GB2622753A - Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof - Google Patents
Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof Download PDFInfo
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- GB2622753A GB2622753A GB2400498.8A GB202400498A GB2622753A GB 2622753 A GB2622753 A GB 2622753A GB 202400498 A GB202400498 A GB 202400498A GB 2622753 A GB2622753 A GB 2622753A
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- silver
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- oxidized nanocellulose
- chitosan
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- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 70
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 46
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 36
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 36
- 230000002335 preservative effect Effects 0.000 title claims abstract description 30
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 28
- 239000003755 preservative agent Substances 0.000 title claims abstract description 28
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 229910052709 silver Inorganic materials 0.000 title abstract description 4
- 239000004332 silver Substances 0.000 title abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229960000583 acetic acid Drugs 0.000 claims abstract description 12
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 20
- 239000012031 Tollens' reagent Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 238000009210 therapy by ultrasound Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000000502 dialysis Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 240000009088 Fragaria x ananassa Species 0.000 claims description 10
- 235000003953 Solanum lycopersicum var cerasiforme Nutrition 0.000 claims description 10
- 240000003040 Solanum lycopersicum var. cerasiforme Species 0.000 claims description 10
- 238000010345 tape casting Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000005923 long-lasting effect Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007970 homogeneous dispersion Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 235000016623 Fragaria vesca Nutrition 0.000 claims description 3
- 235000011363 Fragaria x ananassa Nutrition 0.000 claims description 3
- 235000010149 Brassica rapa subsp chinensis Nutrition 0.000 claims description 2
- 235000000536 Brassica rapa subsp pekinensis Nutrition 0.000 claims description 2
- 241000499436 Brassica rapa subsp. pekinensis Species 0.000 claims description 2
- 240000008067 Cucumis sativus Species 0.000 claims description 2
- 240000008415 Lactuca sativa Species 0.000 claims description 2
- 235000003228 Lactuca sativa Nutrition 0.000 claims description 2
- 235000009812 Momordica cochinchinensis Nutrition 0.000 claims description 2
- 240000008790 Musa x paradisiaca Species 0.000 claims description 2
- 235000018290 Musa x paradisiaca Nutrition 0.000 claims description 2
- 244000183278 Nephelium litchi Species 0.000 claims description 2
- 235000009818 Trichosanthes kirilowii Nutrition 0.000 claims description 2
- 235000009754 Vitis X bourquina Nutrition 0.000 claims description 2
- 235000012333 Vitis X labruscana Nutrition 0.000 claims description 2
- 240000006365 Vitis vinifera Species 0.000 claims description 2
- 235000014787 Vitis vinifera Nutrition 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- VUZNLSBZRVZGIK-UHFFFAOYSA-N 2,2,6,6-Tetramethyl-1-piperidinol Chemical group CC1(C)CCCC(C)(C)N1O VUZNLSBZRVZGIK-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 11
- 238000004321 preservation Methods 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000001186 cumulative effect Effects 0.000 abstract description 2
- 230000003100 immobilizing effect Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- 230000001668 ameliorated effect Effects 0.000 abstract 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 abstract 1
- 238000005266 casting Methods 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 230000002045 lasting effect Effects 0.000 abstract 1
- 230000005764 inhibitory process Effects 0.000 description 12
- 241000894006 Bacteria Species 0.000 description 7
- 235000021012 strawberries Nutrition 0.000 description 7
- 241000588722 Escherichia Species 0.000 description 6
- 241000191967 Staphylococcus aureus Species 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 241000191940 Staphylococcus Species 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 230000002147 killing effect Effects 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/24—Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
- B65D81/28—Applications of food preservatives, fungicides, pesticides or animal repellants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
- C08B15/04—Carboxycellulose, e.g. prepared by oxidation with nitrogen dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/10—Crosslinking of cellulose
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
- C08L1/04—Oxycellulose; Hydrocellulose, e.g. microcrystalline cellulose
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- 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 present invention belongs to the field of functional materials, and relates to a preparation method for a silver-loaded TEMPO oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and the use thereof. The preparation method comprises: uniformly dispersing TEMPO oxidized nanocellulose, and adding a silver-ammonia solution thereto, so as to obtain a TEMPO oxidized nanocellulose, which immobilizes nano-silver, under microwave conditions; and dissolving chitosan in glacial acetic acid, adding the silver-loaded oxidized nanocellulose thereto, and using a casting evaporation method to prepare the TEMPO oxidized nanocellulose/chitosan composite film, which immobilizes nano-silver. In the present invention, the TEMPO oxidized nanocellulose is used as a reducing agent, a stabilizing agent and an immobilizing agent, such that no chemical reducing agent or stabilizing agent is added; the reduction efficiency is high, the cost is low, and toxicity is avoided; the microwave-assisted catalysis efficiency is high, and the energy consumption is low; and the immobilization effect of the nano-silver is improved by means of the film-forming property of the chitosan, such that the problem of cumulative toxicity caused by excessively fast release of the nano-silver is ameliorated, and the nano-silver is applied to the field of lasting antibacterial preservation of fruits and vegetables.
