CN113842846A - Preparation method of beta-cyclodextrin/polyvinyl alcohol nano microcapsule - Google Patents
Preparation method of beta-cyclodextrin/polyvinyl alcohol nano microcapsule Download PDFInfo
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- CN113842846A CN113842846A CN202111141557.3A CN202111141557A CN113842846A CN 113842846 A CN113842846 A CN 113842846A CN 202111141557 A CN202111141557 A CN 202111141557A CN 113842846 A CN113842846 A CN 113842846A
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 63
- 229920000858 Cyclodextrin Polymers 0.000 title claims abstract description 41
- 239000001116 FEMA 4028 Substances 0.000 title claims abstract description 41
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 title claims abstract description 41
- 235000011175 beta-cyclodextrine Nutrition 0.000 title claims abstract description 41
- 229960004853 betadex Drugs 0.000 title claims abstract description 41
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 38
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims description 54
- 238000003756 stirring Methods 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 30
- 238000005507 spraying Methods 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 14
- 241000755266 Kathetostoma giganteum Species 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- 239000002775 capsule Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000007590 electrostatic spraying Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 11
- 239000000575 pesticide Substances 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 239000002088 nanocapsule Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- -1 cyclic polysaccharide Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
Abstract
The invention belongs to the technical field of nanotechnology and microcapsules, and particularly relates to a preparation method of beta-cyclodextrin/polyvinyl alcohol nano-microcapsules. The beta-cyclodextrin/polyvinyl alcohol nano microcapsule prepared by the invention has the advantages of nano-scale size, good biocompatibility and biodegradability, no organic solvent is used in the preparation process, the influence on the environment is reduced, and the beta-cyclodextrin/polyvinyl alcohol nano microcapsule has wide application market in the fields of food, medicine, pesticide and the like.
Description
Technical Field
The invention belongs to the technical field of nanotechnology and microcapsules, and particularly relates to a preparation method of a beta-cyclodextrin/polyvinyl alcohol nano microcapsule.
Background
At present, the preparation technology of microcapsules is mature, but most microcapsules prepared by a physical or chemical method stay at the micron level, so that the encapsulated medicine cannot effectively play a role, for example, in the aspect of pesticides, the usage amount of the pesticides in China is as high as more than 200 million tons every year, but the traditional method has the defects of small pesticide action area, easy falling and the like due to the large size of medicine particles, so that a large amount of pesticide residues in soil or water are caused, and the environment is seriously damaged.
Nanotechnology has become the leading subject field of the leading edge of modern science and technology, and is a subject with strong crossability. The nano material can realize special functions which are not possessed by the traditional material by combining with other fields through special properties such as special small-size effect, quantum effect, material localization, surface interface effect and the like. The research field of preparing the nano-grade drug-carrying microcapsule is formed by organically combining the nano technology and the microcapsule preparation technology. The nano microcapsule overcomes some defects of the traditional microcapsule, can effectively improve the embedding rate and the slow release effect of the medicine, enables the medicine to act on a target more efficiently due to the unique small-size effect, and improves the use efficiency of the medicine.
Beta-cyclodextrin is a cyclic polysaccharide, has the advantages of no toxicity, good biocompatibility, capability of preventing the oxidative decomposition of drugs and the like, is easy to dissolve in water, is easy to form stable hydrate, has a truncated cone-shaped structure, regular spatial structure, hydrophobicity in a cavity and hydrophilicity on the outer layer, is easy to form an inclusion compound with polar hydrophobic drug molecules, and is very suitable for preparing drug-loaded microcapsules. At present, research on preparing microcapsules by using beta-cyclodextrin is more, but the size of the prepared microcapsules is basically in the range of several micrometers to dozens of micrometers, so that the utilization rate of a medicament is low, and the preparation also uses organic solvents such as an emulsifier, a dispersing agent and the like, so that the preparation not only influences the characteristics of the microcapsules, but also pollutes the environment.
