CN112871100A - Multi-spraying device and method for continuously preparing microcapsules - Google Patents
Multi-spraying device and method for continuously preparing microcapsules Download PDFInfo
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- CN112871100A CN112871100A CN202110231018.2A CN202110231018A CN112871100A CN 112871100 A CN112871100 A CN 112871100A CN 202110231018 A CN202110231018 A CN 202110231018A CN 112871100 A CN112871100 A CN 112871100A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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Abstract
The invention discloses a multi-spraying device, which comprises the following components: a spray can (G); a plurality of nozzles (P) disposed at an upper portion of an inner wall of the spray can (G); each nozzle is respectively externally connected with a spray pipe (T); a plurality of paddles (M), wherein at least one paddle is disposed at an upper portion or a lower portion of the plurality of nozzles, wherein at least one paddle is disposed at a lower portion of the spray can (G). The invention also discloses a method for continuously preparing microcapsules by using the multi-spraying device. The device of the invention can be used for continuously preparing the microcapsules, and the encapsulation efficiency of the obtained microcapsules is obviously improved.
Description
Technical Field
The invention belongs to the technical field of spice preparation, and particularly relates to a multi-spraying device and a method for continuously preparing microcapsules.
Background
The microcapsule takes natural or synthetic or semi-synthetic polymer material as a capsule wall, and an embedding object is wrapped in the capsule wall to form a shell-core structure. The substances embedded in the polymer carrier can be slowly released, and the utilization rate, action time and stability of the effective components are improved.
The volatile fragrant substance has the characteristics of strong volatility and easy oxidative deterioration, the microcapsule can effectively protect the stability of fragrant molecules, and the fragrant substance can be diffused to the surface of the capsule from the inside of the capsule through the micropores of the capsule wall at different release rates by regulating and controlling the temperature, the material of the capsule wall and the size of the micropores on the capsule wall, so that the fragrant component is released.
The flavor substance microcapsule is mostly prepared by a physical method, and mainly comprises a complex coacervation method, a single coacervation method, a spray drying method and the like. The complex coacervation method comprises the steps of taking two or more polymer materials as wall materials, dispersing the fragrance substance into the wall materials, and carrying out electrostatic interaction on the wall materials to reduce the solubility of the wall materials under the conditions of changing a fixed temperature, a pH value or inorganic salt and the like, so that the wall materials are coacervated and wrapped to form microcapsules; the operation is carried out at normal temperature, and the inclusion rate and the yield are higher. Preparing mixed emulsion of a fragrant substance and a wall material by a spray drying method, then carrying out spray drying on the emulsion in a dryer, forming a reticular structure after the wall material is heated, and wrapping the fragrant substance in meshes to form a microcapsule; when heated, the fragrant substances are released through the meshes due to the thermal movement of molecules; spray drying is generally carried out at 100-300 ℃ and is suitable for inclusion of core materials with stable properties, but not necessarily for flavor substances with strong volatility. The single coacervation method is that volatile fragrant substances are dispersed in a polymer wall material to prepare emulsion, uniform emulsion is prepared under the condition of high-speed dispersion, the pH value is adjusted, ionized salt is added to reduce the solubility of the polymer material and maintain the high salinity of the encapsulated substance, and the fragrant substances are encapsulated into microcapsules after coacervation; the single coacervation method adopts a single wall material, has high inclusion rate, is operated at normal temperature, is simple and convenient to operate, and is suitable for wrapping of fragrant substances and expanded production of the process. The prior relevant documents for preparing the microcapsule by a single coacervation method report that: the Liujun and the like adopt a single coacervation method to prepare and optimize a process scheme in the preparation and release performance research of the mosquito repellent fabric loaded with the citronella oil microspheres, and when the concentration of gelatin is 2%, the yield, the encapsulation rate, the oil loading amount and the release rate of the gelatin citronella oil microspheres all reach higher values; the release rate of the citronella oil is related to the particle size of the microspheres, and the smaller the particle size of the microspheres is, the larger the release area of the coated substance is, and the higher the release rate is.