Description
PREPARATION METHOD AND USE OF SILVER-LOADED TEMPO-OXIDIZED NANOCELLULOSE/CHITOSAN ANTIBACTERIAL PRESERVATIVE FILM FOR FRUIT AND VEGETABLE PACKAGING [00011 The present application claims priority to the Chinese Patent Application No. CN202310006473.], filed to the China National Intellectual Property Administration (CNIPA) on January 4, 2023 and entitled "PREPARATION METHOD AND USE OF SILVER-LOADED TEMPO-OXIDIZED NANOCELLULOSE/CHITOSAN ANTIBACTERIAL PRESERVATIVE FILM FOR FRUIT AND VEGETABLE PACKAGING", all content of which is incorporated by reference herein in its entirety.
TECHNICAL FIELD
[0002] The present disclosure belongs to the field of functional materials, and specifically relates to a method for preparing a nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan long-lasting antibacterial preservative film, which may be used in fruit and vegetable packaging and other related fields.
BACKGROUND
[0003] The disclosure of the information for this background section is merely for the purpose of facilitating the understanding of the overall background of the present disclosure and is not necessarily to be regarded as an acknowledgment or any form of implication that the information constitutes the prior art already known to those of ordinary skill in the art.
[0004] With the continuous improvement of people's living standards, the expansion of demand for the quality of fruits and vegetables and the excessive use of non-degradable fossil products have caused the continuous deterioration of the ecological environment. One of the important challenges facing humans is to develop a degradable and pollution-free antibacterial preservative material system while maintaining the quality of fruits and vegetables. Film packaging is one of the common technologies used to maintain the post-harvest quality of fruits and vegetables while extending shelf life, having the advantages of low cost, simple operation, and wide applicability. Moreover, film packaging is a commonly used preservation and storage material for fruits and vegetables. However, traditional film materials generally have the disadvantages of low porosity and poor effect, as well as non-biodegradability, which is not conducive to environmental protection. In addition, traditional film materials cannot actively kill microorganisms such as bacteria, and cannot alleviate decay and deterioration. As a result, the microorganisms such as bacteria multiply during the preservation process, causing large amounts of losses. In view of this, it is necessary to improve the antibacterial activity and fresh-keeping effect of preservative film materials for fruits and vegetables by using a green, efficient, and degradable method.
SUMMARY
[00051 In order to solve the above problems, the present disclosure proposes a long-lasting antibacterial composite preservative film for fruit and vegetable packaging and a preparation method and use thereof The composite preservative film has obvious antibacterial and fresh-keeping effects, excellent mechanical and physical properties, simple operation, environmental friendliness, and biodegradability.
