CN115216998A - Preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion - Google Patents

Preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion Download PDF

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CN115216998A
CN115216998A CN202210752507.7A CN202210752507A CN115216998A CN 115216998 A CN115216998 A CN 115216998A CN 202210752507 A CN202210752507 A CN 202210752507A CN 115216998 A CN115216998 A CN 115216998A
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essential oil
cellulose
activated carbon
paper
baili
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邵平
刘黎明
林杨
伊财富
潘杰峰
陈杭君
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/10—Packing paper
    • 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
    • A01N25/08—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 containing solids as carriers or diluents
    • 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
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • 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
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08—Magnoliopsida [dicotyledons]
    • A01N65/22—Lamiaceae or Labiatae [Mint family], e.g. thyme, rosemary, skullcap, selfheal, lavender, perilla, pennyroyal, peppermint or spearmint
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P3/00—Fungicides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/38—Coatings with pigments characterised by the pigments
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/46—Non-macromolecular organic compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/22—Agents rendering paper porous, absorbent or bulky
    • D21H21/24—Surfactants
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
    • Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics

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Abstract

The invention discloses a preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion, which comprises the following steps: (1) preparing a porous cellulose activated carbon sample; (2) preparing a baili essential oil microemulsion; (3) Preparing a cellulose activated carbon/Baili essential oil micro-emulsion compound; (4) mixing the components in a mass ratio of 1:20-25, dissolving the cellulose activated carbon/Baili essential oil micro-emulsion compound and ethyl cellulose in absolute ethyl alcohol, and fully dissolving to prepare a coating liquid; (5) Uniformly coating the coating liquid on the surface of food packaging base paper to obtain coated paper; and fully drying the coated paper at room temperature to obtain the antibacterial paper. The preparation method can increase the loading capacity of the antibacterial agent essential oil, enhance the antibacterial effect of the essential oil and prolong the release time of the essential oil; meanwhile, the permeability of water vapor and carbon dioxide of the paper can be improved, the air permeability and the water permeability can be increased, the mechanical property of the paper is improved, and the service life of the antibacterial paper is prolonged.

Description

Preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion
(I) the technical field
The invention belongs to the technical field of packaging paper, and particularly relates to a preparation method of antibacterial paper.
(II) technical background
The food is easily polluted by bacteria, mould and other microorganisms in the processes of production, circulation and storage, so that the nutritional value of the food is reduced, the quality of the food is deteriorated, and the health of people is even harmed. Therefore, in order to ensure the safety and hygiene of food, it is necessary to properly package the food so as to prevent the invasion of external environmental factors. At present, plastic films are the most common packaging materials in the aspect of food preservation, and are widely applied to the market due to the advantages of transparency, low price, convenient use and the like. However, the conventional plastic packaging film also has the following disadvantages: the food has no antibacterial function and is difficult to store for a long time; the film has poor water vapor permeability, and when the film is applied to fruits, vegetables and other foods, condensed water can be generated inside the package to cause breeding of microorganisms and rotting and deterioration; petroleum-based plastic films are not biodegradable and can cause serious environmental pollution. Therefore, a new packaging material is required to replace it.
Packaging of paper materials is a largest sub-industry of the packaging industry. The paper material packaging is widely applied in the market and has various varieties, and the paper material belongs to a green packaging material with wide prospect. As an indispensable material in life, wrapping paper is required to have not only basic mechanical properties but also certain functionality. The antibacterial paper has great research significance, and the packaged food can be delayed from deteriorating and the edible period can be prolonged by applying the antibacterial paper to the packaging of the daily food. The traditional antibacterial paper is coated with the antibacterial agent through wet cloth addition, surface sizing, spraying, dipping, coating and other modes, and has short action time and poor fresh-keeping effect.
Patent CN106884360A discloses a method for preparing safe and highly effective antibacterial food wrapping paper, which comprises spraying antibacterial agent onto the inner surface of base paper with kraft paper as base paper and plant extract as antibacterial agent, and coating adhesive and waterproof layer to form antibacterial wrapping paper. The method has the advantages that the antibacterial agent cannot be uniformly distributed in the paper base by simple spraying, and the effective components are easily lost. Patent CN109134942B discloses a preparation method of transparent nano cellulose antibacterial paper, which comprises adding sodium alginate, nano cellulose and glycerol into a certain amount of deionized water according to a certain ratio as antibacterial agent, stirring, ultrasonic dispersing, and vacuum filtering to obtain the transparent nano cellulose antibacterial paper. The method has limited antibacterial effect, and is easy to cause loss of effective components in the antibacterial agent, and cannot exert antibacterial effect for a long time.
