CN115678070A - Preparation and application of AgNPs composite film - Google Patents
Preparation and application of AgNPs composite film Download PDFInfo
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- CN115678070A CN115678070A CN202211558380.1A CN202211558380A CN115678070A CN 115678070 A CN115678070 A CN 115678070A CN 202211558380 A CN202211558380 A CN 202211558380A CN 115678070 A CN115678070 A CN 115678070A
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Images
Classifications
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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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- Manufacture Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for preparing and applying AgNPs composite film, belonging to the technical field of packaging material, comprising the following steps: the wormwood residue after the wormwood essential oil is extracted is subjected to water bath, wormwood extracting solution is further extracted and obtained, the extracting solution is used as a template agent, nano silver (AgNPs) is prepared by adopting a green synthesis method, a composite film is prepared by the nano silver (AgNPs), sodium alginate and starch, the composite film is subjected to characterization such as mechanical property and opacity, the tensile strength of the AgNPs composite film with the content of 0.027 wt% reaches 12.04 MPa, structural analysis and microscopic morphology observation are carried out on the AgNPs composite film by adopting technologies such as SEM and the like, then the antioxidant performance of the composite film is tested, the antioxidant capacity reaches 64.1% when the content of the AgNPs reaches 0.027 wt%, finally the composite film is used for storing small tomatoes, 28 d is stored at 4 ℃, the content of small total phenols in the AgNPs composite film with the content of 9.45 zxft 3763/g is only reduced by 19.8%, and the mildew does not occur, and the fresh-keeping capacity of the AgNPs composite film is proved.
Description
The technical field is as follows:
the invention belongs to the technical field of packaging materials, and particularly relates to preparation and application of an AgNPs composite film.
Background art:
film packaging is an economical and effective way to protect food from contamination, so that the amount of packaging film used in human life is increasing. However, films made of chemically synthesized polymers are difficult to degrade, generate a large accumulation of solid waste, and white pollution is increasingly aggravated, thereby causing environmental problems. As a solution, the faster decomposition rate of biodegradable films compared to petroleum-based synthetic films has attracted attention. Shortening the degradation time of the film can reduce the generation of waste and is beneficial to environmental protection. Biodegradable films are mostly made from carbohydrate-based raw materials, such as starch and proteins, including whey protein isolates and natural polysaccharides. The sodium alginate has unique biological, chemical and physical properties, and can be used in wound dressing. Silver nanoparticles are known for their powerful antimicrobial activity, incorporating antimicrobial properties into polymers with excellent biocompatibility, rendering the polymers antimicrobial, which is a promising application.
At present, there are few reports of composite films prepared by AgNPs, sodium alginate and potato starch. Chinese patent CN114031911A discloses a degradable bio-based film material and a preparation method thereof, common straws in China villages are used as main raw materials, and the composite bio-based material is easy to obtain raw materials, good in degradability, excellent in mechanical property and wide in application. Chinese patent CN114015211A discloses a full-degradable antibacterial food packaging film and a preparation method thereof, wherein biodegradable ester, hydrophilic colloid, antibacterial nano-particles and other raw materials are fed in a segmented manner, and after one-step extrusion granulation, the packaging film is obtained through extrusion blow molding, so that the degradable film is endowed with a good antibacterial effect. Chinese patent CN114044941A discloses a preparation method of a green degradable composite film, which solves the problems of poor water resistance, poor film forming property, poor mechanical property, poor water resistance and the like of a single starch film.
Based on the invention, firstly, the wormwood residue after extraction of essential oil is subjected to water bath extraction, wormwood extract is obtained through filtration, and the wormwood extract is used for preparing nano-silver AgNPs through green reduction of silver nitrate. Composite films were prepared by AgNPs together with sodium alginate and also potato starch. And then, various basic performances, oxidation resistance and fresh-keeping application of the composite film are tested, and at present, no report or patent exists for preparing AgNPs and then preparing the composite film through the wormwood residue extracting solution. Compared with the traditional method for preparing the composite film, the method increases the comprehensive utilization of the wormwood, and has the advantages of good environmental protection, stable mechanical property of the product, higher opacity, oxidation resistance, fresh-keeping capability and the like.