[0006] To achieve the above object, the present disclosure adopts the following technical solutions: [0007] A first aspect of the present disclosure provides a method for preparing a nano-silver-immobilized 2,2,6,6-tetramethylpiperidin-l-oxyl (TEMPO)-oxidized nanocellulose /chitosan antibacterial preservative film for fruit and vegetable packaging, including: [0008] uniformly dispersing a TEMPO-oxidized nanocellulose, and mixing with a Tollens' reagent uniformly to obtain a mixed solution; [0009] subjecting the mixed solution to a reaction under a microwave condition, and removing unreacted Tollens' reagent by dialysis after the reaction is completed to obtain a nano-silver-immobilized TEMPO-oxidized nanocellulose and [0010] dissolving chitosan in a glacial acetic acid solution, mixing with the nano-silver-immobilized TEMPO-oxidized nanocellulose to obtain a mixture, subjecting the mixture to homogeneous dispersion and ultrasonic treatment in sequence to obtain a mixed liquid, placing the mixed liquid in a mold by a tape casting evaporation method, and drying to obtain the nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging; [0011] wherein a ratio of a mass of the chitosan to a volume of the nano-silver-immobilized IEMPO-oxidized nanocellulose is in a range of (0.1-0.3) g: (2-10) mL [0012] Nano-silver is a kind of nano-level metallic silver elemental with broad-spectrum antibacterial properties. Nano-silver shows desirable inhibitory and killing effects on more than 40 common pathogenic microorganisms such as Staphylococcus aureus, Escherichia coil, and Pseudomonas aeruginosa. TEMPO-oxidized nanocellulose is a green, renewable, and environmentally friendly biomass resource, contains a large number of reducing functional groups in its molecular chain, and can be greenly and efficiently reduced to prepare precious metal nano-silver without the addition of chemical reducing agents. Moreover, the TEMPO-oxidized nanocellulose can be immobilized in situ by relying on a long-chain structure of the fiber itself, and can also be compounded with chitosan, which has desirable film-forming properties, to form an antibacterial preservative film, thereby exhibiting broad application prospects. The method has low energy consumption, simple operation, green environmental protection, high yield, uniform product, low equipment requirements and large-scale producti on.
[0013] A second aspect of the present disclosure provides a nano-silver-immobilized IEWO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging prepared by the above method.
[0014] A third aspect of the present disclosure provides use of the above nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging in long-lasting, antibacterial, and fresh-keeping packaging of fruit and vegetable, wherein the fruit and vegetable includes one or more selected from the group consisting of strawberry, litchi, grape, banana, cherry tomato, lettuce, Chinese cabbage, and cucumber.
[0015] The present disclosure has the following beneficial effects: [0016] (1) In the present disclosure, the TEMPO-oxidized nanocellulose is used as a reducing agent, stabilizer, and immobilizing agent without the addition of any chemical reducing agent or stabilizer. The method has simple operation, environmental friendliness, high reduction efficiency, low cost, and no toxicity.
[0017] (2) In the present disclosure, the method assisted by microwave has high catalytic efficiency, desirable reduction effect, and low energy consumption.
[0018] (3) In the present disclosure, the film-forming properties with the help of chitosan can further improve the immobilization effect of nanopart cies, achieve secondary immobilization, reduce the rapid release of nano-silver, and solve the cumulative toxicity, thereby making the nano-silver be applied in the field of long-lasting and antibacterial preservation of fruit and vegetable
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The accompanying drawings, which constitute a part of the present disclosure, are used to provide a further understanding of the present disclosure, and the illustrative embodiments of the present disclosure and the description thereof are used to explain the present disclosure and are not to be construed as unduly limiting the present disclosure.
[0020] FIG. I_ shows an electron microscope image of the nano-silver-immobilized TEMPO-oxidized nanocellulose (a) and nano-silver (b).
[0021] FIG. 2 is a graph showing the inhibition zone effects of different composite films on Staphylococcus aureus and E,scherichia colt, as well as a scanning electron microscopy (SEM) image for comparing before and after killing the two bacteria; wherein panel (a) represents Staphylococcus aureus, panel (d) represents Eschericlua coil, panel (b) represents normal Staphylococcus cutreus, panel (c) represents Staphylococcus aurens killed by the composite film, panel (e) represents normal Escherichia cob, and panel (f) represents Escherichia colt killed by the composite film [0022] FIG. 3 is a graph showing the preservative effects of different composite films on cherry tomatoes.
