CN117024805A - Preparation method and application of nano-silver modified chitosan-nano-cellulose antibacterial film - Google Patents
Preparation method and application of nano-silver modified chitosan-nano-cellulose antibacterial film Download PDFInfo
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- CN117024805A CN117024805A CN202310999340.9A CN202310999340A CN117024805A CN 117024805 A CN117024805 A CN 117024805A CN 202310999340 A CN202310999340 A CN 202310999340A CN 117024805 A CN117024805 A CN 117024805A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920002678 cellulose Polymers 0.000 title claims abstract description 15
- 239000001913 cellulose Substances 0.000 title claims abstract description 15
- 229920001661 Chitosan Polymers 0.000 claims abstract description 81
- 239000002131 composite material Substances 0.000 claims abstract description 75
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 64
- 239000001814 pectin Substances 0.000 claims abstract description 61
- 235000010987 pectin Nutrition 0.000 claims abstract description 61
- 229920001277 pectin Polymers 0.000 claims abstract description 61
- 108010010803 Gelatin Proteins 0.000 claims abstract description 25
- 239000008273 gelatin Substances 0.000 claims abstract description 25
- 229920000159 gelatin Polymers 0.000 claims abstract description 25
- 235000019322 gelatine Nutrition 0.000 claims abstract description 25
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 235000012055 fruits and vegetables Nutrition 0.000 claims abstract description 11
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013530 defoamer Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 230000004888 barrier function Effects 0.000 abstract description 8
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 230000000813 microbial effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 63
- 238000012360 testing method Methods 0.000 description 12
- 229920002749 Bacterial cellulose Polymers 0.000 description 11
- 239000005016 bacterial cellulose Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 229920002907 Guar gum Polymers 0.000 description 7
- 239000000665 guar gum Substances 0.000 description 7
- 229960002154 guar gum Drugs 0.000 description 7
- 235000010417 guar gum Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000003385 bacteriostatic effect Effects 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229920001817 Agar Polymers 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
- A23B7/154—Organic compounds; Microorganisms; Enzymes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/06—Pectin; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- 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
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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- 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
- C08K2003/0806—Silver
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a preparation method and application of a nano-silver modified chitosan-nano-cellulose antibacterial film, wherein chitosan and nano-cellulose are utilized to prepare a chitosan/nano-cellulose composite solution at first; then adding pectin solution and defoamer to prepare chitosan/nanocellulose/pectin composite solution; finally adding a gelatin solution of nano silver to obtain a nano silver modified chitosan/nano cellulose/pectin composite coating; the nano silver modified chitosan/nano cellulose/pectin composite coating film is sprayed on a tetrafluoroethylene plate and naturally dried to obtain a composite film which is biodegradable, nontoxic, edible, good in film forming property, low in cost, good in barrier property, mechanical property and antibacterial property, and can be used for fresh-keeping of fruits and vegetables and reducing microbial pollution.
Description
Technical field:
the invention relates to the technical field of food fresh-keeping film materials, in particular to a preparation method and application of a nano-silver modified chitosan-nano-cellulose antibacterial film.
The background technology is as follows:
at present, along with the improvement of the living standard of people, the quality requirements on fruits and vegetables are increased. The degradable antibacterial film material not only reduces environmental pollution, but also can maintain the quality of fruits and vegetables and prolong the shelf life of the fruits and vegetables, and becomes a research hot spot.
Chitosan has good biocompatibility and film forming property, is safe and nontoxic, and is widely applied to the fields of waste treatment, packaging, food processing and medicine, but. The pure chitosan film has the defects of low bacteriostasis, low mechanical strength, poor water resistance and the like, and the practical application is limited to a certain extent.
The invention comprises the following steps:
the invention aims to provide a preparation method and application of a nano-silver modified chitosan-nano-cellulose antibacterial film.