The invention adopts microemulsion embedding technology, coats plant essential oil with bacteriostasis and sterilization effects, compounds the plant essential oil with porous carrier bio-based active carbon, and uniformly distributes the plant essential oil and the porous carrier bio-based active carbon on the surface of paper, thereby realizing the slow-release sterilization effect and improving the bioavailability of active substances. Meanwhile, after the paper base material is coated by the porous adsorption essential oil microemulsion, the air permeability and the overall mechanical property are improved, the service life and the range of the antibacterial paper are prolonged, and the method has very important significance for promoting the development of the antibacterial paper industry in China.
Disclosure of the invention
In order to solve the problems, the invention aims to provide a preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion, which comprises the following steps:
(1) Weighing cellulose powder, placing the cellulose powder in a ceramic boat, and carbonizing the cellulose powder for 2 to 3 hours at a high temperature of between 500 and 700 ℃ under the protection of argon to obtain a carbon source precursor; adding KOH with the same mass into a carbon source precursor, adding water for dissolving, then freeze-drying, transferring the solid obtained by freeze-drying to a ceramic boat, and reacting in CO 2 Activating for 0.5-1.5h at 700-900 ℃ under the protection of gas, and cooling to obtain a porous cellulose activated carbon sample;
(2) Uniformly mixing a surfactant RH40 and a cosurfactant Span80 according to the mass ratio of 2-4; mixing a mixed surfactant and the Baili essential oil according to a mass ratio of 5-7:1-3, uniformly stirring at 20-30 ℃, and then dropwise adding deionized water into the mixed system at 20-30 ℃ under the stirring condition until a clear and transparent Baili essential oil microemulsion is finally formed;
(3) According to the solid-liquid ratio =2-4:1 weighing porous cellulose active carbon and Baili essential oil microemulsion, and placing the porous cellulose active carbon and Baili essential oil microemulsion in a container for fully mixing; sealing with sealing film, maintaining at 4 deg.C for 1.5-2.5h, transferring to evaporating dish, rapidly washing with diethyl ether to remove excessive essential oil, and vacuum filtering to obtain cellulose activated carbon/Baili essential oil microemulsion complex;
(4) According to the mass ratio of 1:20-25, dissolving the cellulose activated carbon/Baili essential oil micro-emulsion compound and ethyl cellulose in absolute ethyl alcohol, and fully dissolving to prepare a coating liquid; wherein the feeding ratio of the cellulose activated carbon/Baili essential oil microemulsion compound to the absolute ethyl alcohol is 1g:20-30mL;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating amount is controlled to be 4-8g/m 2 Obtaining coated paper;
(6) The coated paper is fully dried at room temperature (preferably 23 +/-2 ℃) to obtain the antibacterial paper.
Preferably, in the step (1), weighing cellulose powder, placing the cellulose powder in a ceramic boat, and carbonizing the cellulose powder at 600 ℃ for 2 hours under the protection of argon gas to obtain a carbon source precursor; adding KOH with the same mass into a carbon source precursor, adding water for dissolving, then freeze-drying, transferring the solid obtained by freeze-drying to a ceramic boat, and adding CO 2 Under the protection of gas at 800Activating for 1h at the temperature of below, and cooling to obtain a porous cellulose activated carbon sample.
Preferably, in the step (1), the feeding ratio of the cellulose powder to the water is 15-30g:80-120mL.
Preferably, in the step (2), the surfactant RH40 and the co-surfactant Span80 are uniformly mixed at a mass ratio of 2.
Preferably, in the step (2), the mixed surfactant and the senecio oil are mixed according to the mass ratio of 7.
Preferably, in the step (2), the mixed surfactant and the Baili essential oil are mixed according to the proportion, and then stirred for 10-20min by a magnetic stirrer at the temperature of 20-30 ℃ and the speed of 400-800r/min, so that the system is uniform; then adding deionized water into the mixed system drop by drop at the temperature of 20-30 ℃ and under the stirring condition of 400-800 r/min.
Preferably, in the step (4), the mass ratio of the cellulose activated carbon/Bailey essential oil microemulsion complex to the ethyl cellulose is 1:20 mL.