[0023] FIG. 4 is a graph showing the preservative effects of different composite films on strawberries.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0024] It should be pointed out that the following detailed description is illustrative and is intended to provide a further description of the present disclosure. Unless otherwise specified, all technical and scientific terms used in the present disclosure have the same meaning as commonly understood by one of ordinary skill in the technical field to which the present disclosure belongs.
[0025] The present disclosure provides a method for preparing a nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use of the nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging in long-lasting, antibacterial, and fresh-keeping of fruit and vegetable. The method includes: uniformly dispersing a certain amount of a TEMPO-oxidized nanocellulose, mixing with a quantitative amount of Tollens' reagent and stirring thoroughly; placing a resulting mixed solution in a microwave reactor and reacting, placing a reaction product in a dialysis bag, and removing unreacted Tollens' reagent by dialysis after the reaction is completed to obtain a nano-silver-immobilized TEMPO-oxidized nanocellulose; and dissolving a certain amount of chitosan in a glacial acetic acid solution, mixing with a quantitative amount of the nano-silver-immobilized TEMPO-oxidized nanocellulose to obtain a mixture, subjecting the mixture to homogeneous dispersion in a homogenizer and ultrasonic treatment in sequence, placing a mixed liquid obtained after the ultrasonic treatment in a mold by a tape casting evaporation method, and drying to obtain the nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging.
[0026] In some embodiments, the method specifically includes the following steps: [0027] (1) Preparation of the nano-silver-immobilized TEMPO-oxidized nanocellulose: 1 g to 5 g of a TEMPO-oxidized nanocellulose is added to 100 mL of deionized water, uniformly dispersed with a homogenizer, then mixed with a 0.025 M to 0.3 M Tollens' reagent in a mass ratio of 5: 2, and stirred uniformly with a glass rod to obtain a mixed liquid. The mixed liquid is placed in a microwave reactor and reacted for 20 min to 60 min at a power of 600 W to 1,000 W and a temperature of 40°C to 100°C. After the reaction is completed, the unreacted silver ions are removed by dialysis to obtain the nano-silver-immobilized ILMPO-oxidized nanocellulose.
[0028] (2) Preparation of the nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging: 0.5 g to 1.5 g of chitosan is dissolved in 100 mL of a 0.1 wt% glacial acetic acid solution, stirred with the homogenizer for 2 min until the chitosan is completely dissolved, immediately mixed with 10 mL to 50 mL of the nano-silver-immobilized TEMPO-oxidized nanocellulose obtained in step (1), and mixed with the homogenizer uniformly to obtain a mixture. The mixture is subjected to ultrasonic treatment. A mixed solution obtained after the ultrasonic treatment is placed in a mold by a tape casting evaporation method, and dried to obtain the nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging.
[0029] According to the demand for antibacterial preservative film materials for the final fruit and vegetable packaging, the antibacterial performance (taking the antibacterial effect on Staphylococcus aureus and Escherichia con as an example) and the fresh-keeping performance (taking the preservation effect on cherry tomato and strawberry as an example) of the composite film are mainly tested. The initial dosage of the TEMPO-oxidized nanocellulose, the addition amount of the Tollens' reagent, and the concentration of chitosan can be adjusted according to different actual conditions.
[0030] In some embodiments, a nanocellulose used in the TEMPO-oxidized nanocellulose is a cellulose nanofibril (CNF) that is prepared by a TEMPO-oxidation method and has a carboxyl content of 1.4 mmol/L to 1.6 mmol/L.
[0031] In some embodiments, 1 g to 5 g of the TEMPO-oxidized nanocellulose is added to 100 mL of a deionized solution.
[0032] In some embodiments, the Tollens' reagent has a concentration of 0.025 M to 0.3 M. [0033] In some embodiments, a mass ratio of the TEMPO-oxidized nanocellulose solution to the Tollens' reagent is in a range of 5: (2-3).
[0034] In some embodiments, the TEMPO-oxidized nanocellulose is fully and uniformly mixed with the Tollens' reagent under the action of glass rod stirring.
[0035] In some embodiments, the IEWO-oxidized nanocellulose and the Tollens' reagent are mixed uniformly, and then reacted under stirring in the microwave reactor.