Disclosure of Invention
The invention aims to overcome the defects of the existing preparation method, and adopts a novel method for preparing the microcapsule, namely a high-voltage electrostatic spraying method for preparing the nano microcapsule, takes nontoxic and environment-friendly water as a solvent, respectively heats and stirs beta-cyclodextrin and polyvinyl alcohol to prepare transparent solutions, uniformly mixes the two solutions according to a certain proportion, puts the transparent solutions into an injector, and applies high voltage to ensure that liquid drops in the solutions form the nano microcapsule. The method avoids the use of organic solvent, adopts degradable biomass material as the capsule wall material, reduces the harm to the environment, meets the requirement of sustainable development, has simple operation and high yield, and has good application prospect.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of beta-cyclodextrin/polyvinyl alcohol nano microcapsules, which comprises the following specific steps:
(1) respectively mixing two capsule wall materials of beta-cyclodextrin and polyvinyl alcohol with water to prepare a wall material solution with a certain mass fraction, stirring and heating to completely dissolve the capsule wall materials, then mixing the two capsule wall material solutions according to a certain proportion, and stirring to uniformly disperse the two capsule wall materials to form a spray solution;
(2) placing the spraying solution obtained in the step (1) into a flat-head needle injector, placing the injector on a high-voltage electrostatic spraying device, connecting a high-voltage live wire at the needle head, grounding at a receiving device, placing a heating device between the needle head and the receiving device, starting spraying after adjusting the injection speed, the receiving distance, the temperature of the heating device and voltage parameters, and obtaining a layer of thick film, namely a nano microcapsule film, on the receiving device after spraying for a period of time;
(3) and (3) grinding the nano microcapsule membrane obtained in the step (2) into powder to obtain nano microcapsule powder, or dissolving the nano microcapsule powder in water to form a nano microcapsule solution.
In the step (1), the mass percentage concentration of the beta-cyclodextrin wall material solution is 2-4%, and the mass percentage concentration of the polyvinyl alcohol wall material solution is 4-5%;
in the step (1), the stirring and heating are carried out by adopting water bath stirring and heating, the temperature of beta-cyclodextrin is 30-50 ℃, the temperature of polyvinyl alcohol is 90-95 ℃, the stirring speed is 200-400 r/min, and the time is 1-1.5 h;
in the step (1), the mass ratio of the beta-cyclodextrin wall material solution to the polyvinyl alcohol wall material solution is 1: 1.5-1: 4;
in the step (1), the stirring speed of the spraying solution is 100-200 r/min;
in the step (2), the size of a needle head of the flat-head needle injector is 23-27G;
in the step (2), the receiving device adopts tinfoil for receiving;
in the step (2), the heating device is heated by an infrared lamp at the temperature of 75-80 ℃;
in the step (2), the injection speed is 2-8 mul/min, the receiving distance is 6-11 cm, and the voltage is 10-15 kv; the spraying time is 2-3 h.
The beta-cyclodextrin/polyvinyl alcohol nano microcapsule prepared by the invention is applied to the fields of food, medicine, environmental protection, pesticide and the like.
The advantages and the characterization effects of the invention are as follows:
(1) the biological nanometer microcapsule membrane provided by the invention has the particle size of 200-700 nm under the observation of a scanning electron microscope, wherein the particle size is mainly distributed between 350-550 nm, the distribution is concentrated, the powder is pure white, the solution dissolved in water is clear and transparent, and the solution is still clear and transparent after being placed for months at room temperature, and the property is stable.
(2) The solvent used in the invention is water, the raw materials are green and environment-friendly and degradable, and no emulsifier or dispersant is used, so that the use of organic solvent is avoided, the environmental pollution is reduced, and the sustainable development requirement is met.
(3) The invention reduces the micro-capsule prepared by beta-cyclodextrin from micro-scale to nano-scale by the novel nano-microcapsule preparation method, which not only improves the effective action area of the microcapsule, but also enhances the adhesion of the microcapsule on a target body.
Drawings
FIG. 1 is SEM image of β -cyclodextrin/PVA nanocapsules of example 1;
FIG. 2 is a distribution diagram of the particle size of the nano-microcapsules obtained by combining the SEM image of the beta-cyclodextrin/polyvinyl alcohol nano-microcapsules of FIG. 1.
Detailed Description
The invention is further illustrated below with reference to specific embodiments and the accompanying drawings.
Example 1
(1) Weighing 0.5g of beta-cyclodextrin and 1.25g of polyvinyl alcohol according to a formula, respectively adding water to the total weight of 20g and 25g, fully stirring by using a magnetic heating stirrer to completely dissolve the beta-cyclodextrin and the polyvinyl alcohol, wherein the temperature for heating the beta-cyclodextrin is 30 ℃, the temperature for heating the polyvinyl alcohol is 90 ℃, the stirring speed is 300r/min, and the stirring and heating time is 1h to obtain a wall material solution;
(2) two wall material solutions were prepared according to the ratio of beta-cyclodextrin: polyvinyl alcohol ═ 3: 7, mixing the mixture into 5g of solution, and fully mixing the solution by using a magnetic stirrer, wherein the stirring speed is 150r/min, and the stirring time is 10min to obtain a spray solution;
(3) sucking enough spraying solution by a flat-head needle injector, placing on a high-voltage electrostatic spraying device, wherein the flat-head needle is 25G in type, a layer of tin foil is laid on a receiving device, a high-voltage live wire and a ground wire are respectively connected with the needle head and the receiving device at the electric connection part, the receiving distance is adjusted to 10cm, the injection rate is 4 mul/min, the voltage is 11.25kv, and the temperature of an infrared heating device is adjusted to 75 ℃. Starting injection, continuously adjusting voltage until the liquid drop at the needle head changes from a spherical shape to a stable conical shape, namely a Taylor cone, continuously spraying vaporous liquid drop to the receiving device, and spraying for 3h to obtain a nano microcapsule film on the tin foil;
(4) the nano microcapsule membrane on the tin foil is slowly torn off and is continuously ground in a mortar to form powder, namely nano microcapsule powder, and the nano microcapsule powder can also be directly dissolved in water to form nano microcapsule solution.