In step (5) of the present invention, there is no particular requirement for the coating method as long as "uniform coating" can be achieved, and the following operations can be generally performed: the food packaging base paper is installed on a coating machine, the coating machine is fixed by a coating rod, a certain volume of coating liquid is taken from one end of the paper, and the coating machine is started to uniformly coat the coating liquid on the paper. Preferably, in the step (4), the mass ratio of the cellulose activated carbon/Bailey essential oil microemulsion complex to the ethyl cellulose is 1:20 mL; in the step (5), the amount of coating is controlled to 6g/m 2 。
By adopting the technology, compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the cellulose activated carbon with an antibacterial effect is used as a carrier, the Baili essential oil is used as an antibacterial agent, and the prepared Baili essential oil microemulsion is combined with the porous activated carbon, so that the loading capacity of the Baili essential oil microemulsion can be increased, the release time of the essential oil can be prolonged, and the slow release effect of the essential oil can be improved. Therefore, compared with the traditional antibacterial paper, the antibacterial wrapping paper has better and longer-lasting antibacterial effect.
2. According to the invention, the ethyl cellulose, the porous cellulose activated carbon and the microemulsion act together, so that the permeability of water vapor and carbon dioxide of the paper can be improved, the air permeability and the water permeability can be increased, the mechanical property of the paper can be improved, and the service life of the antibacterial paper can be prolonged.
(IV) description of the drawings
FIG. 1 is a scanning electron microscope image of cellulose activated carbon and a cellulose activated carbon/Bailey essential oil microemulsion complex prepared in examples and comparative examples.
Fig. 2 is a scanning electron microscope image of a physical image, a coating layer and the surface of the antibacterial paper prepared in the example and the comparative example.
Fig. 3 is a bacteriostatic effect diagram of the antibacterial paper prepared in the example and the comparative example on day 1 after preparation, and the three strips correspond to escherichia coli, staphylococcus aureus and penicillium citrinum from left to right in sequence.
Fig. 4 is a diagram showing the bacteriostatic effect of the antibacterial paper prepared in the examples and comparative examples at day 30 after preparation, wherein the three strips correspond to escherichia coli, staphylococcus aureus and penicillium citrinum from left to right in sequence.
Fig. 5 is a graph of water vapor transmission rates of antibacterial papers prepared in examples and comparative examples.
Fig. 6 is a graph showing carbon dioxide transmission rates of the antibacterial papers prepared in examples and comparative examples.
(V) detailed description of the preferred embodiments
In order to make the objects, technical solutions and advantages of the present application more clear, the technical solutions of the present application will be clearly and completely described below by examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
(1) 20g of cellulose powder (Shanghai Michelin Biochemical technology Co., ltd.) was weighed and placed in a ceramic boat, and high temperature carbonization was performed under argon protection for 2 hours at 600 ℃ to obtain a carbon source precursor. Adding the same mass to a precursor of a carbon sourceKOH, dissolved in 100mL water, freeze dried, the freeze dried solid transferred to a ceramic boat in CO 2 Activating under the protection of gas for 1h at 800 ℃. And cooling to obtain a porous cellulose activated carbon sample.
(2) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1, and preparing the mixed surfactant. Accurately weighing the mixed surfactant and the Baili essential oil according to the mass ratio of 7 to 3, and stirring for 15min by using a magnetic stirrer at 25 ℃ and 400r/min to ensure that the system is uniform. Dropwise adding water-phase deionized water into the mixed system at 25 ℃ under magnetic stirring at 600r/min until finally forming clear and transparent microemulsion of the Bailey essential oil.
(3) Weighing the porous cellulose activated carbon and the bailey essential oil microemulsion according to a solid-to-liquid ratio (w/v = 2) and placing the porous cellulose activated carbon and the bailey essential oil microemulsion in a conical flask for fully mixing. After sealing with a sealing film, the plate was kept at 4 ℃ for 2 hours and then transferred to an evaporation dish. And (3) washing the redundant essential oil by using ether quickly, and performing suction filtration under reduced pressure to obtain the cellulose activated carbon/Baili essential oil micro-emulsion compound.
(4) According to the mass ratio of 1:20, weighing 1g of the cellulose activated carbon/Bailey essential oil microemulsion compound and 20g of ethyl cellulose, dissolving in 20mL of absolute ethyl alcohol, and fully dissolving to prepare a coating solution;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper (purchased from Hangzhou De Sheng farmer market, inwejia Japan) with the coating amount controlled at 6g/m 2 ；
(6) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
Example 2
(1) Weighing 25g of cellulose powder, placing the cellulose powder in a ceramic boat, carrying out high-temperature carbonization under the protection of argon, and carbonizing for 2 hours at 700 ℃ to obtain a carbon source precursor. Adding KOH with the same mass into a carbon source precursor, adding 120mL of water for dissolving, freeze-drying, transferring the freeze-dried solid to a ceramic boat, and adding CO 2 Activating under the protection of gas, and activating at 850 ℃ for 1.5h. And cooling to obtain a porous cellulose activated carbon sample.