The invention content is as follows:
the invention aims to provide preparation and application of AgNPs composite film. The AgNPs preparation method is simple, the process is green and environment-friendly, and large-scale production can be realized; the prepared composite film is smooth and flat, has high opacity and excellent mechanical property, has oxidation resistance, is applied to the field of preservation, and also improves the comprehensive utilization of wormwood resources.
The invention comprises the following steps:
1. green synthesis of AgNPs
Drying the wormwood residue after the wormwood essential oil is extracted, weighing 10-500 g of wormwood residue powder, pouring the wormwood residue powder into a beaker, adding 100-1000 mL of deionized water, heating in a water bath at 70-95 ℃ for 1-3 h to obtain an extracting solution, and filtering and concentrating to obtain the wormwood residue extracting solution. Taking 5 to 20 mL of wormwood extracting solution and 5 to 20 mL of 1 to 10 mmol/L AgNO 3 Mixing the solution, pouring the mixture into a beaker, sealing and stirring at room temperature for 1 to 3 hours to prepare AgNPs solution, and storing the AgNPs solution at the temperature of 4 ℃;
2. preparation of AgNPs composite film
Preparing an AgNPs composite film, firstly weighing 1-3 g of sodium alginate, dissolving in 50-200 mL of deionized water, then dripping 0-10 mL of AgNPs solution, stirring and heating at 50-80 ℃ for 1-3 h; secondly, weighing 1 to 5 g of starch, dissolving the starch in 50 to 200 mL of deionized water, heating the solution in a water bath at 85 ℃ for 5 min, and dripping 1 to 3 mL of glycerol; mixing the solutions, stirring and heating at 50-80 ℃ for 5-20 min, carrying out ultrasonic treatment for 10-30 min, carrying out vacuum air extraction for 3-10 min, pouring the mixture on a polytetrafluoroethylene film-forming plate, drying in an oven at 40 ℃ for 12-24 h, and storing under a constant temperature condition.
3. Composite film performance characterization and applications
(1) Carrying out absorbance and opacity tests on the composite film by using an ultraviolet-visible spectrophotometer;
(2) Carrying out a water vapor transmission rate test on the composite film;
(3) And (4) carrying out mechanical property test and oxidation resistance test on the composite film.
(4) The composite film is applied to preservation.
Description of the drawings:
FIG. 1 is a scanning electron micrograph of the composite film.
FIG. 2 is a Fourier transform infrared spectrum of the composite film.
FIG. 3 is the opacity of the composite film.
FIG. 4 is a schematic diagram of the mechanical properties of the composite film.
FIG. 5 is a schematic diagram of the oxidation resistance of the composite film.
FIG. 6 is a schematic view of the preservation application of the composite film.
The specific implementation mode is as follows:
the technical solutions provided by the present invention are described in detail below with reference to examples, and it should be understood that the following detailed description is only illustrative and not intended to limit the scope of the present invention.
Example 1: green synthetic AgNPs and preparation of composite film thereof
(1) Drying the wormwood residue after the wormwood essential oil is extracted, weighing 100 g wormwood residue powder, pouring the powder into a beaker, adding 100 mL deionized water, heating in a water bath at 95 ℃, extracting for 2 h to obtain an extracting solution, and filtering and concentrating to obtain the wormwood residue extracting solution. Taking 10 mL wormwood extract and 10 mL 10 mmol/L AgNO 3 Mixing the solution, pouring the mixture into a beaker, sealing and stirring at room temperature for 2 h to prepare AgNPs solution, and storing at 4 ℃;
(2) Preparing an AgNPs composite film, firstly weighing sodium alginate 1.5 g, dissolving in 100 mL deionized water, then dripping 2 mL of AgNPs solution, stirring and heating at 60 ℃ for 1 h; secondly, weighing 2.5 g starch, dissolving in 50 mL deionized water, heating in a water bath at 85 ℃ for 5 min, and dripping 2 mL glycerol; mixing the solutions, stirring and heating at 50 deg.C for 10 min, performing ultrasonic treatment for 30 min, vacuum pumping for 5 min, pouring on a polytetrafluoroethylene film-forming plate, oven drying in an oven at 40 deg.C for 12 h, and storing at constant temperature.
