CN115104605B - Compound natural plant extract synergistic antibacterial antiviral multishell microcapsule and preparation method and application thereof - Google Patents
Compound natural plant extract synergistic antibacterial antiviral multishell microcapsule and preparation method and application thereof Download PDFInfo
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- 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
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- A01N65/08—Magnoliopsida [dicotyledons]
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- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
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- A01N65/44—Poaceae or Gramineae [Grass family], e.g. bamboo, lemon grass or citronella grass
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- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
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Abstract
The invention belongs to the technical field of preparation of functional slow-release microcapsules, and particularly relates to a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, and a preparation method and application thereof. The multi-shell microcapsule provided by the invention comprises mesoporous SiO 2 A nanoparticle inner shell; is loaded on the mesoporous SiO 2 The compound natural plant extract in the inner shell mesopores of the nano-particles comprises tea extract, bamboo leaf extract, cedar extract and herba Andrographitis extract; coating the mesoporous SiO 2 The chemical composition of the middle shell on the inner shell surface of the nanoparticle comprises gelatin, acacia and a silane coupling agent; and the shell is coated on the surface of the middle shell, and the chemical composition of the shell comprises polyethyleneimine and octenyl succinic acid esterified starch. The invention adoptsThe synergistic effect of multiple shells ensures that the compound natural plant extract maintains antibacterial and antiviral properties in a hot-pressing environment, and realizes lasting antibacterial and antiviral effects through stable slow release.
Description
Technical Field
The invention belongs to the technical field of preparation of functional slow-release microcapsules, and particularly relates to a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, and a preparation method and application thereof.
Background
Bacteria, viruses and the like enter the room along with dust, air and spray, so that the risk of infection is caused. Therefore, daily necessities closely related to the life of people can become diffusion carriers of bacteria, viruses and the like, and a safe and environment-friendly antibacterial and antiviral house environment is established, and the daily necessities comprise: the surfaces of floors, furniture, wallpaper, retaining walls and the like form an antibacterial and antiviral protective layer, so that bacterial and viral infection can be effectively prevented.
At present, most common antibacterial or antiviral plates are prepared by coating inorganic antibacterial auxiliary agents on the surfaces, and utilizing oxidation-reduction reaction of inorganic ions to destroy or change organic matters of bacteria or viruses so as to achieve the effects of resisting bacteria and inactivating viruses. However, the inorganic antibacterial auxiliary agent has large addition amount, is sensitive to environment and pH value, is easy to trigger photocatalysis and influence the substrate material of the plate, and is easy to wear and lose efficacy after long-term use, thus being easy to cause heavy metal enrichment in human body and damaging the health of the human body. Also, the antibacterial and antiviral effects are generally not compatible.
The extracts of flowers, leaves, stems, roots, wood, bark, seeds or fruits of natural plants have various active ingredients including terpenes, polyphenols, flavonoids, fatty acids and the like, have remarkable antiviral, antibacterial and bactericidal effects, and are widely applied to the fields of medicine, sanitation, agriculture, daily chemicals and the like. However, single plant extract has poor broad-spectrum antibacterial and antiviral effects, and Chinese patent CN 113861739A discloses an antibacterial and antiviral water-based paint containing mugwort, a preparation method and application thereof. The patent adopts AB component for compounding to form synergistic antibacterial and antiviral effects, wherein A component adopts Chinese mugwort, eucalyptus and saffron plant extracts, B component adopts nano silver ion particles and Aikang powder inorganic powder, and has broad-spectrum antibacterial and antiviral effects, but heavy metals and non-environment-friendly components. Meanwhile, the traditional natural plant extract has mild use environment and weak durability, and the artificial board production process needs a certain high-pressure, high-temperature and acid-base environment, so that the conventional emulsion or glassy microcapsule wall material collapses, and the antiviral essential oil is volatilized or dissociated instantaneously, so that the lasting antiviral and antibacterial effects are difficult to achieve.
Chinese patent CN 112176451A discloses an antibacterial and antiviral cellulose fiber and a preparation method thereof, wherein a double-layer wall microcapsule structure is adopted, a beta-cyclodextrin component is adopted in an inner layer wall microcapsule, porous starch is adopted in an outer layer wall microcapsule, and the design can effectively avoid the loss of entrapped substances, but the double-layer wall has the defects of pressure resistance and high temperature resistance.
Disclosure of Invention
The invention aims to provide a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, which comprises mesoporous SiO 2 A nanoparticle inner shell;
is loaded on the mesoporous SiO 2 The compound natural plant extract in the inner shell mesopores of the nano particles comprises tea extract, bamboo leaf extract, cedar extract and andrographis paniculata extract;
coating the mesoporous SiO 2 A middle shell on the inner shell surface of the nanoparticle, wherein the chemical composition of the middle shell comprises gelatin, acacia and a silane coupling agent;
and the chemical composition of the shell comprises polyethyleneimine and octenyl succinic acid esterified starch.
Preferably, the mass ratio of the tea extract to the bamboo leaf extract to the cedar wood extract to the common andrographis herb extract is (2-3)/(3-5)/(1-2).
Preferably, the compound natural plant extract and mesoporous SiO 2 The mass ratio of the nano particles is (2-3) and (5.5-10.5).
Preferably, the mass ratio of the gelatin, the Arabic gum and the silane coupling agent is (10-15): (5-8): 2.