(2) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1, and preparing the mixed surfactant. Accurately weighing the mixed surfactant and the Baili essential oil according to the mass ratio of 6 to 4, and stirring for 15min by using a magnetic stirrer at 25 ℃ and 600r/min to ensure that the system is uniform. And dropwise adding the water-phase deionized water into the mixed system at 25 ℃ under the magnetic stirring of 500r/min until a clear and transparent baili essential oil microemulsion is finally formed.
(3) Weighing the porous cellulose activated carbon and the baili essential oil microemulsion according to a solid-to-liquid ratio (w/v = 3) and placing the porous cellulose activated carbon and the baili essential oil microemulsion in a conical flask for fully mixing. After sealing with a sealing film, the plate was kept at 4 ℃ for 2 hours and then transferred to an evaporation dish. And (3) rapidly washing with diethyl ether to remove redundant essential oil, and performing suction filtration under reduced pressure to obtain the cellulose activated carbon/Baili essential oil microemulsion compound.
(4) According to the mass ratio of 1:20, weighing 1g of the cellulose activated carbon/Bailey essential oil microemulsion compound and 20g of ethyl cellulose, dissolving in 20mL of absolute ethyl alcohol, and fully dissolving to prepare a coating solution;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating weight is controlled at 6g/m 2 ；
(6) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
Example 3
(1) Weighing 25g of cellulose powder, placing the cellulose powder in a ceramic boat, carrying out high-temperature carbonization under the protection of argon, and carbonizing for 2 hours at 700 ℃ to obtain a carbon source precursor. Adding KOH with the same mass into a carbon source precursor, adding 120mL of water for dissolving, freeze-drying, transferring the freeze-dried solid to a ceramic boat, and adding CO 2 Activating under the protection of gas for 1.5h at 850 ℃. And cooling to obtain a porous cellulose activated carbon sample.
(2) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1, and preparing the mixed surfactant. Accurately weighing the mixed surfactant and the Bailey essential oil according to the mass ratio of 7 to 3, and stirring for 15min at 25 ℃ and 800r/min by using a magnetic stirrer to ensure that the system is uniform. And dropwise adding water-phase deionized water into the mixed system at 25 ℃ under magnetic stirring at 600r/min until a clear and transparent microemulsion of the Bailey essential oil is finally formed.
(3) Weighing the porous cellulose activated carbon and the baili essential oil microemulsion according to the solid-to-liquid ratio (w/v = 2) and placing the porous cellulose activated carbon and the baili essential oil microemulsion in a conical flask for fully mixing. After sealing with a sealing film, the plate was kept at 4 ℃ for 2 hours and then transferred to an evaporation dish. And (3) rapidly washing with diethyl ether to remove redundant essential oil, and performing suction filtration under reduced pressure to obtain the cellulose activated carbon/Baili essential oil microemulsion compound.
(4) According to the mass ratio of 1:25, dissolving 1g of cellulose activated carbon/Bailey essential oil micro-emulsion compound and 25g of ethyl cellulose in 30mL of absolute ethyl alcohol, and fully dissolving to prepare a coating liquid;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating weight is controlled at 8g/m 2 ；
(6) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
Comparative example 1: in comparison with example 1, no ethylcellulose was added
(1) And weighing 20g of cellulose powder, placing the cellulose powder in a ceramic boat, carrying out high-temperature carbonization under the protection of argon, and carbonizing for 2 hours at 600 ℃ to obtain a carbon source precursor. Adding KOH with the same mass into a carbon source precursor, adding 100mL of water for dissolving, freeze-drying, transferring the freeze-dried solid to a ceramic boat, and adding CO 2 Activating under the protection of gas for 1h at 800 ℃. And cooling to obtain a porous cellulose activated carbon sample.
(2) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1, and preparing the mixed surfactant. Accurately weighing the mixed surfactant and the Bailey essential oil according to the mass ratio of 7 to 3, and stirring for 15min at 25 ℃ and 400r/min by using a magnetic stirrer to ensure that the system is uniform. And dropwise adding the water-phase deionized water into the mixed system at 25 ℃ under magnetic stirring at 600r/min until a clear and transparent Bailey essential oil microemulsion is finally formed.
(3) Weighing the porous cellulose activated carbon and the bailey essential oil microemulsion according to a solid-to-liquid ratio (w/v = 2) and placing the porous cellulose activated carbon and the bailey essential oil microemulsion in a conical flask for fully mixing. After sealing with a sealing film, the plate was kept at 4 ℃ for 2 hours and then transferred to an evaporation dish. And (3) rapidly washing with diethyl ether to remove redundant essential oil, and performing suction filtration under reduced pressure to obtain the cellulose activated carbon/Baili essential oil microemulsion compound.
