 such that a T-shape structure is formed by the second high-pressure acceleration pipe 14 and the outlet end of the oil phase feed pipe 12. As the inner diameter decrease from the feed pipe to the high-pressure acceleration pipe, a high pressure is formed. Besides, the first high-pressure acceleration pipe 13 and the second high-pressure acceleration pipe 14 are arranged perpendicularly on the sidewall of the aqueous phase feed pipe 11 and the sidewall of the oil phase feed pipe 12, respectively, instead of the end of the aqueous phase feed pipe 11 or the oil phase feed pipe 12. In this case, materials are dispersed better, and under the high pressure, the shearing force of the continuous phase liquid will shear off the dispersed phase thereby forming small droplets to form an emulsion. Then the oil and aqueous phases will form an emulsion with stable sizes after passing through the high-pressure homogenization chamber. The aqueous phase feed pipe 11 and the oil phase feed pipe 12 each include an inlet end, a middle section and an outlet end. Inlet ends and the outlet ends of the aqueous phase feed pipe 11 and the oil phase feed pipe 12 are all arranged along the direction parallel to the mixing pipe 15. Middle sections of the aqueous phase feed pipe 11 and the oil phase feed pipe 12 are both arranged in an outward-inclined manner, such that the aqueous phase feed pipe 11 and the oil phase feed pipe 12 are respectively located at two sides of the mixing pipe 15, and together form a Y-type structure. The first high-pressure acceleration pipe 13 and the second high-pressure acceleration pipe 14 are both arranged perpendicular to the mixing pipe 15. The arrangement of Y-shaped feed pipes and the arrangements of the first high-pressure acceleration pipe 13 and the second high-pressure acceleration pipe 14 perpendicular to the mixing pipe 15 facilitate the material dispersion and mixing to form an emulsion.
[0060] The microchannel reaction chamber 4 includes three reaction flow channels 41 parallel to each other. Each reaction flow channel 41 consists of four microchannels 42 connected in sequence. Specifically, each microchannel 42 consists of two pipes having a hexagonal cross-section, and the two pipes have different sizes, where the pipe with a smaller hexagonal cross-section is arranged inside the pipe with a larger hexagonal cross-section, such that the space between the inner pipe and the outer pipe is configured as a channel for flowing of the emulsion. Each reaction flow channel 41 consists of four microchannels 42 connected in sequence. The inner diameter of the microchannel 42 is small, and the emulsion may hit the pipes with hexagonal cross-sections when passing through the corners of the microchannels 42. In this case, the emulsion can be fully dispersed and thus can fully react in the reaction chamber, which is conducive to the occurrence of interfacial cohesion.
[0061] The deceleration cooling channel 2 is spiral-shaped, whose inlet end is connected to the mixing pipe 15 and outlet end is connected to the reaction flow channel 41. The deceleration cooling channel 2 also includes a cooling water circulating device 7. The cooling water circulating device 7 is provided with a water inlet and a water outlet. The deceleration cooling channel 2 is arranged in the cooling water circulating device 7. The emulsion passes through the deceleration cooling channel 2 such that the temperature and flow rate of the emulsion are reduced, and the heat is taken away by the circulating water outside the pipe.
[0062] The acidity regulation channel 3 includes a connection pipe and an acid feed pipe. The deceleration cooling channel 2 and the microchannel reaction chamber 4 are connected by the connection pipe. The acid feed pipe is arranged on the connection pipe, and a pH detection probe is arranged inside the connection pipe for detecting the pH of the emulsion after acidity regulation. By arranging the acidity regulation channel 3, dilute hydrochloric acid can be fed in control. The pH detection probe is configured to detect and feedback the pH of emulsion, and the emulsion is specifically adjusted from pH>10.5 to pH 6.5-7.5. At this point, the proteins, due to self-assembly, undergo interfacial coagulation at the surface of the emulsion to wrap the oil droplets, thus forming a firm core-shell structure.
