CN116019141A - Nano cellulose aerogel antibacterial essential oil slow-release system and preparation method and application thereof - Google Patents
Nano cellulose aerogel antibacterial essential oil slow-release system and preparation method and application thereof Download PDFInfo
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- CN116019141A CN116019141A CN202310322528.XA CN202310322528A CN116019141A CN 116019141 A CN116019141 A CN 116019141A CN 202310322528 A CN202310322528 A CN 202310322528A CN 116019141 A CN116019141 A CN 116019141A
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Abstract
The invention relates to the technical field of ocean transportation packaging, in particular to a nanocellulose aerogel antibacterial essential oil slow-release system, a preparation method and application thereof. The system takes the hydrophobically modified nano cellulose aerogel as a carrier, and volatile essential oil extracted from plants is taken as an antibacterial active substance, so that the system is used for antibacterial fresh-keeping in the long-period sea transportation process of fruits and vegetables. The essential oil molecules are released to the packaging environment or the surfaces of fruits and vegetables in a diffusible form through aerogel pores, so that the antibacterial effect is realized. The release type antibacterial mode of the system can effectively improve the contact area of antibacterial active substances and fruits and vegetables, improve the antibacterial effect, reduce the consumption of essential oil through the slow release effect of aerogel, and provide long-time antibacterial effect. The slow release matrix and the essential oil are both biological sources, and have higher biological safety.
Description
Technical Field
The invention relates to the technical field of ocean transportation packaging, in particular to a nanocellulose aerogel antibacterial essential oil slow-release system, a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
China is a country where fruits and vegetables are produced, and import and export trade of vegetables and fruits is often carried through ocean. The storage mode adopted in the transportation process is to put fruits and vegetables in a sealed storage bag, and put the fruits and vegetables in a low-temperature environment for refrigeration and fresh-keeping. However, due to the long marine transportation time, certain amount of water vapor can be generated by respiration of fruits and vegetables in the transportation process, and partial bacteria can grow and reproduce even in a low-temperature condition in a closed humid environment for a long time, so that the fruits and vegetables are deteriorated and spoiled.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides an economic, safe and long-acting nano cellulose aerogel antibacterial essential oil slow-release system which is used for preserving fruits and vegetables in long-period ocean transportation.
The antibacterial essential oil slow-release system adopts volatile essential oil extracted from plants as antibacterial active substances, and nano cellulose aerogel as a 'storage reservoir' of the antibacterial essential oil and a 'valve' for regulating release, so as to form a release type antibacterial system. According to the system, the aerogel material nanoscale porous structure is utilized, each pore is used as a storage unit of the essential oil, and the essential oil needs to pass through the pore wall after volatilization, so that the diffusion and volatilization speed of the antibacterial essential oil can be slowed down, and the aim of long-time slow release is fulfilled.
According to the invention, the pore size and the porosity of the nano cellulose aerogel can be controlled by changing the concentration of cellulose raw materials in the preparation process, so that the loading rate of essential oil and the diffusion speed of the essential oil from the inside of the aerogel are regulated and improved, and the requirements of antibacterial and fresh-keeping of different fruits and vegetables are met.
The antibacterial essential oil slow release system has good biological safety, can be directly placed in a storage bag to be stored together with fruits and vegetables, and the volatile essential oil can enable the antibacterial essential oil in a packaging environment to be maintained at a high concentration for a long time, and the essential oil is directly and fully contacted with the surfaces of the fruits and vegetables to directly inactivate bacteria growing on the surfaces of the fruits and vegetables. The slow release system can also be used together with the conventional refrigeration storage mode to improve the fresh-keeping effect.
In order to achieve the technical purpose, the invention provides the following technical scheme.