Preferably, the mass ratio of the polyethylenimine to the octenyl succinic acid esterified starch is (5-6): 10.
The invention provides a preparation method of a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, which comprises the following steps:
mesoporous SiO 2 Mixing the nano particles, the compound natural plant extract, the surfactant and water, and then homogenizing and dispersing to obtain inner shell coating dispersion liquid;
mixing the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent, and homogenizing and dispersing to obtain middle shell coating dispersion liquid;
and mixing the middle-shell coating dispersion liquid, polyethyleneimine and octenyl succinic acid esterified starch, and homogenizing and dispersing to obtain the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule.
Preferably, the compound natural plant extract and mesoporous SiO 2 The mass ratio of the nano particles to the surfactant to the water is (2-3): 5.5-10.5): 1:50.
Preferably, the mass ratio of the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent is (50-80): 10-15): 5-8): 2:1.
Preferably, the mass ratio of the middle shell coating dispersion liquid, the polyethyleneimine and the octenyl succinic acid esterified starch is (90-100): 5-6): 10.
The invention provides a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule according to the technical scheme or application of the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule in an artificial board.
The invention provides a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, which comprises mesoporous SiO 2 A nanoparticle inner shell; is loaded on the mesoporous SiO 2 The compound natural plant extract in the inner shell mesopores of the nano particles comprises tea extract, bamboo leaf extract, cedar extract and andrographis paniculata extract; coating the mesoporous SiO 2 A middle shell on the inner shell surface of the nanoparticle, wherein the chemical composition of the middle shell comprises gelatin, acacia and a silane coupling agent; and the chemical composition of the shell comprises polyethyleneimine and octenyl succinic acid esterified starch. Firstly, the invention adopts a compound natural plant extract comprising tea extract, bamboo leaf extract, cedar wood extract and common andrographis herb extract, and the antibacterial and antiviral composition is obtained through synergistic compounding: wherein the tea extract contains tea polyphenols and purine theophylline, and the tea polyphenols comprises epicatechin, epicatechin gallate, etcThe composition has strong antioxidation effect, and has different degrees of inhibition and killing effects on a plurality of pathogenic bacteria such as common proteus, staphylococcus aureus, staphylococcus epidermidis, streptococcus mutans, botulinum, lactobacillus, vibrio cholerae, oral cavity variable chain bacteria, enteropathogenic bacteria and the like, and also has inhibition effect on common viruses such as influenza viruses, hepatitis B viruses and the like; the purine theophylline is an organic nitrogen-containing compound, and an alkaloid active substance with anti-inflammatory, anti-tumor, anticancer, antiviral and antibacterial effects; in addition, alpha-terpineol, terpinen-4-ol and terpinene in the tea extract have an inhibitory effect on early replication of influenza virus, avian influenza virus and the like. The bamboo leaf extract is rich in flavone, plant polysaccharide and benzoquinone active substances, and has strong inhibition effect on viruses, bacteria, fungi and moulds. Cedar wood extract is rich in cedrol active substances and is effective in reducing herpesvirus type 1 and type 2 plaque formation. Andrographis paniculata extract contains potassium dehydroandrographolide, and can inhibit human herpesvirus, coxsackie virus, etc. by inhibiting viral replication. Then, the invention uses mesoporous SiO 2 The nano particles are used as an inner shell adsorption carrier to adsorb the compound natural plant extract, provide mechanical strength in the hot pressing process, and simultaneously, mesoporous SiO 2 The nano particles have extremely low heat conductivity coefficient, and can play a role in high-temperature resistance protection on bioactive components in the compound natural plant extract loaded in the nano particles under the condition of short-term high temperature in the process of manufacturing the plate material. Subsequently, the invention adopts gelatin and acacia polymer material as composite middle shell wall material, and is connected with the mesoporous SiO through a silane coupling agent 2 The nanometer particle has middle shell with porous structure and inner shell with stable slow releasing effect, and the nanometer particle has ductility at high temperature and high pressure to maintain the stable coating of antiviral extract. Finally, the invention uses the polyethylenimine and octenyl succinic acid esterified starch to compound to form an outer layer for modification, on one hand, the polyethylenimine contains amino groups, which can play a role in synergistic antivirus, and simultaneously, two substances can enhance the cementing property and the hydrophilicity of the adhesive for the artificial board. The invention provides a compound TiantianHowever, the synergistic antibacterial and antiviral multishell microcapsule of the plant extracts can ensure that the compound natural plant extracts keep antibacterial and antiviral properties in a hot-pressing environment by adopting the synergistic effect of multishell structures, and can realize lasting antibacterial and antiviral effects through stable slow release, the effective period can reach several years, and the compound natural plant extract can be widely applied to the field of artificial board processing.