Example 2: characterization and test of various basic performances of AgNPs composite film
(1) The AgNPs composite film prepared in example 1 is tested by UV-visible spectrophotometer for absorbance and opacity at wavelength 550 nm, the increase in AgNPs content increases the opacity, the opacity of 0.000 wt% AgNPs composite film is 3.39 mm -1 0.027 wt% AgNPs opacity reaches 7.07 mm -1 The opacity of the AgNPs composite film is increased, so that the food is prevented from being irradiated by sunlight, the food oxidation can be effectively inhibited, and the loss of the nutritional value of the food is reduced;
(2) Water Vapor Permeability (WVP) is an important selection parameter for food storage antioxidant films. The minimal WVP films reduce water transport through the food product, thereby extending the shelf life of the food product. The WVP reduction was significant for all AgNPs films compared to the control film (p < 0.05). 0.054 wt% AgNPs film WVP was lowest, 37.4% lower than control. The addition of AgNPs fills the structural gaps existing in the sodium alginate potato starch, so that the channel and the way of water transportation through the film are blocked, and the WVP of the composite film is reduced along with the increase of the content of the AgNPs. 0.027 The AgNPs film with the weight percent has no obvious change with the AgNPs film WVP with the weight percent of 0.054 wt percent, and the AgNPs film with the weight percent of 0.027 wt percent is more suitable for being applied to the market from the viewpoint of saving materials;
(3) And (3) testing the mechanical properties of the composite film, measuring the tensile strength and the elongation at break of the film in an electronic universal material testing machine, cutting the composite film into 150 mm X10 mm strips, and fixing two ends of the composite film by a clamping hand of the electronic universal material testing machine to enable the film to stretch naturally. The test speed was set to 50 mm/min. Each group of tests was averaged 3 times;
(4) Antioxidant testing and fresh-keeping application of the composite film, DPPH freeFirstly, respectively cutting films 2 multiplied by 2 cm with different AgNPs contents into 20 mL absolute ethyl alcohol to be used as film sample liquid; secondly, adding the prepared film sample solution 3.0 mL and the prepared DPPH solution 3.0 mL into each test tube, shaking up in dark environment and keeping out of the sun for 0.5 h, testing and zeroing by using absolute ethyl alcohol, and measuring the absorbance of the mixed solution to be A; then adding the film sample solution 3.0 mL and absolute ethyl alcohol 3.0 mL into a new test tube, carrying out light-shielding treatment, and testing to obtain the absorbance A 0 (ii) a Finally, 3.0 mL of DPPH solution and 3.0 mL absolute ethyl alcohol are shaken and mixed evenly, and the absorbance A is obtained by testing 1 The test wavelength of the above experiment was 517 nm; the performance of the active films was evaluated by their antioxidant effect on the storage of small tomatoes. A sample bag was prepared by wrapping two small tomatoes with a test film of size 200 mm x 150 mm. The analysis used sodium alginate starch composite films and AgNPs (0.013 wt%,0.027 wt%) composite films. The samples were stored in a refrigerator at 4 ℃ for 28 d. Small tomato samples were removed from the stored specimen bags on days 1, 7, 14, 21 and 28 for analysis of total phenolic content. All measurements were performed in triplicate and averaged.
FIG. 1 is a scanning electron micrograph of the composite film showing that the AgNPs film composite film of 0.027 wt% is smooth and uniform.
FIG. 2 shows a Fourier transform infrared spectrum of the composite film at 3300 cm for a sodium alginate composite film -1 Stretching vibration of left and right hydroxyl groups (-OH), the peak moves to low frequency, the peak intensity is increased, and the intermolecular hydrogen bond is formed; from the spectrum, the AgNPs composite film is 1601 cm relative to the sodium alginate-starch composite film -1 And 1408 cm -1 The absorption peak is enhanced by asymmetric stretching and symmetric stretching vibration peaks, and the silver nanoparticles and hydroxyl-COO-form metal ion coordination bonds, so that the vibration peak moves to low frequency, and the fact that the metal coordination bonds are introduced into the composite film on the basis of hydrogen bonds is shown, and AgNPs are presumed to be successfully doped into the composite film.