The invention provides a preparation method of a nanocellulose aerogel antibacterial essential oil slow-release system, which mainly comprises the following steps:
(1) Dissolving nano cellulose by an alkali urea system, and stirring at a high speed in an ice-water bath to obtain nano cellulose sol;
(2) Centrifuging the nanocellulose sol at a high speed to remove bubbles, pouring the centrifuged sol into a mold, and freezing;
(3) Heating the frozen sol in water bath to form gel, and soaking the gel in pure water to change water until the pH of the gel becomes neutral;
(4) Replacing the solvent of the nano cellulose gel in ethanol, and drying the nano cellulose gel by a carbon dioxide supercritical device to obtain nano cellulose aerogel;
(5) Carrying out hydrophobization modification on the nano cellulose aerogel;
(6) And loading the antibacterial essential oil on the hydrophobized modified nano cellulose aerogel in a vacuum impregnation mode to obtain the nano cellulose aerogel antibacterial essential oil slow-release system.
Further, the alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of the nanocellulose in the alkali urea system is 3%.
Further, the nanocellulose is one of bacterial cellulose, microcrystalline cellulose and cellulose nanocrystals.
Further, the freezing condition is that the materials are put into a refrigerator with the temperature of minus 15 to minus 10 ℃ to be frozen for 8 to 20 hours; preferably, the mixture is frozen in a refrigerator at-12 ℃ for 12 hours.
Further, the water bath heating temperature is 60-80 ℃, preferably 75 ℃.
Further, the solvent replacement procedure was as follows: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days.
Further, the supercritical carbon dioxide drying conditions are as follows:temperature 60 ℃, pressure 17.5MPa and CO 2 The flow rate was 20g/min.
Further, the modification method of the nano cellulose aerogel is a vapor deposition method, and comprises the following steps:
placing the nanocellulose aerogel and two open glass bottles respectively filled with hydrophobic silane and pure water into a sealed glass container; placing the sealed container into an oven at 80 ℃ for reaction for 10 hours; after the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
Wherein the hydrophobic silane is fluorine-free long-chain silane, and is selected from octadecyl trichlorosilane, hexadecyl trimethoxy silane and the like.
The hydrophobic silane used in the method is a silane reagent which is volatile under the high temperature condition, can be subjected to hydrolysis reaction with surrounding water vapor after being deposited on the surface of the nanocellulose, and further can be subjected to cross-linking reaction with hydroxyl groups on the nanocellulose, so that stable modification of the nanocellulose is realized.
Further, the antibacterial essential oil is one of thyme essential oil, rosemary essential oil, oregano essential oil and cinnamon essential oil.
In a second aspect of the invention, a nanocellulose aerogel antibacterial essential oil slow release system prepared by the preparation method is provided.
The third aspect of the invention provides application of the nanocellulose aerogel antibacterial essential oil slow-release system in fruit and vegetable fresh-keeping, and further application of the nanocellulose aerogel antibacterial essential oil slow-release system in fruit and vegetable fresh-keeping in marine transportation.
The nano cellulose aerogel antibacterial essential oil slow release system provided by the invention has the following advantages:
(1) The slow release system of the invention belongs to a release type antibacterial system, volatile essential oil is slowly volatilized from aerogel materials and released into the whole packaging environment, and the essential oil can fully contact fruits and vegetables, thereby fully playing an antibacterial role.
(2) The nanocellulose aerogel is used as a slow-release matrix, so that the volatilization speed of essential oil is reduced, the antibacterial action time is prolonged, and meanwhile, the excessive consumption of the antibacterial agent is reduced.
(3) The slow release speed of the essential oil can be adjusted by adjusting the porosity and the surface property of the aerogel, so that the method is suitable for the fresh-keeping requirements of fruits and vegetables of different types and has a wide application range;
(4) The slow release material in the slow release system is biomass material, the essential oil is plant extract, and the slow release system has high biological safety, is directly put into fruit and vegetable storage bags for use, and can also be used in combination with the current common preservation technology to improve the preservation effect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a schematic illustration of a nanocellulose aerogel.
Fig. 2 is a schematic diagram of an antimicrobial essential oil loaded nanocellulose aerogel.