[0036] In some embodiments, the microwave reactor has a power of 600 W to 1,000 W, and the reaction is conducted at a temperature of 40°C to 100°C for 20 min to 60 min. [0037] In some embodiments, the dialysis is conducted for 48 h to 72 h to ensure complete precipitation of unreacted Toll ens' reagent.
[0038] In some embodiments, 0.5 g to 1.5 g of the chitosan is dissolved in 100 mL of the glacial acetic acid solution with a concentration of 0.1 wt% to 0.15 wt%.
[0039] In some embodiments, the chitosan solution and the IEMPO-oxidized nanocellulose solution are mixed, the homogenizer has a power of 500 W to 600 W, and the homogeneous is conducted at room temperature for 2 min to 3 min. [0040] In some embodiments, the homogeneous mixed solution is subjected to ultrasonic treatment at a power of 1,200W to 1,300 W and a temperature of 18°C to 20°C for 15 mm to 20 min. [0041] In some embodiments, the drying is conducted by drying the mold containing the mixed liquid in an oven at a temperature of 38°C to 40°C for 11 h to 12 h. 100421 The present disclosure will be further described below in detail with reference to specific examples, and it should be pointed out that the specific examples are an explanation of the present disclosure, not a limitation.
[0043] In the following examples, the inhibition zone test adopts existing methods in the industry with specific reference to the following papers: [0044] 1.http s://doi org/10 1016/j. indcrop.2020. 112987.
[0045] 2.https://doi.org/10.1016/j.cej.2021.129815.
[0046] 3.http s://doi.org/10.1016/j.msec.2020.111012.
[0047] Example 1:
[0048] 1 g of a LEMPO-oxidized nanocellulose was added to 100 mL of deionized water, uniformly dispersed with a homogenizer, and then mixed with a 0.025 M Tollens' reagent in a mass ratio of 5: 2, and the resulting mixture was stirred uniformly with a glass rod, obtaining a mixed liquid. The mixed liquid was placed in a three-neck flask, then placed in a microwave reactor, and reacted for 60 min at a power of 1,000 W and 100°C. After the reaction was completed, the unreacted Tollens' reagent was removed by dialysis for 48 h, obtaining a nano-silver-immobilized IEMPO-oxidized nanocellulose. 0.5 g of chitosan was dissolved in 100 mL of a glacial acetic acid solution with a concentration of 0.1 wt%, and stirred with the homogenizer for 2 min until chitosan was completely dissolved, obtaining a mixture. The mixture was subjected to ultrasonic treatment. The mixed solution obtained after the ultrasonic treatment was placed in a mold by a tape casting evaporation method, and dried, obtaining a nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging.
[0049] The prepared composite film produces an inhibition zone with a diameter of 2.21 mm against Staphylococcus allre71.5 and an inhibition zone with a diameter of 1.30 mm against Escherichia coll. The prepared composite film could preserve fresh cherry tomatoes for up to 9 days and fresh strawberries for up to 4 days.
[0050] Example 2:
[0051] 2 g of a TEMPO-oxidized nanocellulose was added to 100 mL of deionized water, uniformly dispersed with a homogenizer, and then mixed with a 0.05 M Tollens' reagent in a mass ratio of 5: 2, and the resulting mixture was stirred uniformly with a glass rod, obtaining a mixed liquid. The mixed liquid was placed in a three-neck flask, then placed in a microwave reactor, and reacted for 40 min at a power of 800 W and 80°C. After the reaction was completed, the unreacted Toliens' reagent was removed by dialysis for 48 h, obtaining a nano-silver-immobilized TEWO-oxidized nanocellulose. 1 g of chitosan was dissolved in 100 ml. of a glacial acetic acid solution with a concentration of 0.1 wt%, and stirred with the homogenizer for 2 min until chitosan was completely dissolved, obtaining a mixture. The mixture was subjected to ultrasonic treatment. The mixed solution obtained after the ultrasonic treatment was placed in a mold by a tape casting evaporation method, and dried, obtaining a nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging.