(4) Weighing 1g of cellulose activated carbon/Bailey essential oil microemulsion compound, dissolving in 20mL of deionized water, and fully dissolving to prepare a coating solution;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating weight is controlled at 6g/m 2 ；
(6) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
From a comparison of example 1 and comparative example 1, it is clear that ethyl cellulose, acting in combination with a microemulsion, improves the permeability of the paper to water vapor and carbon dioxide and the mechanical properties of the paper.
Comparative example 2: in contrast to example 1, the essential oil microemulsion complex was not loaded on activated carbon
(1) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1 to prepare the mixed surfactant. Accurately weighing the mixed surfactant and the Bailey essential oil according to the mass ratio of 7 to 3, and stirring for 15min at 25 ℃ and 400r/min by using a magnetic stirrer to ensure that the system is uniform. Dropwise adding water-phase deionized water into the mixed system at 25 ℃ under magnetic stirring at 600r/min until finally forming clear and transparent microemulsion of the Bailey essential oil.
(2) According to the mass ratio of 1:20, weighing 1g of the Bailey essential oil microemulsion prepared in the step (1) and 20g of ethyl cellulose, dissolving in 20mL of absolute ethyl alcohol, and fully dissolving to prepare a coating liquid;
(3) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating weight is controlled at 6g/m 2 ；
(4) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
From a comparison of example 1 and comparative example 2, the antimicrobial effect of porous activated carbon (as evidenced by the data for example 1 and comparative example 2 in figure 3) and the fixation and sustained release effect of the essential oil microemulsion (as evidenced by the data for example 1 and comparative example 2 in figure 4 and table 1) are shown.
Comparative example 3:
(1) Weighing 20g of cellulose powder, placing the cellulose powder in a ceramic boat, and carrying out height increase under the protection of argonCarbonizing at a warm temperature, and carbonizing for 2h at 700 ℃ to obtain a carbon source precursor. Adding KOH with the same mass into a carbon source precursor, adding 100mL of water for dissolving, freeze-drying, transferring the freeze-dried solid to a ceramic boat, and adding CO 2 Activating under the protection of gas, and activating at 900 ℃ for 1h. And cooling to obtain a porous cellulose activated carbon sample.
(2) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1, and preparing the mixed surfactant. Accurately weighing the mixed surfactant and the Bailey essential oil according to the mass ratio of 7 to 3, and stirring for 15min at 25 ℃ and 400r/min by using a magnetic stirrer to ensure that the system is uniform. Dropwise adding water-phase deionized water into the mixed system at 25 ℃ under magnetic stirring at 600r/min until finally forming clear and transparent microemulsion of the Bailey essential oil.
(3) Weighing the porous cellulose activated carbon and the baili essential oil microemulsion according to the solid-to-liquid ratio (w/v = 2) and placing the porous cellulose activated carbon and the baili essential oil microemulsion in a conical flask for fully mixing. After sealing with a sealing film, the plate was kept at 4 ℃ for 2 hours and then transferred to an evaporation dish. And (3) rapidly washing with diethyl ether to remove redundant essential oil, and performing suction filtration under reduced pressure to obtain the cellulose activated carbon/Baili essential oil microemulsion compound.
(4) According to the mass ratio of 1:20, weighing 1g of the cellulose activated carbon/Bailey essential oil microemulsion compound and 20g of ethyl cellulose, dissolving in 20mL of absolute ethyl alcohol, and fully dissolving to prepare a coating solution;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating weight is controlled at 6g/m 2 ；
(6) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
As can be seen from the comparison of example 1 with comparative example 3, the activation temperature has an effect on the morphology of the activated carbon (comparison of example 1 and comparative example 3 in fig. 1), the antibacterial properties (as evidenced by the data of example 1 and comparative example 3 in fig. 3), and the effect on the sustained release of the essential oil microemulsion (as evidenced by the data of example 1 and comparative example 3 in fig. 4 and table 1).
Comparative example 4: compared with example 1, the variety of essential oil is changed
(1) Weighing 20g of cellulose powder, placing the cellulose powder in a ceramic boat, and carrying out high temperature treatment under the protection of argonCarbonizing for 2h at 600 ℃ to obtain the precursor of the carbon source. Adding KOH with the same mass into a carbon source precursor, adding 100mL of water for dissolving, freeze-drying, transferring the freeze-dried solid to a ceramic boat, and adding CO 2 Activating under the protection of gas, and activating at 800 ℃ for 1h. And cooling to obtain a porous cellulose activated carbon sample.