FIG. 3 is an opacity chart of a composite film, increasing the opacity of an AgNPs composite filmThe food is prevented from being irradiated by sunlight, the food oxidation can be effectively inhibited, and the loss of the food nutritive value is reduced. And testing the opacity and absorbance of the AgNPs composite film by using an ultraviolet-visible spectrophotometer. The opacity of the sodium alginate/starch film and the 0.027 wt% AgNPs composite film is 3.35 mm respectively at a wavelength of 550 nm -1 、7.07 mm -1 The AgNPs are shown to increase the opacity of the composite film, reduce the light transmittance of the composite film and be more beneficial to food preservation.
FIG. 4 is a graph showing the mechanical properties of the composite film, 0.000 wt% of the tensile strength of the AgNPs composite film of 5.64 MPa, and 0.027 wt% of the tensile strength of the AgNPs film of 12.04 MPa.
Fig. 5 is a graph showing the oxidation resistance of the composite film, which shows that the DDPH radical scavenging rate of the AgNPs film of 0.027 wt% reaches 64.1%.
Fig. 6 is a schematic diagram of the application of the composite film in preservation, small tomatoes preserved by three films on the first day have no change, and have no obvious change even after the seventh day, and can be found to have obvious changes on the 28 th day, two small tomatoes have obvious mildew under the preservation of the film of pure sodium alginate starch, relatively speaking, only one small tomato added with the composite film of 0.013 wt% AgNPs has weak mildew, while the small tomatoes added with the composite film of 0.027 wt% AgNPs have no mildew, and show good preservation capability.
In conclusion, the wormwood residue after the wormwood essential oil is extracted is subjected to water bath to further extract a wormwood extracting solution, the extracting solution is used as a template agent, nano silver (AgNPs) is prepared by adopting a green synthesis method, a composite film is prepared by the nano silver (AgNPs), sodium alginate and starch, the composite film is characterized by mechanical property, opacity and the like, the tensile strength of the AgNPs composite film with the content of 0.027 wt% reaches 12.04 MPa, the AgNPs composite film is subjected to structural analysis and microscopic morphology observation by adopting technologies such as FT-IR, SEM and the like, then the oxidation resistance of the composite film is tested, when the content of the AgNPs reaches 0.027 wt%, the oxidation resistance reaches 64.1%, finally, the composite film is stored for a small time, the content of small tomatoes in the composite film with the content of 28 d at 4 ℃ and the content of small tomatoes in the AgNPs composite film with the weight% is 9.45 zxft 3763/g and is only reduced by 19.8%, and the freshness keeping capability of the tomatoes are all proved.
Claims (3)
1. The preparation method of the AgNPs composite film is characterized by comprising the following steps:
drying the wormwood residue after the wormwood essential oil is extracted, weighing 10-500 g of wormwood residue powder, pouring the wormwood residue powder into a beaker, adding 100-1000 mL of deionized water, heating in a water bath at 70-95 ℃ for 1-3 h to obtain an extracting solution, and filtering and concentrating to obtain the wormwood residue extracting solution.
2. Taking 5 to 20 mL of wormwood extracting solution and 5 to 20 mL of 1 to 10 mmol/L AgNO 3 Mixing the solution, pouring the mixture into a beaker, sealing and stirring at room temperature for 1 to 3 hours to prepare AgNPs solution, and storing the AgNPs solution at the temperature of 4 ℃; preparing an AgNPs composite film, firstly, dissolving 1 to 3 g of sodium alginate in 50 to 200 mL of deionized water, then dripping 0 to 10 mL of AgNPs solution, stirring and heating at 50 to 80 ℃ for 1 to 3 hours; secondly, weighing 1 to 5 g of starch, dissolving the starch in 50 to 200 mL of deionized water, heating the solution in a water bath at the temperature of 85 ℃ for 5 min, and dripping 1 to 3 mL of glycerol; mixing the solutions, stirring and heating at 50-80 ℃ for 5-20 min, carrying out ultrasonic treatment for 10-30 min, carrying out vacuum air extraction for 3-10 min, pouring the mixture on a polytetrafluoroethylene film-forming plate, drying in an oven at 40 ℃ for 12-24 h, and storing under a constant temperature condition.