[0052] The prepared composite film produces an inhibition zone with a diameter of 2.85 mm against Staphylococcus alums and an inhibition zone with a diameter of 1.80 mm against Eycherichia colt The prepared composite film could preserve fresh cherry tomatoes for up to 10 days, and fresh strawberries for up to 4 days.
[0053] Example 3:
[0054] 3 g of a TEMPO-oxidized nanocellulose was added to 100 mL of deionized water, uniformly dispersed with a homogenizer, and then mixed with a 0.1 M Tollens' reagent in a mass ratio of 5: 2, and the resulting mixture was stirred uniformly with a glass rod, obtaining a mixed liquid. The mixed liquid was placed in a three-neck flask, then placed in a microwave reactor, and reacted for 30 min at a power of 800 W and 60°C. After the reaction was completed, the unreacted Toliens' reagent was removed by dialysis for 72 h, obtaining a nano-silver-immobilized TEMPO-oxidized nanocellulose. 1.5 g of chitosan was dissolved in 100 mL of a glacial acetic acid solution with a concentration of 0.1 wt%, and stirred with the homogenizer for 2 min until chitosan was completely dissolved, obtaining a mixture. The mixture was subjected to ultrasonic treatment. The mixed solution obtained after the ultrasonic treatment was placed in a mold by a tape casting evaporation method, and dried, obtaining a nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging.
[0055] The prepared composite film produces an inhibition zone with a diameter of 4.58 mm against Staphylococcus aureus and an inhibition zone with a diameter of 2.50 mm against Eycherichia colt The prepared composite film could preserve fresh cherry tomatoes for up to 12 days, and fresh strawberries for up to 6 days.
[0056] FTG. 1 shows an electron microscope image of the n ano-si 1 ver-i m m obi I ized TEMPO-oxidized nanocellulose (a) and the prepared nano-silver (b); wherein the inset in panel (a) represents the particle size distribution of the nano-silver.
[0057] It can be seen that the nano-silver is uniformly attached to the nanocellulose fibers, with a relatively uniform particle size.
[0058] FIG. 2 is a graph showing the inhibition zone effects of different composite films on Staphylococcus aurezts and Escherichia colt, as well as an electron microscopy image for comparing before and after killing the two bacteria. As shown in FIG. 2, the composite film has a significant inhibitory effect on the two kinds of bacteria and produces an obvious inhibition zone. Compared with the appearance of the bacteria before killing (round and smooth), the bacteria after lulling becomes shriveled and incomplete.
100591 FIG. 3 and FIG. 4 are graphs showing the preservation effects of different composite films on fresh cherry tomatoes and strawberries. As shown in FIG. 3 and FIG. 4, the composite film has a desirable fresh-keeping effect on the cherry tomatoes and strawberries, which basically maintained a complete, fresh, and shiny state after 12 days and 6 days, respectively, with no mildew or volume shrinkage.
[0060] Example 4:
[0061] 5 g of a TEMPO-oxidized nanocellulose was added to 100 mL of deionized water, uniformly dispersed with a homogenizer, and then mixed with a 0.2 M Toliens reagent in a mass ratio of 5: 2, and the resulting mixture was stirred uniformly with a glass rod, obtaining a mixed liquid. The mixed liquid was placed in a three-neck flask, then placed in a microwave reactor, and reacted for 20 min at a power of 600 W and 40°C. After the reaction was completed, the unreacted Toliens' reagent was removed by dialysis for 72 h, obtaining a nano-silver-immobilized TEMPO-oxidized nanocellulose. 1.5 g of chitosan was dissolved in 100 mL of a glacial acetic acid solution with a concentration of 0.1 wt%, and stirred with the homogenizer for 2 min until chitosan was completely dissolved, obtaining a mixture. The mixture was subjected to ultrasonic treatment. The mixed solution obtained after the ultrasonic treatment was placed in a mold by a tape casting evaporation method, and dried, obtaining a nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging.
[0062] The prepared composite film produces an inhibition zone with a diameter of 4.10 mm against Staphylococcus aureus and an inhibition zone with a diameter of 2.10 mm against Eycherichia colt The prepared composite film could preserve fresh cherry tomatoes for up to 10 days, and fresh strawberries for up to 5 days.