(2) Mixing the surfactant RH40 and the cosurfactant Span80 in a ratio of 2:1, and preparing the mixed surfactant. Accurately weighing the mixed surfactant and the cinnamon essential oil according to the mass ratio of 7 to 3, and stirring for 15min at 25 ℃ and 400r/min by using a magnetic stirrer to ensure that the system is uniform. Dropwise adding water-phase deionized water into the mixed system at 25 ℃ under magnetic stirring until clear and transparent cinnamon essential oil microemulsion is finally formed.
(3) Weighing the porous cellulose activated carbon and the cinnamon essential oil microemulsion according to a solid-to-liquid ratio (w/v = 2) and placing the porous cellulose activated carbon and the cinnamon essential oil microemulsion in a conical flask for fully mixing. After sealing with a sealing film, the plate was kept at 4 ℃ for 2 hours and then transferred to an evaporation dish. And (3) rapidly washing with diethyl ether to remove redundant essential oil, and performing vacuum filtration to obtain the cellulose activated carbon/cinnamon essential oil microemulsion compound.
(4) According to the mass ratio of 1:20, weighing 1g of cellulose activated carbon/cinnamon essential oil microemulsion compound and 20g of ethyl cellulose, dissolving in 20mL of absolute ethyl alcohol, and fully dissolving to prepare a coating liquid;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating weight is controlled at 6g/m 2 ；
(6) And fully drying the coated paper at room temperature (23 +/-2 ℃) to obtain the antibacterial paper.
As can be seen from comparison between example 1 and comparative example 4, the mechanical properties of the prepared paper are not greatly different, but the slow release properties and the antibacterial properties are greatly different.
The antibacterial papers prepared in the examples and comparative examples were tested by the following methods:
1. and (3) testing mechanical properties:
the paper to be tested was sampled according to GB/T450-2008 and the samples were equilibrated at 25 ℃ and 50% RH for at least 24h.
Ring crush strength: referring to GB/T2679.8-1995, the ring crush strength of paper is measured by a ring crush strength compression instrument and expressed by a ring crush strength index, and three groups of samples are taken for each sample, and an average value is taken.
Ring crush strength index Rd =1000R/W, wherein Rd represents ring crush index (N "m/g); r represents ring crush strength (kN/m); w represents the quantitative (g/m) of the sample 2 )。
Burst strength: with reference to GB/T454-2002, the burst strength of paper is measured using an electron burst tester, three sets of each sample are taken and the average is expressed in kPa.
2. Smoothness testing:
with reference to GB/T456-2002, smoothness of the paper is determined using a smoothness tester, three sets of each sample are made and the average is taken and denoted by s.
3. Determination of Water vapor Permeability and carbon dioxide Permeability
The water vapor and carbon dioxide permeability was measured using a water vapor transmission rate tester (W3/060, jinan Sike test technologies, inc.). At room temperature, the air compressor was turned on, confirming the air compressor output pressure: 0.3MPa to 0.7MPa. The instrument was opened, the sample was taken with a sampler, and the sample was cut into a size of 150mm × 95 mm. Clamping a sample by the moisture permeable cup, wherein the distance between the moisture permeable cup and the sample is about 5 mm. And putting the moisture permeable cups into a tray station of the moisture permeable cups one by one for testing. The test was repeated 5 times, and the water vapor transmission amount and the carbon dioxide transmission amount of each sample were calculated by taking an average value.
4. Essential oil release test:
the antibacterial paper was analyzed daily by gas chromatography using HP-5MS (30 m.times.0.25 μm.times.0.25 mm) as column, high purity helium as carrier gas at flow rate of 0.91mL/min, and no split-flow injection. The injection port temperature was 250 ℃ and the injection amount was 1. Mu.L. The temperature programming mode is adopted, wherein the column temperature is 80 ℃, the temperature is kept for 3min, and then the temperature is raised to 280 ℃ at the speed of 8 ℃/min, and the temperature is kept for 30min. The mass spectrum conditions comprise that the ion source temperature is 230 ℃, the interface temperature is 250 ℃, the solvent delay is 2min, the EI electron source and the electron energy are 70 ev, and the m/z scanning range is 35-500 amu.