[0063] The ultrafiltration desalination chamber 5 is connected to the outlet end of the microchannel reaction chamber 4 for removing Na.sup.+ and Cl.sup.− from the reaction material. The ultrafiltration desalination chamber 5 includes a hollow fiber ultrafiltration inner chamber and an inlet, a first outlet and a second outlet, where the inlet, the first outlet and the second outlet are connected to the hollow fiber ultrafiltration inner chamber. The emulsion flows through the entire ultrafiltration pipes under pressure drive and filters Na.sup.+ and Cl.sup.− ions outward through the fibers. After removal of Na.sup.+ and Cl.sup.− ions, the emulsion flows out from the first outlet, and the waste liquid containing Na.sup.+ and Cl.sup.− ions is discharged from the second outlet.
[0064] The spray dryer 6 is connected to the ultrafiltration desalination chamber 5 and is configured for drying the reaction material. The spray dryer includes a primary tower and a secondary tower. The deionized emulsion undergoes spray drying to form stable, highly oil-loaded microcapsules.
[0065] As shown in
[0066] The microchannel device in this embodiment can be used for preparing microcapsules in an efficient, stable, and sustainable way. An aqueous-phase liquid and an oil-phase liquid formulated in advance are directly fed into two pipes of the microchannel device. The two immiscible liquids can form a single emulsion with uniform dispersion and micro size through a pressurized pipe. Then the emulsion flows rapidly in the microchannels and undergoes dispersion, homogenization, and emulsification, shortening the time for preparing oil-in-water emulsions compared with the traditional process. Moreover, the emulsion prepared by using the microchannel device has a high-quality single microdroplet, which provides a technical basis for the preparation of high-quality high-oil-load microcapsules from emulsions.
[0067] The present disclosure will be further described in detail with reference to the following examples, but the present disclosure is not limited thereto.
Example 1
[0068] Provided herein was a method of preparing high-oil-load microcapsules by using the aforementioned microchannel device, which included the following steps.
[0069] (S1) Gluten powder was dissolved in an aqueous solution of pH 11 to obtain a solution with a gliadin concentration of 10% (w/v), which was centrifuged at 5,000 rpm for 10 min. The precipitate was discarded, and the resultant supernatant was added with maltodextrin and α-cyclodextrin, and continuously stirred with a stirrer for 30 min to obtain an aqueous phase mixture (containing protein and polysaccharide) for preparing an emulsion of the microcapsules, where a weight ratio of the gliadin to the maltodextrin was 5:1, and a weight ratio of the gliadin to the α-cyclodextrin was 5:1.
[0070] (S2) Linseed oil was selected as an oil phase, where a weight ratio of the oil phase (core material) to the aqueous phase mixture (wall material) was 4:1 (i.e., an oil load rate of 80%).
[0071] (S3) A 2 mol/L dilute hydrochloric acid solution was prepared for use.
[0072] (S4) The aqueous phase mixture and the oil phase were separately fed into the aforementioned microchannel device to prepare an oil-in-water emulsion with a certain size. The dilute hydrochloric acid was continuously fed into the acidity regulation channel until the emulsion was adjusted to pH 7 such that the interfacial coacervation occurred at the emulsion surface to trigger the formation of a firm core-shell structure.
[0073] (S5) The emulsion with the core-shell structure was desalted in the ultrafiltration-desalination chamber to remove Na.sup.+ and Cl.sup.− ions.
[0074] (S6) The emulsion was fed into the spray dryer for spray drying, during which the inlet air temperature was kept at 175° C., and the emulsion was stirred continuously to obtain the high-oil-load microcapsule powder.
Example 2
[0075] Provided herein was a method of preparing high-oil-load microcapsules by using the aforementioned microchannel device, which included the following steps.
[0076] (S1) Corn gluten meal was dissolved in an aqueous solution of pH 11 to obtain a solution with a zein concentration of 5% (w/v), which was centrifuged at 5,000 rpm for 10 min. The precipitate was discarded, and the resultant supernatant was added with carrageenan and octenyl succinic anhydride-modified (OSA)-modified-starch, and continuously stirred with a stirrer for 30 min to obtain an aqueous phase mixture (containing protein and polysaccharide) for preparing an emulsion of the microcapsules, where a weight ratio of the zein to the carrageenan was 10:1, and a weight ratio of the zein to the OSA-starch was 5:1.