Example 2
(1) Weighing 0.6g of beta-cyclodextrin and 1.25g of polyvinyl alcohol according to a formula, respectively adding water to the total weight of 20g and 25g, fully stirring by using a magnetic heating stirrer to completely dissolve the beta-cyclodextrin and the polyvinyl alcohol, wherein the temperature for heating the beta-cyclodextrin is 40 ℃, the temperature for heating the polyvinyl alcohol is 90 ℃, the stirring speed is 300r/min, and the stirring and heating time is 1h to obtain a wall material solution;
(2) mixing two wall material solutions according to the proportion of beta-cyclodextrin: polyvinyl alcohol ═ 2: 8, mixing the mixture into 5g of solution, and fully mixing the solution by using a magnetic stirrer, wherein the stirring speed is 150r/min, and the stirring time is 10min to obtain a spray solution;
(3) sucking enough spraying solution by a flat-head needle injector, placing on a high-voltage electrostatic spraying device, wherein the flat-head needle is 25G in type, a layer of tin foil is laid on a receiving device, a high-voltage live wire and a ground wire are respectively connected with the needle head and the receiving device at the electric connection part, the receiving distance is adjusted to 11cm, the injection rate is 7 mul/min, the voltage is 13.90kv, and the temperature of an infrared heating device is 75 ℃. Starting injection, continuously adjusting voltage until the liquid drop at the needle head changes from a spherical shape to a stable conical shape, namely a Taylor cone, continuously spraying vaporous liquid drop to the receiving device, and spraying for 3h to obtain a nano microcapsule film on the tin foil;
(4) the nano microcapsule membrane on the tin foil is slowly torn off and is continuously ground in a mortar to form powder, namely nano microcapsule powder, and the nano microcapsule powder can also be directly dissolved in water to form nano microcapsule solution.
Example 3
(1) Weighing 0.6g of beta-cyclodextrin and 1.25g of polyvinyl alcohol according to a formula, respectively adding water to the total weight of 20g and 25g, fully stirring by using a magnetic heating stirrer to completely dissolve the beta-cyclodextrin and the polyvinyl alcohol, wherein the temperature for heating the beta-cyclodextrin is 40 ℃, the temperature for heating the polyvinyl alcohol is 90 ℃, the stirring speed is 300r/min, and the stirring and heating time is 1h to obtain a wall material solution;
(2) mixing two wall material solutions according to the proportion of beta-cyclodextrin: polyvinyl alcohol ═ 3: 7, mixing the mixture into 5g of solution, and fully mixing the solution by using a magnetic stirrer, wherein the stirring speed is 150r/min, and the stirring time is 10min to obtain a spray solution;
(3) sucking enough spraying solution by a flat-head needle injector, placing on a high-voltage electrostatic spraying device, wherein the flat-head needle is 25G in type, a layer of tin foil is laid on a receiving device, a high-voltage live wire and a ground wire are respectively connected with the needle head and the receiving device at the electric connection part, the receiving distance is adjusted to 10cm, the injection rate is 7 mul/min, the voltage is 14.39kv, and the temperature of an infrared heating device is 75 ℃. Starting injection, continuously adjusting voltage until the liquid drop at the needle head changes from a spherical shape to a stable conical shape, namely a Taylor cone, continuously spraying vaporous liquid drop to the receiving device, and spraying for 3h to obtain a nano microcapsule film on the tin foil;
(4) the nano microcapsule membrane on the tin foil is slowly torn off and is continuously ground in a mortar to form powder, namely nano microcapsule powder, and the nano microcapsule powder can also be directly dissolved in water to form nano microcapsule solution.