5. Test of bacteriostatic Effect
The antibacterial effect of the antibacterial packaging paper on three test food-borne microorganisms (provided by laboratories of microbiology of Zhejiang industrial university) is tested by adopting a gas phase diffusion mode. The method comprises the steps of taking about 15mL of sterilized nutrient agar culture medium (Hangzhou microbial reagent limited) and pouring the nutrient agar culture medium into the bottom of a culture dish, coating bacterial suspension (100 mu L, the concentration is about 1.0 multiplied by 105 CFU/mL) on the culture medium, and placing a cut round antibacterial packing paper sample with the diameter of 25mm at the center of a cover of the culture dish so as to keep a gap of 8-10 mm between the antibacterial packing paper sample and the bacterial suspension. Traditional antibacterial wrapping paper (purchased from Hangzhou Desheng farmer market, inwejia, japan) is used as a control. The culture temperature of the bacteria is 37 ℃, and the culture time is 24h; the culture temperature of the mould is 28 ℃, and the culture time is 48h. 3 parts of each sample. The test is carried out on the 1 st day and the 30 th day after the antibacterial wrapping paper is prepared.
As can be seen from FIG. 1, the cellulose activated carbon prepared in example 1 is cubic, has relatively obvious edges and corners, and has uniform particle size distribution of 2-5 μm; the cellulose activated carbon/Baili essential oil micro-emulsion compound is in a more compact block shape, and the scanning electron microscope observation shows that the surface of the particles is smoother compared with the particles without the essential oil. The surface of the cellulose activated carbon prepared in example 2 generates a small amount of roughness, and the overall morphology is still good. The surface of the cellulose activated carbon prepared in example 3 generates a large amount of rough, edges and corners disappear, the particle size is obviously reduced, and the cellulose activated carbon/Baili essential oil micro-emulsion compound is generated in a small amount. Comparative example 3 the cellulose activated carbon prepared has irregular morphology and greatly reduced particle size, which may be a destructive effect of an excessively high activation temperature, and the cellulose activated carbon/Bailey essential oil microemulsion complex also exhibits severe agglomeration.
Fig. 2 shows a physical diagram and a surface coating SEM diagram of the antibacterial wrapping paper prepared in the examples and comparative examples. All examples and comparative examples had smoother surfaces but slightly different colors. This is related to the presence or absence of ethylcellulose in the coating of the antimicrobial wrapper and the amount of coating. SEM images of the coating surface show that the paper substrate has a cross section of porous fibers with a large number of irregular particle coating fillers aggregated and attached to the fibers. The filler can block part of the pore size and affect the gas permeability. After being coated with a composite coating solution prepared from a cellulose activated carbon/essential oil micro-emulsion complex and ethyl cellulose, the composite coating solution has a tendency to form a film on the paper, and the film bonds the polymeric filler to the fibers and affects the structure of the paper itself. In example 1, the polymeric filler on the cellulose activated carbon/essential oil microemulsion composite-ethyl cellulose coated paper was dispersed and distributed more uniformly on the fibers, and the paper structure remained unchanged and the polymeric filler was dispersed more uniformly compared to the other examples and comparative example coated paper. Example 3 the coating was over-coated to allow the coating filler to aggregate, and the amount of essential oil microemulsion coated with the cellulose activated carbon load in the coating of comparative example 2 was not significantly reduced.
Fig. 3 shows a bacteriostatic effect diagram of the antibacterial paper prepared in the examples and comparative examples on day 1 after preparation, and the bacteriostatic effect is represented by the diameter of the bacteriostatic circle, and the larger the diameter is, the better the bacteriostatic effect is. As can be seen from the figure, the antibacterial wrapping paper prepared by all the examples has better bacteriostatic effect. The antibacterial wrapping paper of example 1 has the best antibacterial effect, which is the coordinated effect of the vitamin activated carbon and the microemulsion of the Bailey essential oil. The Baili essential oil has the best antibacterial effect on penicillium citrinum, and the cinnamon essential oil has the best antibacterial effect on escherichia coli.
Fig. 4 shows a bacteriostatic effect pattern of the antibacterial wrapping paper prepared in examples and comparative examples at day 30 after the preparation, which reflects the antibacterial effect of the antibacterial wrapping paper. As can be seen from the figure, the antibacterial wrapping paper prepared in the example 1 still has a good antibacterial effect after being stored for 30 days, and is far higher than other wrapping papers. It is illustrated that the vitamin activated carbon in example 1 has the best sustained release effect on the microemulsion of senecio oil, which is related to the structure of the prepared vitamin activated carbon and the stability of the microemulsion of senecio oil, which is consistent with the results of fig. 1 and table 1.