The invention provides a preparation method of a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, which comprises the following steps: mesoporous SiO 2 Mixing the nano particles, the compound natural plant extract, the surfactant and water, and then homogenizing and dispersing to obtain inner shell coating dispersion liquid; mixing the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent, and homogenizing and dispersing to obtain middle shell coating dispersion liquid; and mixing the middle-shell coating dispersion liquid, polyethyleneimine and octenyl succinic acid esterified starch, and homogenizing and dispersing to obtain the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule. The preparation method provided by the invention is used for coating the multi-shell microcapsule structure layer by layer in a solution environment in steps, and meanwhile, the surfactant is added in the preparation method of the inner shell coating dispersion liquid, so that the compound natural plant extract can enter the mesoporous SiO 2 In mesoporous pore canal of nano particle, adding silane coupling agent and dispersant when preparing mesochite coating dispersion liquid, the dispersant is beneficial to uniform dispersion of gelatin and acacia macromolecules in mesochite coating dispersion liquid, and the silane coupling agent realizes mesoporous SiO 2 The gelatin and the Arabic gum are connected on the surfaces of the nano-particles, so that the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule is successfully prepared.
And the silane coupling agent, the dispersing agent and the surfactant solution can ensure that the prepared compound natural plant extract synergistic antibacterial antiviral multishell microcapsule has good interfacial compatibility with water.
Detailed Description
The invention provides a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, which comprises mesoporous SiO 2 A nanoparticle inner shell;
is loaded on the mesoporous SiO 2 The compound natural plant extract in the inner shell mesopores of the nano particles comprises tea extract, bamboo leaf extract, cedar extract and andrographis paniculata extract;
coating the mesoporous SiO 2 A middle shell on the inner shell surface of the nanoparticle, wherein the chemical composition of the middle shell comprises gelatin, acacia and a silane coupling agent;
and the chemical composition of the shell comprises polyethyleneimine and octenyl succinic acid esterified starch.
In the present invention, all preparation materials/components are commercially available products well known to those skilled in the art unless specified otherwise.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention comprises mesoporous SiO 2 A nanoparticle inner shell.
In the present invention, mesoporous SiO 2 The mesoporous pore diameter of the nanoparticle is preferably 5 to 30nm, more preferably 10 to 20nm.
In the present invention, the mesoporous SiO 2 The total pore Rong Youxuan of the nano particles is 0.4-0.8 cm 3 Preferably 0.7 to 0.8cm per gram 3 /g。
In the present invention, the mesoporous SiO 2 The specific surface area of the nanoparticles is preferably 300 to 600m 2 Preferably 500 to 600m 2 /g。
In the present invention, the mesoporous SiO 2 The sphericity of the nanoparticles is good.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention comprises a mesoporous SiO supported by 2 The compound natural plant extract in the inner shell mesopores of the nano particles comprises tea extract, bamboo leaf extract, cedar extract and herba Andrographitis extract.
In the invention, the mass ratio of the tea extract, the bamboo leaf extract, the cedar wood extract and the common andrographis herb extract is preferably (2-3): (3-5): (1-2), and more preferably 2.5:4:1.5:1.5.
The four natural plant extracts are compounded, and the four natural plant extracts are different in active ingredients, can play a synergistic role in compounding and use, have very broad-spectrum inactivation on various viruses and bacteria, and have the characteristics of broad-spectrum antivirus, antibiosis, high efficiency, long-acting, biological non-resistance and the like compared with the traditional inorganic metal nanoparticle antibacterial agent. Compared with inorganic metal nano particle antiviral particles, the preparation method has the characteristics of safety, environmental friendliness, no harm to human body and the like.
In the invention, the compound natural plant extract and mesoporous SiO 2 The mass ratio of the nano particles is preferably (2-3): 5.5-10.5, more preferably (2-3): 7-9.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention comprises mesoporous SiO coated on the mesoporous SiO 2 And the chemical composition of the middle shell comprises gelatin, acacia and a silane coupling agent.
In the present invention, the silane coupling agent preferably includes a silane coupling agent of isocyanatopropyl triethoxysilane and/or a silane coupling agent of vinyltrimethoxysilane, more preferably includes a silane coupling agent of isocyanatopropyl triethoxysilane and a silane coupling agent of vinyltrimethoxysilane.
In the present invention, when the silane coupling agent preferably includes a silane coupling agent of isocyanatopropyl triethoxysilane and a silane coupling agent of vinyltrimethoxysilane, the mass ratio of the silane coupling agent of isocyanatopropyl triethoxysilane to the silane coupling agent of vinyltrimethoxysilane is preferably 2:1.
In the present invention, the mass ratio of the gelatin, the gum arabic and the silane coupling agent is preferably (10 to 15): 5 to 8): 2, more preferably (11.5 to 14.5): 5.5 to 7.5): 2.
At the bookIn the invention, gelatin and Arabic gum pass through a silane coupling agent and mesoporous SiO 2 The nanoparticles react.
In the invention, the acacia is taken as a plant natural gum, has good water solubility and emulsifying property, and the gelatin is taken as an animal protein gum, has elasticity and flexibility.
In the invention, the silane coupling agent can improve gelatin, arabic gum and mesoporous SiO 2 The interface property of the nano particles is that gelatin and Arabic gum are connected with mesoporous SiO through the action bond of a silane coupling agent 2 Nanoparticle surface, forming mesochite.
In the invention, the gelatin and the Arabic gum have the ductility and the pressure resistance of high molecular polymers, can play a role of a buffer layer in a short hot pressing process, furthest protect the inner shell and the biological active components in the loaded compound natural plant extract from being damaged, the middle shell is compounded by adopting the gelatin and the Arabic gum, the mass ratio of the gelatin and the Arabic gum to the silane coupling agent is adjusted within the range, the surface of the middle shell can form a porous structure, and the inner shell forms a release passage, so that the stable slow release effect is realized.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention comprises a shell coated on the surface of a middle shell, wherein the chemical composition of the shell comprises polyethylenimine and octenyl succinic acid esterified starch.