The microcapsules prepared by the complex coacervation method, the single coacervation method, the spray drying method and other preparation methods can maintain the stability of the fragrance molecules and can stably release fragrance components at a certain temperature. The preparation method is simple and convenient and is easy for industrial production. However, the above preparation methods are all intermittent operations, and have poor controllability, and the continuous preparation of the microcapsules cannot be carried out; and the prepared microcapsule has low encapsulation efficiency.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention discloses a multi-spraying device and a method for continuously preparing microcapsules by using the multi-spraying device. The multi-spraying device can be used for continuously preparing the microcapsules, and the encapsulation efficiency of the obtained microcapsules is obviously improved. The device of the invention is simple and easy to operate, and is easy for industrial production.
The technical scheme of the invention is as follows:
the invention discloses a multi-spraying device in a first aspect, which comprises the following components:
a spray can G;
a plurality of nozzles P arranged on an upper portion of an inner wall of the spray can G; each nozzle is respectively externally connected with a spray pipe T;
a plurality of paddles M, at least one of which is disposed at an upper portion or a lower portion of the plurality of nozzles, at least one of which is disposed at a lower portion of the spray can G.
Preferably, the nozzles are arranged in an even number in the same horizontal plane, two of which are opposite to each other.
Preferably, the number of the plurality of paddles is 2, wherein the paddles disposed at the upper or lower portion of the plurality of nozzles are first paddles M1, and the paddles disposed at the lower portion of the spray can G are second paddles M2.
Preferably, the first stirring paddle M1 and the second stirring paddle M2 are a common stirring shaft M, and a driving device D is connected to the stirring shaft M.
Preferably, the middle part of the spraying tank G is provided with a feed inlet J, and the bottom of the spraying tank G is provided with a discharge outlet C.
In a second aspect of the invention, a method for continuously preparing microcapsules by using the multi-spraying device is disclosed, which comprises the following steps:
firstly, preparing an emulsion containing fragrant substances and wall materials, and connecting the emulsion with a nozzle through a spray pipe;
preparing two parts of salt solution, wherein one part has higher concentration and the other part has lower concentration; connecting the salt solution with larger concentration with a nozzle through a spray pipe; wherein the nozzle connecting the salt solution with larger concentration is opposite to the nozzle connecting the emulsion;
thirdly, injecting the salt solution with small concentration prepared in the second step into a spraying tank G through a feed inlet J;
starting the driving device D to start the stirring paddle M, starting the nozzle P, and regulating and controlling the size of liquid drops to spray;
fully mixing the solution at the bottom of the spray tank G, and discharging the mixed solution into an intermediate storage tank through a discharge port C;
sixthly, continuously mixing the materials in the middle storage tank;
and filtering, freezing and drying to obtain the microcapsule.
Preferably, the fragrant substance in the step (i) is one or more of peppermint oil, perilla oil or citronella oil; the wall material is gelatin.
Preferably, the salt solution in the step (II) is one or more of sodium sulfate, potassium sulfate, sodium chloride or potassium chloride salt solution; the concentration of the salt solution with larger concentration is 20-40 wt%; the concentration of the salt solution with smaller concentration is 10-15 wt%.
Preferably, the rotation speed of the stirring paddle M in the step (iv) is 500-.