[0077] (S2) Camellia oil was selected as an oil phase, where a weight ratio of the oil phase (core material) to the aqueous phase mixture (wall material) was 4:1 (i.e., an oil load rate of 80%).
[0078] (S3) A 2 mol/L dilute hydrochloric acid solution was prepared for use.
[0079] (S4) The aqueous phase mixture and the oil phase were separately fed into the aforementioned microchannel device to prepare an oil-in-water emulsion with a certain size. The dilute hydrochloric acid was continuously fed into the acidity regulation channel until the emulsion was adjusted to pH 7 such that the interfacial coacervation occurred at the emulsion surface to trigger the formation of a firm core-shell structure.
[0080] (S5) The emulsion with the core-shell structure was desalted in the ultrafiltration-desalination chamber to remove Na.sup.+ and Cl.sup.− ions.
[0081] (S6) The emulsion was fed into the spray dryer for spray drying, during which the inlet air temperature was kept at 175° C., and the emulsion was stirred continuously to obtain the high-oil-load microcapsule powder.
Example 3
[0082] Provided herein was a method of preparing high-oil-load microcapsules by using the aforementioned microchannel device, which included the following steps.
[0083] (S1) Sorghum flour that was defatted and decolored was dissolved in an aqueous solution of pH 11 to obtain a solution with a kafirin concentration of 5% (w/v), which was centrifuged at 5,000 rpm for 15 min. The precipitate was discarded, and the resultant supernatant was added with arabic gum and OSA-starch, and continuously stirred with a stirrer for 30 min to obtain an aqueous phase mixture (containing protein and polysaccharide) for preparing an emulsion of the microcapsules, where a weight ratio of the kafirin to the arabic gum was 10:1, and a weight ratio of the kafirin to the OSA-starch was 5:1.
[0084] (S2) Peony seed oil was selected as an oil phase, where a weight ratio of the oil phase (core material) to the aqueous phase mixture (wall material) was 4:1 (i.e., an oil load rate of 80%).
[0085] (S3) A 2 mol/L dilute hydrochloric acid solution was prepared for use.
[0086] (S4) The aqueous phase and the oil phase were separately fed into the aforementioned microchannel device to prepare an oil-in-water emulsion with a certain size. The dilute hydrochloric acid was continuously fed into the acidity regulation channel until the pH of the emulsion was adjusted to 7 such that the emulsion underwent interfacial polymerization on the surface thereof to form a firm core-shell structure.
[0087] (S5) The emulsion with the core-shell structure was desalted in the ultrafiltration chamber to remove Na.sup.+ and Cl.sup.− ions.
[0088] (S6) The emulsion was fed into the spray dryer with an inlet air temperature of 175° C. for spray drying, during which the emulsion was stirred continuously to obtain the microcapsules with a high oil load.
Example 4
[0089] Provided herein was a method of preparing high-oil-load microcapsules by using the aforementioned microchannel device, which included the following steps.
[0090] (S1) Gluten powder and corn gluten meal were dissolved in an aqueous solution of pH 11 to obtain a solution with a gliadin concentration of 5% and a zein concentration of 5%, which was centrifuged at 5,000 rpm for 10 min. The precipitate was discarded, and the resultant supernatant was added with guar gum, and continuously stirred with a stirrer for 30 min to obtain an aqueous phase mixture (containing protein and polysaccharide), where a weight ratio of the total protein to the guar gum was 12:1.
[0091] (S2) Grape seed oil was selected as an oil phase, where the weight ratio of the oil phase (core material) to the aqueous phase mixture (wall material) was 4:1 (i.e., an oil load rate of 80%).
[0092] (S3) A 2 mol/L dilute hydrochloric acid solution was prepared for use.
[0093] (S4) The aqueous phase mixture and the oil phase were separately fed into the aforementioned microchannel device to prepare an oil-in-water emulsion with a certain size. The dilute hydrochloric acid was continuously fed into the acidity regulation channel until the emulsion was adjusted to pH 7 such that the interfacial coacervation occurred at the emulsion surface to trigger the formation of a firm core-shell structure.
[0094] (S5) The emulsion with the core-shell structure was desalted in the ultrafiltration-desalination chamber to remove Na.sup.+ and Cl.sup.− ions.