In the present invention, the mass ratio of the polyethyleneimine to the octenyl succinic acid esterified starch is preferably (5 to 6): 10, more preferably (5 to 6): 9.
According to the invention, both the octenyl succinic acid esterified starch and the polyethyleneimine have a cross-linked network structure, the octenyl succinic acid esterified starch and the polyethyleneimine are compounded, the octenyl succinic acid esterified starch and the polyethyleneimine further form a network cross-linked structure with stable structure through hydrogen bonding, a synergistic enhancement effect is achieved, the obtained shell structure has higher supporting strength, and the structure of the multi-shell microcapsule is more stable; and the polyethyleneimine has amino groups, has antiviral effect, and can play a role in synergistic antiviral effect.
In the invention, gelatin in the middle shell has a large number of carbonyl groups, polyethyleneimine in the outer shell has a large number of amino groups, octenyl succinic acid esterified starch has a large number of hydroxyl groups, both the amino groups of the polyethyleneimine and hydrogen in the hydroxyl groups of the octenyl succinic acid esterified starch can be used as hydrogen bond donors, and oxygen atoms in the carbonyl groups of the gelatin can be used as hydrogen bond acceptors, so that stable covalent bond effect between the middle shell and the outer shell is realized, and the structural stability is strong.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule preferably further comprises a mesoporous SiO supported by the invention 2 And (3) a surfactant in the mesopores of the inner shells of the nano particles.
In the present invention, the surfactant is preferably tween-80 and span 80.
In the present invention, the mass ratio of tween-80 to span 80 is preferably 5 (1-2), more preferably 5:2.
In the present invention, the mesoporous SiO 2 The ratio of the mass of the nanoparticle to the mass of the surfactant is preferably (5.5 to 10.5): 1, more preferably (6 to 10): 1.
The compound natural plant extract antiviral microcapsule with stable and slow release multi-shell structure provided by the invention has the diameter of preferably 100-200 nm.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention has good dispersibility in aqueous solution, can be directly mixed with urea-formaldehyde resin, phenolic resin, melamine resin and bean pulp adhesive when being used in an artificial board process, does not influence the dosage and cementing property of the adhesive, and simultaneously achieves the effects of stable slow release and broad-spectrum antiviral.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention, and the chemical composition of the middle shell preferably further comprises a dispersing agent.
In the present invention, the dispersant is preferably sodium polyacrylate.
In the present invention, the mass ratio of the silane coupling agent to the dispersant is preferably 2:1.
In the invention, the dispersing agent and the surfactant can further improve the synergistic antibacterial antiviral multishell microcapsule of the compound natural plant extract with the silane coupling agent to keep better interfacial compatibility with water.
The invention provides a preparation method of a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule, which comprises the following steps:
mesoporous SiO 2 Mixing the nano particles, the compound natural plant extract, the surfactant and water, and then homogenizing and dispersing to obtain inner shell coating dispersion liquid;
mixing the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent, and homogenizing and dispersing to obtain middle shell coating dispersion liquid;
and mixing the middle-shell coating dispersion liquid, polyethyleneimine and octenyl succinic acid esterified starch, and homogenizing and dispersing to obtain the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule.
The invention uses mesoporous SiO 2 The nanoparticle, the compound natural plant extract, the surfactant and the water are mixed (hereinafter referred to as first mixing) and then homogeneously dispersed (hereinafter referred to as first homogeneously dispersed) to obtain an inner shell coated dispersion.
In the present invention, the water is preferably deionized water.
In the invention, the compound natural plant extract and mesoporous SiO 2 The mass ratio of the nano particles, the surfactant and the water is preferably (2-3): 5.5-10.5): 1:50, more preferably (2-3): 7-9): 1:50, and even more preferably 2.5:8:1:50.
In the present invention, the mesoporous SiO 2 The nano particles can play a role of loading the compound natural plant extract, the loading capacity is large, and because of SiO 2 The nano particles have higher hardness, pressure resistance and extremely low heat conductivity coefficient, and can play a role in high-temperature resistance protection on bioactive components in the compound natural plant extract loaded in the nano particlesThe active ingredients in the compound natural plant are effectively prevented from losing or damaging in a severe environment, so that the long-term, stable and effective performance of the compound natural plant extract is ensured.
In the present invention, the order of the first mixing is preferably: mesoporous SiO 2 The nano particles, the compound natural plant extract, the surfactant and the water are sequentially mixed.
In the present invention, the rotation speed of the first homogeneous dispersion is preferably 5000 to 8000r/min, more preferably 6000 to 7000r/min.
In the present invention, the time of the first homogeneous dispersion is preferably 2 to 10 minutes, more preferably 5 to 6 minutes.
After the inner shell-coated dispersion is obtained, the inner shell-coated dispersion, gelatin, gum arabic, a silane coupling agent, and a dispersing agent are mixed (hereinafter referred to as second mixing) and then homogeneously dispersed (hereinafter referred to as second homogeneously dispersed) to obtain a middle shell-coated dispersion.
In the invention, the mass ratio of the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent is preferably (50-80): (10-15): (5-8): 2:1, more preferably 65:12:6:2:1.