FIGS. 5 and 6 show water vapor and CO of antibacterial wrapping paper prepared in each example and comparative example 2 The permeability, which reflects the air and water permeability of the wrapping paper. It can be seen from the figure that the antibacterial paper prepared in example 1 has a slightly higher water vapor transmission rate than other groups, and CO 2 The transmittance is much higher than that of other groups of antibacterial paper. Water vapor transmission rate and CO 2 The increase in transmittance is a result of the action of the coating. The essential oil microemulsion has film forming property, has certain barrier effect on water vapor and carbon dioxide, and after the ethyl cellulose is combined with the essential oil microemulsion, the film forming property is weakened, and the coating filler is combined with the fiber. When the wet coating liquid is coated on paper to expand the fibers, and after the wet coating liquid is dried, the fibers contract, the inter-fiber micropore structure is increased, the coating layer and the inter-fiber structure are loosened, and the air permeability and the water permeability of the coated paper are increased.
TABLE 1
Figure BDA0003718775530000151

Claims (8)

1. A preparation method of antibacterial paper based on porous cellulose activated carbon adsorption essential oil microemulsion is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) Weighing cellulose powder, placing the cellulose powder in a ceramic boat, and carbonizing the cellulose powder for 2 to 3 hours at a high temperature of between 500 and 700 ℃ under the protection of argon to obtain a carbon source precursor; adding KOH with the same mass into a carbon source precursor, adding water for dissolving, then freeze-drying, transferring the solid obtained by freeze-drying to a ceramic boat, and adding CO 2 Activating for 0.5-1.5h at 700-900 ℃ under the protection of gas, and cooling to obtain a porous cellulose activated carbon sample;
(2) Uniformly mixing a surfactant RH40 and a cosurfactant Span80 according to the mass ratio of 2-4; mixing a mixed surfactant and the Baili essential oil according to the mass ratio of 5-7 to 1-3, uniformly stirring at 20-30 ℃, and then dropwise adding deionized water into the mixed system at 20-30 ℃ under the stirring condition until a clear and transparent Baili essential oil microemulsion is finally formed;
(3) According to the solid-liquid ratio =2-4:1 weighing porous cellulose active carbon and Baili essential oil microemulsion, and placing the porous cellulose active carbon and Baili essential oil microemulsion in a container for fully mixing; sealing with sealing film, maintaining at 4 deg.C for 1.5-2.5h, transferring to evaporating dish, rapidly washing with diethyl ether to remove excessive essential oil, and vacuum filtering to obtain cellulose activated carbon/Baili essential oil microemulsion complex;
(4) According to the mass ratio of 1:20-25, dissolving the cellulose activated carbon/Baili essential oil micro-emulsion compound and ethyl cellulose in absolute ethyl alcohol, and fully dissolving to prepare a coating liquid; wherein the feeding ratio of the cellulose activated carbon/Baili essential oil microemulsion compound to the absolute ethyl alcohol is 1g:20-30mL;
(5) Uniformly coating the coating liquid on the surface of food packaging base paper, wherein the coating amount is controlled to be 4-8g/m 2 Obtaining coated paper;
(6) And fully drying the coated paper at room temperature to obtain the antibacterial paper.
2. The method of claim 1, wherein: weighing cellulose powder, placing the cellulose powder in a ceramic boat, and carbonizing the cellulose powder for 2 hours at 600 ℃ under the protection of argon gas to obtain a carbon source precursor; adding KOH with the same mass into a carbon source precursor, adding water for dissolving, then freeze-drying, transferring the solid obtained by freeze-drying to a ceramic boat, and reacting in CO 2 Activating for 1h at 800 ℃ under the protection of gas, and cooling to obtain a porous cellulose activated carbon sample.
3. The method of claim 1, wherein: in the step (1), the feeding ratio of the cellulose powder to the water is 15-30g:80-120mL.
4. The method of claim 1, wherein: in the step (2), the surfactant RH40 and the cosurfactant Span80 are uniformly mixed according to the mass ratio of 2.
5. The method of claim 1, wherein: in the step (2), mixing the mixed surfactant and the Bailey essential oil according to the mass ratio of 7.
6. The method of claim 1, wherein: in the step (2), mixing the mixed surfactant and the Baili essential oil according to a proportion, and stirring for 10-20min at 20-30 ℃ by using a magnetic stirrer at 400-800r/min to ensure that the system is uniform; then adding deionized water into the mixed system drop by drop at the temperature of 20-30 ℃ and under the stirring condition of 400-800 r/min.
7. The method of claim 1, wherein: in the step (4), the mass ratio of the cellulose activated carbon/Bailey essential oil microemulsion compound to the ethyl cellulose is 1:20 mL.
8. The method of claim 1, wherein: in the step (4), the mass ratio of the cellulose activated carbon/Bailey essential oil microemulsion compound to the ethyl cellulose is 1:20 mL; in the step (5), the amount of coating is controlled to 6g/m 2 。
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