FIG. 3 is a scanning electron microscope image of nanocellulose aerogel.
Fig. 4 is a transmission electron microscopy image of nanocellulose aerogel.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Bacterial cellulose is dissolved by an alkali urea system, and the bacterial cellulose is stirred by a high-speed stirrer in ice water bath to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of bacterial cellulose in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-12 ℃ for 12 hours.
(3) The sol was heated in a 75 ℃ water bath to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Rosemary essential oil is loaded on the hydrophobically modified nanocellulose aerogel by vacuum impregnation (as shown in figure 2).
Scanning electron microscope images and transmission electron microscope images of the nanocellulose aerogel are shown in fig. 3 and 4.
Example 2
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Dissolving microcrystalline cellulose by an alkali urea system, and stirring in ice water bath by a high-speed stirrer to obtain the nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of microcrystalline cellulose in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-12 ℃ for 12 hours.
(3) The sol was heated in a 75 ℃ water bath to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Rosemary essential oil is loaded on the hydrophobically modified nanocellulose aerogel by vacuum impregnation (as shown in figure 2).
Example 3
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Dissolving cellulose nanocrystalline by an alkali urea system, and stirring in ice water bath by a high-speed stirrer to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of the cellulose nanocrystalline in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-12 ℃ for 12 hours.
(3) The sol was heated in a 75 ℃ water bath to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Rosemary essential oil is loaded on the hydrophobically modified nanocellulose aerogel by vacuum impregnation (as shown in figure 2).
Example 4
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Dissolving cellulose nanocrystalline by an alkali urea system, and stirring in ice water bath by a high-speed stirrer to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of the cellulose nanocrystalline in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at high speed to remove bubbles, the centrifuged sol is poured into a mould and is put into a refrigerator at-15 ℃ for freezing for 8 hours.
(3) The sol was heated in a water bath at 80 ℃ to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Rosemary essential oil is loaded on the hydrophobically modified nanocellulose aerogel by vacuum impregnation (as shown in figure 2).
Example 5
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Dissolving cellulose nanocrystalline by an alkali urea system, and stirring in ice water bath by a high-speed stirrer to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of the cellulose nanocrystalline in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-10 ℃ for 20 hours.
(3) The sol was heated in a water bath at 60 ℃ to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Rosemary essential oil is loaded on the hydrophobically modified nanocellulose aerogel by vacuum impregnation (as shown in figure 2).
Example 6
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Bacterial cellulose is dissolved by an alkali urea system, and the bacterial cellulose is stirred by a high-speed stirrer in ice water bath to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of bacterial cellulose in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-12 ℃ for 12 hours.
(3) The sol was heated in a 75 ℃ water bath to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Thyme essential oil was loaded onto hydrophobically modified nanocellulose aerogel by means of vacuum impregnation (as shown in fig. 2).
Example 7
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Bacterial cellulose is dissolved by an alkali urea system, and the bacterial cellulose is stirred by a high-speed stirrer in ice water bath to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of bacterial cellulose in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-12 ℃ for 12 hours.
(3) The sol was heated in a 75 ℃ water bath to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Oregano essential oil was loaded onto the hydrophobically modified nanocellulose aerogel by vacuum impregnation (as shown in FIG. 2).
Example 8
The preparation of the fruit and vegetable antibacterial slow-release system mainly comprises the following steps:
(1) Bacterial cellulose is dissolved by an alkali urea system, and the bacterial cellulose is stirred by a high-speed stirrer in ice water bath to obtain nano cellulose sol. The alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea is 7:13:80; the mass fraction of bacterial cellulose in the alkali urea system is 3%.
(2) The nanocellulose sol is centrifuged at a high speed to remove bubbles, the centrifuged sol is poured into a mold and is frozen in a refrigerator at-12 ℃ for 12 hours.
(3) The sol was heated in a 75 ℃ water bath to form a gel, and the gel was immersed in pure water to constantly change the water until the gel pH became neutral.