In the invention, the gelatin and the Arabic gum have the ductility and the pressure resistance of high molecular polymers, can play a role of a buffer layer in a short hot pressing process, furthest protect the inner shell and the biological active components in the loaded compound natural plant extract from being damaged, the middle shell is compounded by adopting the gelatin and the Arabic gum, the mass ratio of the gelatin and the Arabic gum is adjusted within the range, the surface of the middle shell forms a porous structure, and the inner shell forms a release passage, so that the stable slow release effect is realized.
In the present invention, the inner shell-coated dispersion is preferably allowed to stand still for defoaming before the second mixing.
In the present invention, the order of the second mixing is preferably: the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent are sequentially mixed to obtain a mixed liquid, and after the mixed liquid is obtained, the mixed liquid is preferably continuously stirred and mixed at 45 ℃ until the gelatin and the Arabic gum are completely dissolved.
In the present invention, the rotation speed of the second homogeneous dispersion is preferably 5000 to 8000r/min, more preferably 6000 to 7000r/min.
In the present invention, the time of the second homogeneous dispersion is preferably 5 to 15 minutes, more preferably 8 to 10 minutes.
After the middle-shell coating dispersion liquid is obtained, the compound natural plant extract synergistic antibacterial antiviral multi-shell microcapsule is obtained by mixing the middle-shell coating dispersion liquid, polyethylenimine and octenyl succinic acid esterified starch (hereinafter referred to as third mixing) and then performing uniform dispersion (hereinafter referred to as third uniform dispersion).
In the present invention, the mass ratio of the mesochite-coated dispersion, polyethyleneimine and octenyl succinic acid esterified starch is preferably (90 to 100): (5 to 6): 10, more preferably 95:5.5:10.
In the invention, the polyethyleneimine contains amino groups and can play a role in synergistic antiviral effect. The polyethyleneimine and the octenyl succinic acid esterified starch can improve the hydrophilicity and interface compatibility of the multi-shell microcapsules, and can enhance the cementing property of the adhesive for the artificial board.
In the present invention, the present invention preferably sets the mesocarp coating dispersion to be defoamed before the third mixing.
In the present invention, the order of the third mixing is preferably: the mesochite coating dispersion, polyethylenimine and octenyl succinic acid esterified starch were mixed in sequence.
In the present invention, the rotation speed of the third homogeneous dispersion is preferably 800 to 1000r/min, more preferably 900r/min.
In the present invention, the time of the third homogeneous dispersion is preferably 2 to 4 hours, more preferably 3 hours.
The invention provides a compound natural plant extract synergistic antibacterial antiviral multishell microcapsule according to the technical scheme or application of the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule in an artificial board.
The invention provides impregnated bond paper, which comprises a base material, glue for the impregnated bond paper impregnated in the base material and the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule according to the technical scheme.
In the invention, the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule accounts for 0.5% of the mass of the adhesive for impregnated bond paper.
The invention has no special requirements on the specific types of the base material and the glue for the impregnated bond paper.
The invention provides a preparation method of impregnated bond paper, which comprises the following steps: mixing the glue for impregnating the adhesive film paper with the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule according to the technical scheme to form an impregnating solution;
impregnating a substrate material in an impregnating solution to obtain an impregnated substrate material;
and drying the impregnated base material to obtain the impregnated bond paper.
In the present invention, the time of the impregnation is preferably 30 minutes.
In the present invention, the temperature of the drying is preferably 105℃and the incubation time of the drying is preferably 10min.
In the present invention, the drying is preferably performed in a drying oven.
The invention provides an ecological plate, which comprises a base plate and the impregnated bond paper.
The invention has no special requirements on the type of the substrate.
The invention provides a preparation method of the ecological plate, which comprises the following steps:
and sticking the impregnated bond paper in the technical scheme on the surface of the substrate, and then sequentially carrying out hot pressing and maintenance to obtain the ecological plate.
In the present invention, the temperature of the hot pressing is preferably 130 ℃.
In the present invention, the pressure of the hot pressing is preferably 0.8MPa.
In the invention, the heat and pressure maintaining time of the hot pressing is preferably 7min.
In the present invention, the time of the oxidation is preferably 30 days.
The compound natural plant extract synergistic antibacterial antiviral multishell microcapsule provided by the invention has good dispersibility in aqueous solution, can be directly mixed with urea-formaldehyde resin, phenolic resin, melamine resin and bean pulp adhesive when being used in an artificial board process, does not influence the dosage and cementing property of the adhesive, and simultaneously achieves the effects of stable slow release and broad-spectrum antiviral.
The above technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
100g of deionized water is added into a 500mL beaker, 4g of deionized water with 6.5nm aperture and good sphericity is added, and the total pore volume is 0.758cm 3 Per g, specific surface area of 513m 2 Mesoporous SiO/g 2 And (3) uniformly mixing 11g of the nano particles, 2g of the mixture of tween-80 and span 80, and uniformly dispersing for 2min by using a homogenizer at a rotating speed of 8000r/min to obtain an inner shell coated dispersion.
The compound natural plant extract comprises tea extract, bamboo leaf extract, cedar wood extract and herba Andrographitis extract, wherein the mass ratio is 2:3:1:1.
The mass ratio of the tween-80 to span 80 is 5:1.