3. The AgNPs composite film prepared according to claim 1 is tested and analyzed, characterized by comprising the steps of:
carrying out absorbance and opacity tests by using an ultraviolet-visible spectrophotometer; carrying out a water vapor transmission rate test on the composite film; performing characterization on the composite film by using a microscope, a scanning electron microscope, fourier transform infrared and thermogravimetric analysis; the method comprises the following steps of (1) performing mechanical performance on a composite film, measuring the tensile strength and the elongation at break of the film in an electronic universal material testing machine, cutting the composite film into 150 mm x 10 mm strips, fixing two ends of the composite film by a clamp of the electronic universal material testing machine to enable the film to stretch naturally, setting the testing speed to be 10-100 mm/min, taking an average value for 3 times of each group of tests, and performing oxidation resistance testing and fresh-keeping application on the AgNPs composite film prepared in the claim 1, wherein the method is characterized by comprising the following steps of:
the DPPH free radical scavenging capacity experimental method comprises the steps of firstly, respectively cutting films with different AgNPs contents 2X 2 cm, dissolving the films in 10-100 mL of absolute ethyl alcohol to serve as film sample liquid, then adding 1.0-5.0 mL of prepared film sample liquid and 1.0-5.0 mL of prepared DPPH solution into each test tube, shaking uniformly in a dark environment and keeping dark for 0.5-2 hours, testing and zeroing by using absolute ethyl alcohol, and measuring the absorbance of a mixed solution to be A; then adding 1.0-5.0 mL of film sample liquid and 1.0-5.0 mL of absolute ethyl alcohol into a new test tube, processing in the dark similarly, and testing to obtain the absorbance A 0 (ii) a Finally, 1.0 to 5.0 mL of DPPH solution and 1.0 to 5.0 mL of absolute ethanol are shaken and mixed, and the absorbance A is obtained by testing 1 The test wavelength of the above experiment was 517 nm; the evaluation of the properties of the composite films was carried out by their antioxidant effect on the storage of small tomatoes, by preparing sample bags by wrapping two small tomatoes with a test film of 200 mm × 150 mm size, analyzing using a sodium alginate starch composite film and an AgNPs (0.013 to 0.108 wt%) composite film, storing the samples in a refrigerator at 4 ℃ for 28 days, taking out small tomato samples from the stored sample bags on days 1 to 28 to analyze their total phenolic content, and taking the average of all measurements in triplicate.
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| CN116515175A (en) * | 2023-04-11 | 2023-08-01 | 东莞东美食品有限公司 | Oxidized starch and preparation method thereof |
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| CN111085693A (en) * | 2019-12-31 | 2020-05-01 | 云南大学 | Synthetic AgNPs and preparation method of transplantable self-assembled film thereof |
| CN113667157A (en) * | 2021-08-24 | 2021-11-19 | 安徽大学绿色产业创新研究院 | Preparation method of functional folium artemisiae argyi polysaccharide composite film |
| CN113693124A (en) * | 2021-08-05 | 2021-11-26 | 河南工业大学 | Rosa roxburghii polysaccharide nano-silver compound and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111085693A (en) * | 2019-12-31 | 2020-05-01 | 云南大学 | Synthetic AgNPs and preparation method of transplantable self-assembled film thereof |
| CN113693124A (en) * | 2021-08-05 | 2021-11-26 | 河南工业大学 | Rosa roxburghii polysaccharide nano-silver compound and preparation method and application thereof |
| CN113667157A (en) * | 2021-08-24 | 2021-11-19 | 安徽大学绿色产业创新研究院 | Preparation method of functional folium artemisiae argyi polysaccharide composite film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116515175A (en) * | 2023-04-11 | 2023-08-01 | 东莞东美食品有限公司 | Oxidized starch and preparation method thereof |
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