(4) The solvent replacement of the nanocellulose gel in ethanol comprises the following specific replacement processes: soaking cellulose gel in absolute ethanol, and replacing solvent every 12h for 5 days. Drying by a carbon dioxide supercritical device to obtain the nano cellulose aerogel (shown in figure 1).
(5) The modification steps of the nanocellulose aerogel are as follows:
the nanocellulose aerogel was placed in a sealed glass container along with two open glass bottles each containing hydrophobic silane and pure water. The sealed vessel was placed in an 80 ℃ oven and reacted for 10 hours. After the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
(6) Cinnamon essential oil was loaded onto hydrophobically modified nanocellulose aerogel by means of vacuum impregnation (as shown in fig. 2).
The foregoing description of the preferred embodiments of the present invention is not intended to limit the scope of the claims, which follow, as defined in the claims.
Claims (10)
1. The preparation method of the nano cellulose aerogel antibacterial essential oil slow-release system is characterized by comprising the following steps of:
(1) Dissolving nano cellulose by an alkali urea system, and stirring at a high speed in an ice-water bath to obtain nano cellulose sol;
(2) Centrifuging the nanocellulose sol at a high speed to remove bubbles, pouring the centrifuged sol into a mold, and freezing;
(3) Heating the frozen sol in water bath to form gel, and soaking the gel in pure water to change water until the pH of the gel becomes neutral;
(4) Replacing the solvent of the nano cellulose gel in ethanol, and drying the nano cellulose gel by a carbon dioxide supercritical device to obtain nano cellulose aerogel;
(5) Carrying out hydrophobization modification on the nano cellulose aerogel;
(6) And loading the antibacterial essential oil on the hydrophobized modified nano cellulose aerogel in a vacuum impregnation mode to obtain the nano cellulose aerogel antibacterial essential oil slow-release system.
2. The preparation method according to claim 1, wherein the alkali urea system consists of NaOH, urea and water, and the mass ratio of the alkali urea system to the urea system is 7:13:80; the mass fraction of the nanocellulose in the alkali urea system is 3%.
3. The method of claim 1, wherein the nanocellulose is one of bacterial cellulose, microcrystalline cellulose, and cellulose nanocrystals.
4. The preparation method according to claim 1, wherein the freezing condition is that the mixture is frozen in a refrigerator at-15 to-10 ℃ for 8 to 20 hours; preferably, the mixture is frozen in a refrigerator at-12 ℃ for 12 hours.
5. The preparation method according to claim 1, wherein the water bath heating temperature is 60-80 ℃, preferably 75 ℃.
6. The method of claim 1, wherein the solvent displacement process is as follows: soaking cellulose gel in absolute ethyl alcohol, replacing the solvent every 12 hours, and continuously soaking for 5 days;
the supercritical carbon dioxide drying conditions are as follows: temperature 60 ℃, pressure 17.5MPa and CO 2 The flow rate was 20g/min.
7. The method of claim 1, wherein the nanocellulose aerogel modification process is a vapor deposition process;
preferably, the specific modification steps are as follows:
placing the nanocellulose aerogel and two open glass bottles respectively filled with hydrophobic silane and pure water into a sealed glass container; placing the sealed container into an oven at 80 ℃ for reaction for 10 hours; after the reaction was completed, the modified nanocellulose aerogel was placed in an oven at 60 ℃ to remove residual reagents.
8. The method of claim 1, wherein the antimicrobial essential oil is one of thyme essential oil, rosemary essential oil, oregano essential oil, and cinnamon essential oil.
9. The nanocellulose aerogel antibacterial essential oil extended release system prepared by the method for preparing the nanocellulose aerogel antibacterial essential oil extended release system of any one of claims 1-8.
10. The use of a nanocellulose aerogel antimicrobial essential oil extended release system as claimed in claim 9 in fruit and vegetable preservation, preferably in marine transportation.
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