After standing and defoaming the inner shell coating dispersion liquid, adding 100g of the inner shell coating dispersion liquid into a 500mL beaker, adding 20g of gelatin, 10g of Arabic gum, 4g of a mixture of silane coupling agent, namely, isocyanatopropyl triethoxysilane and silane coupling agent, namely, vinyl trimethoxysilane, and 2g of sodium polyacrylate, magnetically stirring at 45 ℃ until the gelatin and the Arabic gum are completely dissolved, and uniformly dispersing for 5min at a rotating speed of 5000r/min to obtain the middle shell coating dispersion liquid.
The mass ratio of the silane coupling agent, namely the isocyanatopropyl triethoxysilane to the silane coupling agent, namely the vinyl trimethoxysilane is 2:1.
And standing and defoaming the middle-shell coating dispersion liquid, adding 90g of the middle-shell coating dispersion liquid into a 500mL beaker, adding 5g of polyethylenimine and 10g of octenyl succinic acid esterified starch, and mechanically stirring and dispersing at a rotating speed of 800r/min for 2h to obtain the compound natural plant extract synergistic antibacterial and antiviral multi-shell microcapsule.
Example 2
100g of deionized water is added into a 500mL beaker, 6g of deionized water with the aperture of 30nm and good sphericity is added, and the total pore volume is 0.412cm 3 Per g, specific surface area 323m 2 Mesoporous SiO/g 2 And (3) uniformly mixing 21g of the nano particles, 2g of the mixture of tween-80 and span 80, and uniformly dispersing for 10min by using a homogenizer at a rotating speed of 5000r/min to obtain an inner shell coated dispersion.
The compound natural plant extract comprises tea extract, bamboo leaf extract, cedar wood extract and herba Andrographitis extract, wherein the mass ratio is 3:5:2:2.
The mass ratio of the tween-80 to span 80 is 5:1.
After standing and defoaming the inner shell coating dispersion, adding 160g of the inner shell coating dispersion into a 500mL beaker, adding 30g of gelatin, 16g of Arabic gum, 4g of a mixture of silane coupling agent, namely, isocyanatopropyl triethoxysilane and silane coupling agent, namely, vinyl trimethoxysilane, and 2g of sodium polyacrylate, magnetically stirring at 45 ℃ until the gelatin and the Arabic gum are completely dissolved, and uniformly dispersing for 15min at a rotating speed of 8000r/min to obtain the middle shell coating dispersion.
The mass ratio of the silane coupling agent, namely the isocyanatopropyl triethoxysilane to the silane coupling agent, namely the vinyl trimethoxysilane is 2:1.
And standing and defoaming the middle-shell coating dispersion liquid, adding 100g of the middle-shell coating dispersion liquid into a 500mL beaker, adding 6g of polyethylenimine and 10g of octenyl succinic acid esterified starch, and mechanically stirring and dispersing for 4 hours at a rotating speed of 1000r/min to obtain the compound natural plant extract synergistic antibacterial and antiviral multi-shell microcapsule.
Example 3
100g of deionized water is added into a 500mL beaker, 5g of deionized water with a pore diameter of 15nm and good sphericity is added, and the total pore volume is 0.769cm 3 Per gram, specific surface area of 598m 2 Mesoporous SiO/g 2 And (3) uniformly mixing 16g of the nano particles, 2g of the mixture of tween-80 and span 80, and uniformly dispersing for 6min by using a homogenizer at a rotating speed of 6000r/min to obtain an inner shell coated dispersion.
The compound natural plant extract comprises tea extract, bamboo leaf extract, cedar wood extract and herba Andrographitis extract, wherein the mass ratio is 2.5:4:1.5:1.5.
The mass ratio of the tween-80 to span 80 is 5:1.
After standing and defoaming the inner shell coating dispersion, adding 130g of the inner shell coating dispersion into a 500mL beaker, adding 24g of gelatin, 12g of Arabic gum, 4g of a mixture of silane coupling agent, namely, isocyanatopropyl triethoxysilane and silane coupling agent, namely, vinyl trimethoxysilane, and 2g of sodium polyacrylate, magnetically stirring at 45 ℃ until the gelatin and the Arabic gum are completely dissolved, and uniformly dispersing for 9min at a rotating speed of 6000r/min to obtain the middle shell coating dispersion.
The mass ratio of the silane coupling agent, namely the isocyanatopropyl triethoxysilane to the silane coupling agent, namely the vinyl trimethoxysilane is 2:1.
And standing and defoaming the middle-shell coating dispersion liquid, adding 95g of the middle-shell coating dispersion liquid into a 500mL beaker, adding 5.5g of polyethylenimine and 10g of octenyl succinic acid esterified starch, and mechanically stirring and dispersing for 3 hours at the rotating speed of 900r/min to obtain the compound natural plant extract synergistic antibacterial and antiviral multi-shell microcapsule.
Comparative example 1
100g of deionized water is added into a 500mL beaker, 5g of deionized water with a pore diameter of 15nm and good sphericity is added, and the total pore volume is 0.769cm 3 Per gram, specific surface area of 598m 2 Mesoporous SiO/g 2 Nanoparticle, mixing uniformly compound natural plant extract 16g, tween-80 and span 80 mixture 2g, mixing with glass rod, and stirring at 6000r/min with homogenizerHomogenizing and dispersing for 6min under the piece to obtain inner shell coating dispersion liquid.