The method for continuously preparing the microcapsules by using the multi-spraying device of the invention comprises the following specific steps, taking the wall material as gelatin and the fragrant substance as peppermint oil as an example:
dissolving a proper amount of gelatin in distilled water at 40-70 ℃ to prepare a gelatin solution with the concentration of 1-10 wt%; adding appropriate amount of oleum Menthae Dementholatum, controlling the mass ratio of oleum Menthae Dementholatum to gelatin at 1:1-1:4, adjusting pH to 3.5-3.8 with acetic acid, emulsifying at 13000 and 18000rpm for 2-3min, and performing ultrasonic treatment for 3-5min to obtain oleum Menthae Dementholatum gelatin emulsion; wherein the frequency of the ultrasonic wave is 20-30kHz, and the power is 200-250W;
dissolving one or more of anhydrous sodium sulfate, potassium sulfate, sodium chloride or potassium chloride in water to prepare a concentrated salt solution with the concentration of 20-40 wt% and a dilute salt solution with the concentration of 10-15 wt%, and respectively adjusting the pH value of acetic acid to 3.5-3.8 for later use;
step three, injecting the dilute salt solution with the concentration of 10-15 wt% prepared in the step two into a spraying tank G through a feed port J;
step four, the driving device D is started, and the first stirring paddle M1 and the second stirring paddle M2 are respectively stirred at the rotating speed of 500-1000 rpm; opening a nozzle for spraying;
step five, spraying the peppermint oil gelatin emulsion obtained in the step one and the concentrated salt solution obtained in the step two into the spraying tank G through a first nozzle P1 and a second nozzle P2 respectively, wherein the diameter of the sprayed fog drops is 300-1000 mu m; the two nozzles are arranged at the horizontal opposite positions of the inner wall of the spraying tank G, as shown in figure 1, the sprayed droplets are collided and mixed with each other, the two droplets are fully mixed under the action of a first stirring paddle M1, gelatin is condensed under the action of a concentrated salt solution, the mint oil is wrapped in the concentrated salt solution to form microcapsules, and the microcapsules are settled or flow downstream to the bottom of the spraying tank G in figure 1 along the inner wall of the spraying tank G under the action of gravity and the inertia force of the first stirring paddle M1; simultaneously, the second stirring paddle M2 fully mixes the liquid drops with the dilute salt solution at the rotating speed of 500-1000rpm, and continuously stirs for 5-15 min;
step six, discharging the liquid substances in the step five through a discharge port C, placing the liquid substances in an intermediate storage device, continuously stirring at the speed of 500 plus 1000rpm, and cooling to 0-10 ℃; continuously stirring, slowly dripping 10-15M formaldehyde solution, slowly dripping 15-25 wt% sodium hydroxide solution, adjusting pH to 8-9, keeping temperature at 0-10 deg.C, and continuously stirring for 2-5 h. The formaldehyde is added to solidify the microcapsule, and the reaction mechanism is that under the alkaline condition, the formaldehyde reacts with NH in the gelatin2The reaction is an irreversible chemical reaction, and a solidified colloid is formed after the reaction, so that the depolymerization of the gelatin is avoided.
Step seven, filtering, washing the filter cake with water until the filtrate can not change the hydroxylamine phosphate solution from light yellow to pink, and freeze-drying to obtain a finished product, namely the microcapsule; the obtained microcapsule has particle diameter of 10-50 μm. If the microcapsules retain formaldehyde, the hydroxylamine phosphate solution is pink, and if there is no residue, the solution is pale yellow.
The invention has the beneficial effects that:
1. the multi-spraying device is provided with a plurality of nozzles for the first time, and the number and the relative positions of the plurality of nozzles can be set according to the properties of the emulsion and the salt solution, so that sprayed emulsion droplets and sprayed salt solution droplets are fully mixed.
2. The multi-spraying device is provided with at least two stirring paddles, wherein at least one stirring paddle is used for mixing fog drops, and further mixing of the sprayed emulsion fog drops and strong salt solution fog drops is guaranteed.
3. The encapsulation efficiency of the microcapsule perfume prepared by the multi-spraying device is obviously improved.
4. The multi-spraying device can continuously prepare the microcapsules, and has strong controllability and improved production efficiency compared with the batch operation in the prior art.
Drawings
Fig. 1 is a schematic view of a multi-spray apparatus of example 1.
Fig. 2 is a top view of the multi-spray apparatus of example 2.
Fig. 3 is an SEM image of gelatin peppermint oil microcapsules prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to the examples.
Example 1
The schematic diagram of the multi-spraying device used in this example is shown in fig. 1. The device comprises the following components: the bottom of the spray can G is provided with a discharge hole C, and the two nozzles are respectively a first nozzle P1 and a second nozzle P2 which are oppositely arranged on the same horizontal plane; the lower part of the nozzle P is provided with a feed inlet J; two stirring rakes, wherein arrange the stirring rake of nozzle lower part is first stirring rake M1, arranges the stirring rake of lower part is second stirring rake M2 in the spraying jar G, and two stirring rakes are total (mixing) shaft M, even there is drive arrangement D on the (mixing) shaft M.