[0063] The above descriptions are merely preferred embodiments of the present disclosure and are not intended to limit the present disclosure. It should be noted that for a person of ordinary skill in the art, the present disclosure can be variously modified and changed. Any modification, equivalent substitution, improvement, etc. within the spirit and principles of the present disclosure shall fall within the scope of protection of the present disclosure.
Claims (1)
- WHAT IS CLAIMED IS: 1. A method for preparing a nano-silver-immobilized 2,2,6,6-tetramethylpiperidin-1 -oxyl (TEMPO)-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, comprising: uniformly dispersing a TEMPO-oxidized nanocellulose, and mixing with a Tollens' reagent uniformly to obtain a mixed solution; subjecting the mixed solution to a reaction under a microwave condition, and removing unreacted Tollens' reagent by dialysis after the reaction is completed to obtain a nano-silver-immobilized TEMPO-oxidized nanocellulose; and dissolving chitosan in a glacial acetic acid solution, mixing with the nano-silver-immobilized IEMPO-oxidized nanocellulose to obtain a mixture, subjecting the mixture to homogeneous dispersion and ultrasonic treatment in sequence to obtain a mixed liquid, placing the mixed liquid in a mold by a tape casting evaporation method, and drying to obtain the nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging; wherein a ratio of a mass of the chitosan to a volume of the nano-silver-immobilized TEMPO-oxidized nanocellulose is in a range of (0.1-0.3) g: (2-10) mL 2. The method of claim 1, wherein a nanocellulose used in the TEMPO-oxidized nanocellulose is a cellulose nanofibril that is prepared by a TEMPO-oxidation method and has a carboxyl content of 1.4 mmol/L to 1.6 mmol/L 3. The method of claim 1, wherein uniformly dispersing the TEMPO-oxidized nanocellulose is conducted by adding I g to 5 g of the TEMPO-oxidized nanocellulose into 100 mL of deionized water, and uniformly dispersing with a homogenizer to obtain a TEMPO-oxidized nanocellulose solution.4. The method of claim 1, wherein the Tollens' reagent has a concentration of 0.025 M to 0.3 5. The method of claim 1 or 4, wherein a mass ratio of the I EMPO-oxidized nanocellulose solution to the Tollens' reagent is in a range of 5: (2-3).6. The method of claim 1, wherein the microwave condition refers to a power of 600 W to 1,000W and a temperature of 40°C to 100°C, and the reaction is conducted for 20 min to 60 min. 7. The method of claim 1, wherein the dialysis is conducted for 48 h to 72 h. 8. The method of claim 1, wherein the glacial acetic acid solution has a concentration of 0.1 wt% to 0.15 wt%, and a ratio of the mass of the chitosan to a volume of the glacial acetic acid solution is in a range of (0.5-1.5) g: 100 mL 9. The method of claim 1, wherein the homogeneous dispersion is conducted at a power of 500 W to 600W by stirring at room temperature for 2 min to 3 min. 10. The method of claim 1, wherein the ultrasonic treatment is conducted at a power of 1,200 W to 1,300 W and a temperature of 18°C to 20°C for 15 min to 20 min. 11. The method of claim 1, wherein the drying is conducted by drying the mold containing the mixed liquid in an oven at a temperature of 38°C to 40°C for 11 h to 12 h. 12. A nano-silver-immobilized TEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging prepared by the method of any one of claims 1 to 11.13. Use of the nano-silver-immobilized LEMPO-oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging of claim 12 in long-lasting, antibacterial, and fresh-keeping packaging of fruit and vegetable, wherein the fruit and vegetable comprises one or more selected from the group consisting of strawberry, litchi, grape, banana, cherry tomato, lettuce, Chinese cabbage, and cucumber.
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| PCT/CN2023/120961 WO2024012609A2 (en) | 2023-01-04 | 2023-09-25 | Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof |
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| CN117304559A (en) * | 2023-10-27 | 2023-12-29 | 齐鲁工业大学(山东省科学院) | Preparation method and application of antibacterial fresh-keeping composite sponge |
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