The compound natural plant extract comprises tea leaf extract and bamboo leaf extract, and the mass ratio is 2.5:4.
The mass ratio of the tween-80 to span 80 is 5:1.
After standing and defoaming the inner shell coating dispersion, adding 130g of the inner shell coating dispersion into a 500mL beaker, adding 24g of gelatin, 12g of Arabic gum, 4g of a mixture of silane coupling agent, namely, isocyanatopropyl triethoxysilane and silane coupling agent, namely, vinyl trimethoxysilane, and 2g of sodium polyacrylate, magnetically stirring at 45 ℃ until the gelatin and the Arabic gum are completely dissolved, and uniformly dispersing for 9min at a rotating speed of 6000r/min to obtain the middle shell coating dispersion.
The mass ratio of the silane coupling agent, namely the isocyanatopropyl triethoxysilane to the silane coupling agent, namely the vinyl trimethoxysilane is 2:1.
And standing and defoaming the middle-shell coating dispersion liquid, adding 95g of the middle-shell coating dispersion liquid into a 500mL beaker, adding 5.5g of polyethylenimine and 10g of octenyl succinic acid esterified starch, and mechanically stirring and dispersing for 3 hours at the rotating speed of 900r/min to obtain the compound natural plant extract synergistic antibacterial and antiviral multi-shell microcapsule.
Comparative example 2
100g of deionized water is added into a 500mL beaker, 5g of deionized water with a pore diameter of 15nm and good sphericity is added, and the total pore volume is 0.769cm 3 Per gram, specific surface area of 598m 2 Mesoporous SiO/g 2 And (3) uniformly mixing 16g of the nano particles, 2g of the mixture of tween-80 and span 80, and uniformly dispersing the mixture for 6min by using a homogenizer at a rotating speed of 6000r/min to obtain the synergistic antibacterial and antiviral microcapsule of the compound natural plant extract.
The compound natural plant extract comprises tea extract, bamboo leaf extract, cedar wood extract and herba Andrographitis extract, wherein the mass ratio is 2.5:4:1.5:1.5.
The mass ratio of the tween-80 to span 80 is 5:1.
Comparative example 3
100g of deionized water, 5g of well, was added to a 500mL beakerHas a diameter of 15nm and a sphericity of 0.769cm 3 Per gram, specific surface area of 598m 2 Mesoporous SiO/g 2 And (3) uniformly mixing 16g of the nano particles, 2g of the mixture of tween-80 and span 80, and uniformly dispersing for 6min by using a homogenizer at a rotating speed of 6000r/min to obtain an inner shell coated dispersion.
The compound natural plant extract comprises tea extract, bamboo leaf extract, cedar wood extract and herba Andrographitis extract, wherein the mass ratio is 2.5:4:1.5:1.5.
The mass ratio of the tween-80 to span 80 is 5:1.
And (3) standing and defoaming the inner shell coating dispersion liquid, adding 130g of the inner shell coating dispersion liquid into a 500mL beaker, adding 24g of gelatin, 12g of acacia, 4g of a mixture of silane coupling agent, namely isocyanatopropyl triethoxysilane and silane coupling agent, namely vinyltrimethoxysilane, and 2g of sodium polyacrylate, magnetically stirring at 45 ℃ until the gelatin and acacia are completely dissolved, and uniformly dispersing for 9min at a rotating speed of 6000r/min to obtain the compound natural plant extract synergistic antibacterial antiviral double-shell microcapsule.
The mass ratio of the silane coupling agent, namely the isocyanatopropyl triethoxysilane to the silane coupling agent, namely the vinyl trimethoxysilane is 2:1.
Test example 1
The compound natural plant extracts prepared in examples 1 to 3 and comparative example 1 were tested for antiviral activity and antibacterial performance in cooperation with the antibacterial and antiviral multishell microcapsules, and the test results are shown in tables 1 and 2.
TABLE 1 results of microcapsule antiviral Activity test (μg/mL)
As can be seen from the data in Table 1, the compound natural plant extracts prepared in examples 1 to 3 cooperate with the antibacterial and antiviral multishell microcapsules to have the effects of resisting H3N2 influenza, hepatitis B, feline calicivirus, enteroEV 71 virus and herpes virus, and particularly has the effect of inhibiting the herpes virus obviously better than the effect of inhibiting H3N2 influenza virus and hepatitis B virus.
As can be seen from the comparison results of examples 1 to 3 and comparative example 1, the microcapsules lacking the extracts of cedar wood and common andrographis herb have greatly reduced effects on resisting hepatitis B and herpes virus, and slightly reduced antiviral ability on H3N2 influenza virus, feline calicivirus and enteroEV 71 virus; this shows that the compound natural plant extract provided by the invention has synergistic antiviral effect.
TABLE 2 antibacterial ratio of microcapsules (%)
| Sequence number | Staphylococcus aureus | Coli bacterium | Candida albicans |
| Example 1 | 97.3 | 95.3 | 89.2 |
| Example 2 | 96.5 | 93.2 | 88.3 |
| Example 3 | 99.3 | 96.9 | 92.7 |
| Comparative example 1 | 90.1 | 90.4 | 85.4 |
As can be seen from the data in Table 2, the compound natural plant extracts prepared in examples 1-3 have synergistic antibacterial and antiviral multi-shell microcapsules with the effect of inhibiting staphylococcus aureus, escherichia coli and candida albicans.