Example 4
(1) Weighing 0.5g of beta-cyclodextrin and 1.25g of polyvinyl alcohol according to a formula, respectively adding water to the total weight of 20g and 25g, fully stirring by using a magnetic heating stirrer to completely dissolve the beta-cyclodextrin and the polyvinyl alcohol, wherein the temperature for heating the beta-cyclodextrin is 40 ℃, the temperature for heating the polyvinyl alcohol is 90 ℃, the stirring speed is 300r/min, and the stirring and heating time is 1h to obtain a wall material solution;
(2) mixing two wall material solutions according to the proportion of beta-cyclodextrin: polyvinyl alcohol ═ 3: 7, mixing the mixture into 5g of solution, and fully mixing the solution by using a magnetic stirrer, wherein the stirring speed is 150r/min, and the stirring time is 10min to obtain a spray solution;
(3) sucking enough spraying solution by a flat-head needle injector, placing on a high-voltage electrostatic spraying device, wherein the flat-head needle is 25G in type, a layer of tinfoil is laid on a receiving device, a high-voltage live wire and a ground wire are respectively connected with the needle head and the receiving device at the electric connection part, the receiving distance is adjusted to 8cm, the injection rate is 5 mul/min, the voltage is 12.44kv, and the temperature of an infrared heating device is 75 ℃. Starting injection, continuously adjusting voltage until the liquid drop at the needle head changes from a spherical shape to a stable conical shape, namely a Taylor cone, continuously spraying vaporous liquid drop to the receiving device, and spraying for 3h to obtain a nano microcapsule film on the tin foil;
(4) the nano microcapsule membrane on the tin foil is slowly torn off and is continuously ground in a mortar to form powder, namely nano microcapsule powder, and the nano microcapsule powder can also be directly dissolved in water to form nano microcapsule solution.
FIG. 1 is SEM image of β -cyclodextrin/PVA nanocapsules of example 1; FIG. 2 is a distribution diagram of the particle size of the nano-microcapsules obtained by combining the SEM image of the beta-cyclodextrin/polyvinyl alcohol nano-microcapsules of FIG. 1; as can be seen from FIGS. 1 and 2, the particle size is 200-700 nm, wherein the particle size is mainly distributed between 350-550 nm, and the distribution is concentrated.
Claims (9)
1. A preparation method of beta-cyclodextrin/polyvinyl alcohol nano-microcapsules is characterized by comprising the following steps:
(1) respectively mixing two capsule wall materials of beta-cyclodextrin and polyvinyl alcohol with water to prepare a wall material solution with a certain mass fraction, stirring and heating to completely dissolve the capsule wall materials, then mixing the two capsule wall material solutions according to a certain proportion, and stirring to uniformly disperse the two capsule wall materials to form a spray solution;
(2) placing the spraying solution obtained in the step (1) into a flat-head needle injector, placing the injector on a high-voltage electrostatic spraying device, connecting a high-voltage live wire at the needle head, grounding at a receiving device, placing a heating device between the needle head and the receiving device, starting spraying after adjusting the injection speed, the receiving distance, the temperature of the heating device and voltage parameters, and obtaining a layer of thick film, namely a nano microcapsule film, on the receiving device after spraying for a period of time;
(3) and (3) grinding the nano microcapsule membrane obtained in the step (2) into powder to obtain nano microcapsule powder, or dissolving the nano microcapsule powder in water to form a nano microcapsule solution.
2. The preparation method of claim 1, wherein in the step (1), the mass percentage concentration of the beta-cyclodextrin wall material solution is 2-4%, and the mass percentage concentration of the polyvinyl alcohol wall material solution is 4-5%.
3. The preparation method of claim 1, wherein in the step (1), the stirring and heating are performed by water bath stirring and heating, the temperature of the beta-cyclodextrin is 30-50 ℃, the temperature of the polyvinyl alcohol is 90-95 ℃, the stirring speed is 200-400 r/min, and the time is 1-1.5 h.
4. The preparation method of claim 1, wherein in the step (1), the mass ratio of the beta-cyclodextrin wall material solution to the polyvinyl alcohol wall material solution is 1: 1.5-1: 4.
5. the method according to claim 1, wherein the stirring rate of the spray solution in the step (1) is 100 to 200 r/min.
6. The method of claim 1, wherein in step (2), the needle size of the flat-head needle injector is 23-27G.
7. The method according to claim 1, wherein in the step (2), the receiving device receives the molten tin foil.
8. The preparation method according to claim 1, wherein in the step (2), the heating device is heated by an infrared lamp at a temperature of 75-80 ℃.
9. The method according to claim 1, wherein in the step (2), the injection speed is 2 to 8 μ l/min, the receiving distance is 6 to 11cm, and the voltage is 10 to 15 kv; the spraying time is 2-3 h.
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| CN115024339A (en) * | 2022-05-16 | 2022-09-09 | 江苏大学 | Preparation method of plant-source nano pesticide microcapsule |
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