[0095] (S6) The emulsion was fed into the spray dryer for spray drying, during which the inlet air temperature was kept at 175° C., and the emulsion was stirred continuously to obtain the high-oil-load microcapsule powder.
Comparative Example 1
[0096] Provided herein was a method of preparing microcapsules, which included the following steps.
[0097] (S1) Gluten powder was dissolved in distilled water and centrifuged at 5,000 rpm for 10 min.
[0098] It was found that the gluten powder was almost insoluble in water, and mainly existed as precipitates after centrifugation. Hence, it was impossible to perform the subsequent processes.
Comparative Example 2
[0099] Provided herein was a method of preparing microcapsules by using a dispersion device, which included the following steps.
[0100] (S1) Gluten powder was dissolved in an aqueous solution of pH 11 to obtain a solution with a gliadin concentration of 10% (w/v), which was centrifuged at 5,000 rpm for 10 min. The precipitate was discarded, and the resultant supernatant was added with carrageenan and α-cyclodextrin, and continuously stirred with a stirrer for 30 min to obtain an aqueous phase mixture (containing protein and polysaccharide), where a weight ratio of the gliadin to the carrageenan was 10:1, and a weight ratio of the gliadin to the α-cyclodextrin was 5:1.
[0101] (S2) Grape seed oil was selected as an oil phase, where a weight ratio of the oil phase (core material) to the aqueous phase mixture (wall material) was 4:1 (i.e., an oil load rate of 80%).
[0102] (S3) A 2 mol/L dilute hydrochloric acid solution was prepared for use.
[0103] (S4) The aqueous phase mixture and the oil phase were fed into the dispersion device at 12,000 rpm for 2 min to prepare an emulsion.
[0104] (S5) The 2 mol/L dilute hydrochloric acid was dropwise fed into the emulsion until the emulsion was adjusted to pH 7, during which the emulsion was stirred with a stirrer.
[0105] (S6) The emulsion was fed into the spray dryer for spray drying, during which the inlet air temperature was kept at 175° C., and the emulsion was stirred continuously to obtain the high-oil-load microcapsule powder.
Experimental Results
[0106] The microcapsules prepared in Examples 1-4 and Comparative Example 2 were observed under scanning electron microscopy and were tested regarding their oil loads and encapsulation rates as follows.
[0107] (1) Determination of Encapsulation Rate
[0108] The encapsulation rate (%) of the microcapsule was calculated by [(total oil content−surface oil content)/total oil content]×100%.
[0109] The surface oil content of the microcapsule was determined through the following steps.
[0110] To a triangular flask with a constant weight of m.sub.1 were added 2 g of a sample (accurate to 0.001 g) and 15 mL of petroleum ether for extraction for 10 min, during which the triangular flask was shaken at intervals. After that, the sample was filtered with filter paper. After extraction 3 times, the triangular flask and the filter paper were rinsed with 10 mL of petroleum ether. The filtrates were gathered in a dried and weighed evaporation flask and subjected to vacuum spin dry at 30° C. Then the evaporation flask was cooled and weighed as m.sub.2.
[0111] (2) Determination of Oil Load
[0112] The surface oil content (%) was calculated by (m.sub.2−m.sub.1)/m×100%, where m was the weight of the sample.
[0113] The total oil content of the microcapsule was determined through the following steps.
[0114] 1 g of microcapsule powder was weighed and dispersed in 25 ml of a mixture, and stirred at 800 rpm for 15 min, followed by centrifugation at 8000 rpm for 2 min, where the mixture consisted of hexane and isopropanol in a volume ratio of 3:1. After that, the clear upper phase was collected and the lower aqueous phase was re-extracted with an equal amount of solvent. The two organic phases were gathered and were subjected to rotary evaporation drying at 105° C. for 2 h to remove excess solvent.
[0115] The SEM images of the microcapsules prepared in Examples 1-4 and Comparative Example 2 were shown in
[0116] The test results of the oil loads and the encapsulation rates were shown in
[0117] Described above are merely preferred embodiments of the present disclosure, which are not intended to limit the disclosure. Any equivalent substitutions, changes and modifications made by those skilled in the art without departing from the spirit of the disclosure shall fall within the scope of the present disclosure defined by the appended claims.