From the comparison results of examples 1 to 3 and comparative example 1, it can be seen that the microcapsules lacking the extracts of cedar wood and common andrographis herb have greatly reduced effects on staphylococcus aureus, escherichia coli and candida albicans, which indicates that the compound natural plant extract provided by the invention has synergistic antibacterial effect.
Test example 2
In order to further illustrate that the compound natural plant extract synergistic antibacterial and antiviral multishell microcapsule provided by the invention has high temperature resistance and high pressure resistance, samples prepared in examples 1-3 and comparative examples 2 and 3 are respectively added into glue for impregnated bond paper, the addition amount is 0.5% of the adhesive, the impregnated bond paper is impregnated for 30 seconds, dried in an oven at 10min and 105 ℃, stuck to an ecological plate, and subjected to hot pressing at 130 ℃ for 7min and 0.8MPa, and then placed for 30 days for antiviral test. The test results are shown in tables 3 and 4.
Table 3 results table of antiviral Activity test of Compound Natural plant extract microcapsules prepared in examples 1 to 3 and comparative examples 2 and 3 (μg/mL)
As can be seen from the data in Table 3, the multi-shell compound natural plant extract microcapsules prepared in examples 1 to 3 have the effects of resisting H3N2 influenza, hepatitis B, feline calicivirus, enteroEV 71 virus and herpes virus after being used in ecological plates. Comparative example 2 shows that the antiviral effect is obviously weakened after the microcapsule coated by the inner shell is used for the ecological plate; comparative example 3 shows that the antiviral properties of the microcapsules are improved after the inner and outer shells are structurally designed, but still lower than those of the multi-shell microcapsules.
Table 4 Compound Natural plant extract microcapsules prepared in examples 1 to 3 and comparative examples 2 and 3 were used for ecological plate bacteriostasis rate (%)
| Sequence number | Staphylococcus aureus | Coli bacterium | Candida albicans |
| Example 1 | 96.2 | 94.9 | 86.2 |
| Example 2 | 95.5 | 92.7 | 87.8 |
| Example 3 | 98.1 | 95.7 | 90.2 |
| Comparative example 2 | 88.4 | 85.1 | 83.2 |
| Comparative example 3 | 90.8 | 89.4 | 84.4 |
As can be seen from the data in table 4, the multi-shell compound natural plant extract microcapsules prepared in examples 1 to 3 still have the effect of inhibiting staphylococcus aureus, escherichia coli and candida albicans after being used in ecological plates. Comparative example 2 shows that the antibacterial effect is obviously weakened after the microcapsule coated by the inner shell is used for the ecological plate; comparative example 3 shows that the antibacterial property of the microcapsules is improved after the inner shell and the outer shell are structurally designed, but is still lower than that of the multi-shell microcapsules.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (8)
1. The application of the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule in the artificial board is characterized in that the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule comprises mesoporous SiO 2 A nanoparticle inner shell;
is loaded on the mesoporous SiO 2 The compound natural plant extract in the inner shell mesopores of the nano particles comprises tea extract, bamboo leaf extract, cedar extract and andrographis paniculata extract; the tea leaf extract, the bamboo leaf extract, the cedar wood extract and the andrographis paniculata extractThe mass ratio is (2-3): 3-5): 1-2;
coating the mesoporous SiO 2 A middle shell on the inner shell surface of the nanoparticle, wherein the chemical composition of the middle shell comprises gelatin, acacia and a silane coupling agent;
and the chemical composition of the shell comprises polyethyleneimine and octenyl succinic acid esterified starch.
2. The use according to claim 1, characterized in that the compound natural plant extract and mesoporous SiO 2 The mass ratio of the nano particles is (2-3) and (5.5-10.5).
3. The use according to claim 1, characterized in that the mass ratio of the gelatin, the gum arabic and the silane coupling agent is (10-15): (5-8): 2.
4. The use according to claim 1, characterized in that the mass ratio of polyethylenimine to octenyl succinic esterified starch is (5-6): 10.
5. The use according to any one of claims 1 to 4, wherein the preparation method of the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule comprises the following steps:
mesoporous SiO 2 Mixing the nano particles, the compound natural plant extract, the surfactant and water, and then homogenizing and dispersing to obtain inner shell coating dispersion liquid;
mixing the inner shell coating dispersion liquid, gelatin, arabic gum, silane coupling agent and dispersing agent, and homogenizing and dispersing to obtain middle shell coating dispersion liquid;
and mixing the middle-shell coating dispersion liquid, polyethyleneimine and octenyl succinic acid esterified starch, and homogenizing and dispersing to obtain the compound natural plant extract synergistic antibacterial antiviral multishell microcapsule.
6. Use according to claim 5Characterized in that the compound natural plant extract and mesoporous SiO 2 The mass ratio of the nano particles to the surfactant to the water is (2-3): 5.5-10.5): 1:50.
7. The use according to claim 5, wherein the mass ratio of the inner shell coating dispersion, gelatin, gum arabic, silane coupling agent and dispersant is (50-80): (10-15): (5-8): 2:1.
8. The use according to claim 5, wherein the mass ratio of the mesochite coating dispersion, polyethyleneimine and octenyl succinic acid esterified starch is (90-100): 5-6): 10.
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