The procedure for preparing gelatin peppermint oil microcapsules using the multi-spray apparatus of this example was as follows:
dissolving a proper amount of gelatin in distilled water at 50 ℃ to prepare a gelatin solution with the concentration of 5 wt%; adding oleum Menthae Dementholatum, controlling the mass ratio of oleum Menthae Dementholatum to gelatin at 1:2, adjusting pH to 3.8 with acetic acid, emulsifying at 13000rpm for 2min, and performing ultrasonic treatment for 3min to obtain oleum Menthae Dementholatum gelatin emulsion; wherein the frequency of the ultrasonic wave is 20kHz, and the power is 200W.
Dissolving a proper amount of anhydrous sodium sulfate in water, controlling the concentration to be 40 wt%, and adjusting the pH value to be 3.8 by using acetic acid to prepare a concentrated anhydrous sodium sulfate solution; dissolving a proper amount of anhydrous sodium sulfate in water, controlling the concentration to be 10 wt%, and adjusting the pH value to be 3.8 by acetic acid to prepare a dilute anhydrous sodium sulfate solution.
A10 wt% dilute anhydrous sodium sulfate solution was injected into spray tank G through feed port J.
The driving device D is started, and the first stirring paddle M1 and the second stirring paddle M2 are respectively stirred at the rotating speed of 800 rpm; the spray nozzle is opened for spraying and the two nozzles are arranged in the horizontal opposite positions in the spray can G as shown in fig. 1.
Spraying the prepared gelatin emulsion into the spraying tank G through a first nozzle P1, spraying a concentrated anhydrous sodium sulfate solution into the spraying tank G through a second nozzle P2, enabling sprayed droplets to collide with each other and mix, then fully mixing under the action of a first stirring paddle M1, settling the droplets or enabling the droplets to flow downstream along the inner wall of the spraying tank G into a dilute anhydrous sodium sulfate solution at the bottom of the spraying tank G under the action of gravity or inertia force of the stirring paddle, simultaneously fully mixing the above liquids through a second stirring paddle M2, and continuously stirring for 10 min;
discharging the liquid into an intermediate storage device (not shown in the attached drawing) through a discharge port C, continuously stirring at the speed of 800rpm, cooling to 5 ℃, continuously stirring, slowly dropwise adding 12M formaldehyde solution, then slowly dropwise adding 20 wt% sodium hydroxide solution, adjusting the pH value to 8.5, keeping the temperature at 5 ℃ unchanged, and continuously stirring for 2 hours.
Filtering, washing the filter cake with water until the filtrate can not change the color of the hydroxylamine phosphate solution from light yellow to pink, and freeze-drying to obtain the final product gelatin peppermint oil microcapsule, wherein the SEM picture is shown in figure 3, and the particle size is 40-50 microns. The encapsulation efficiency was tested to be 80.4%.
Comparative example:
the preparation method is consistent with the conventional single agglomeration reported in the literature. The preparation methods of 40 wt% and 10 wt% anhydrous sodium sulfate solution, peppermint oil gelatin emulsion, formaldehyde and sodium hydroxide solution, etc. were the same as in example 1.
The method comprises the following steps: putting appropriate amount of oleum Menthae Dementholatum gelatin emulsion in beaker, adding appropriate amount of acetic acid solution to adjust pH to 3.8, slowly dropwise adding appropriate amount of 40 wt% anhydrous sodium sulfate solution, stirring for 5min, adding appropriate amount of 10 wt% anhydrous sodium sulfate solution, and stirring for 5 min. Cooling to 5 ℃, continuously stirring, slowly dripping 12M formaldehyde solution, then slowly dripping 20 wt% sodium hydroxide solution, adjusting the pH value to 8.5, keeping the temperature at 5 ℃, and continuously stirring for 2 hours. Filtering, washing the filter cake with water until the filtrate can not change the color of the hydroxylamine phosphate solution from light yellow to pink, and freeze-drying to obtain the final product gelatin peppermint oil microcapsule with the particle size of 10-80 microns. The encapsulation efficiency was tested to be 71.9%.
Example 2
The multi-spraying device used in the embodiment is the same as that in embodiment 1, except that four nozzles are arranged in the spraying tank G, all the nozzles are arranged in a horizontal plane, the plane is parallel to the bottom of the spraying tank G, as shown in the top view of fig. 2, droplets sprayed from the four nozzles collide with each other and are mixed, and then are further mixed under the action of the first stirring paddle M1, and the droplets settle or flow downstream to the bottom of the spraying tank G along the inner wall of the spraying tank G under the action of gravity or the blade inertia force of the stirring paddle to be mixed with the dilute anhydrous sodium sulfate solution. The rest is the same as example 1. The particle size of the gelatin peppermint oil microcapsule is 40-50 microns and the encapsulation rate is 82.5 percent.
Example 3
The multi-spray device used in this example was the same as in example 1. The components and concentrations of the raw materials were the same as in example 1, except that: the spice is perilla oil. The encapsulation rate of the obtained finished product of gelatin perilla oil microcapsule is 80.8 percent.
Example 4
The multi-spray device used in this example was the same as in example 2. The ingredients and concentrations of the raw materials were the same as in example 2, except that: the perfume is citronella oil. The encapsulation rate of the obtained gelatin citronella oil microcapsule is 82.7%.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A multiple spray device, comprising:
a spray can (G);
a plurality of nozzles (P) disposed at an upper portion of an inner wall of the spray can (G); each nozzle is respectively externally connected with a spray pipe (T);
a plurality of paddles (M), wherein at least one paddle is disposed at an upper portion or a lower portion of the plurality of nozzles, wherein at least one paddle is disposed at a lower portion of the spray can (G).
2. A multi-spray apparatus according to claim 1 wherein an even number of said nozzles are arranged in a common horizontal plane, two of which are opposed.
3. The multi-spray apparatus according to claim 1, wherein the plurality of paddles is 2, wherein the paddles disposed at the upper or lower portion of the plurality of nozzles are first paddles (M1), and the paddles disposed at the lower portion of the spray tank (G) are second paddles (M2).
4. Multi-spray device according to claim 4, characterised in that the first and second paddles (M1, M2) are a common stirring shaft (M) to which a drive (D) is connected.
5. A multi-spray device according to claim 1, characterized in that the spray tank (G) has a feed inlet (J) in the middle and a discharge outlet (C) in the bottom.
6. A process for the continuous production of microcapsules using a multi-spray device according to claims 1-6, characterized in that it comprises the following steps:
firstly, preparing an emulsion containing fragrant substances and wall materials, and connecting the emulsion with a nozzle through a spray pipe;
preparing two parts of salt solution, wherein one part has higher concentration and the other part has lower concentration; connecting the salt solution with larger concentration with a nozzle through a spray pipe; wherein the nozzle connecting the salt solution with larger concentration is opposite to the nozzle connecting the emulsion;
thirdly, the salt solution with small concentration prepared in the second step is injected into the spraying tank (G) through the feed port (J);
starting the driving device (D), starting the stirring paddle (M), starting the nozzle (P), and regulating and controlling the size of liquid drops to spray;
fully mixing the solution at the bottom of the spray tank (G) and discharging the mixed solution into an intermediate storage tank through a discharge hole (C);
sixthly, continuously mixing the materials in the middle storage tank;
and filtering, freezing and drying to obtain the microcapsule.
7. The preparation method according to claim 6, wherein the fragrant substance of step (r) is one or more of peppermint oil, perilla oil or citronella oil; the wall material is gelatin.
8. The preparation method according to claim 6, wherein the salt solution of step (II) is one or more of sodium sulfate, potassium sulfate, sodium chloride or potassium chloride salt solution; the concentration of the salt solution with larger concentration is 20-40 wt%; the concentration of the salt solution with smaller concentration is 10-15 wt%.
9. The preparation method according to claim 6, wherein the rotation speed of the stirring paddle (M) in the step (r) is 500-1000rpm respectively.
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| CN202110231018.2A CN112871100A (en) | 2021-03-02 | 2021-03-02 | Multi-spraying device and method for continuously preparing microcapsules |
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| CN202110231018.2A CN112871100A (en) | 2021-03-02 | 2021-03-02 | Multi-spraying device and method for continuously preparing microcapsules |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115191611A (en) * | 2022-07-15 | 2022-10-18 | 江西中科农牧动物保健品有限公司 | Enteric-coated probiotic preparation and preparation method thereof |
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2021
- 2021-03-02 CN CN202110231018.2A patent/CN112871100A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115191611A (en) * | 2022-07-15 | 2022-10-18 | 江西中科农牧动物保健品有限公司 | Enteric-coated probiotic preparation and preparation method thereof |
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