The invention is realized by the following technical scheme:
the preparation method of the nano-silver modified chitosan-nano-cellulose antibacterial film comprises the following steps of:
1) Preparing a chitosan/nanocellulose composite solution: dissolving nano cellulose in deionized water, uniformly dispersing by ultrasonic, adding chitosan and glacial acetic acid, adding plasticizer glycerol, and continuously stirring until the mixture is uniform to obtain a chitosan/nano cellulose composite solution;
2) Preparing a chitosan/nanocellulose/pectin composite solution: dissolving pectin in deionized water, stirring to dissolve completely, adding into chitosan/nanocellulose composite solution, mixing well, adding defoamer silicone oil, and continuing stirring until no bubbles appear to obtain chitosan/nanocellulose/pectin composite solution;
3) Preparing a gelatin solution containing nano silver: dissolving gelatin in deionized water, stirring to form a clear solution, adding silver nitrate solution, uniformly mixing, and placing in an ultraviolet camera to react to form a brown solution to obtain a gelatin solution containing nano silver;
4) Adding the nano silver gelatin solution obtained in the step 3) into the chitosan/nano cellulose/pectin composite solution obtained in the step 2), and stirring until the mixture is uniform, thus obtaining a nano silver modified chitosan/nano cellulose/pectin composite coating;
5) And (3) spraying the nano-silver modified chitosan/nano-cellulose/pectin composite coating film obtained in the step (4) on a tetrafluoroethylene plate to obtain a composite film.
Preferably, the mass ratio of the nanocellulose to the chitosan is 10:1-20:1.
Preferably, the mass concentration of nanocellulose is 5wt%.
Preferably, the mass concentration of pectin is 10-30wt%.
Preferably, the volume ratio of pectin solution to chitosan/nanocellulose is 1:1.
Preferably, the concentration of silver nitrate is 0.005M-0.01M; the mass concentration of gelatin was 0.5wt%.
Preferably, the volume ratio of the nano silver gelatin solution to the chitosan/nano cellulose/pectin composite solution is 1:1.
The invention also protects the application of the nano silver modified chitosan/nano cellulose/pectin antibacterial film obtained by the preparation method,
the film is degradable, has good antibacterial property, and can be used in the field of fruit and vegetable fresh-keeping.
The beneficial effects of the invention are as follows:
1) The raw material chitosan used in the invention is biodegradable, nontoxic, edible, has good film forming property and low cost;
2) According to the invention, the nano cellulose and pectin are added, so that the barrier property and mechanical property of the coating can be enhanced;
3) The defoaming agent used in the invention is silicone oil, so that bubbles in the composite solution are removed, and the uniformity of the film is improved;
4) The method for preparing the nano silver particles by means of the ultraviolet reduction method is simple in operation, green and safe;
5) According to the invention, the antibacterial performance of the nano silver modified chitosan/nano cellulose/pectin composite film is improved, and the nano silver modified chitosan/nano cellulose/pectin composite film is used for preserving fruits and vegetables and reducing microbial pollution.
6) The preparation method is simple in preparation process, safe and green, and can be used for mass production.
In summary, the invention utilizes chitosan and nanocellulose to prepare chitosan/nanocellulose composite solution first; then adding pectin solution and defoamer to prepare chitosan/nanocellulose/pectin composite solution; finally adding a gelatin solution of nano silver to obtain a nano silver modified chitosan/nano cellulose/pectin composite coating; the nano silver modified chitosan/nano cellulose/pectin composite coating film is sprayed on a tetrafluoroethylene plate and naturally dried to obtain a composite film which is biodegradable, nontoxic, edible, good in film forming property, low in cost, good in barrier property, mechanical property and antibacterial property, and can be used for fresh-keeping of fruits and vegetables and reducing microbial pollution.
Description of the drawings:
FIG. 1 is a graph showing the comparison of the water vapor barrier properties of the composite film materials of examples 1,2,3, and 4;
FIG. 2 is a graph showing the comparison of oxygen barrier properties of the composite film materials of examples 1,2,3, and 4;
FIG. 3 is a graph comparing tensile properties of the composite film materials of examples 1,2,3, and 4.
The specific embodiment is as follows:
the following is a further illustration of the invention and is not a limitation of the invention.
Example 1: preparation method of nano-silver modified chitosan/nano-cellulose/pectin antibacterial film
The method comprises the following steps:
1) Preparing a chitosan/nanocellulose composite solution: taking 50g of nanocellulose in 1000mL of deionized water, uniformly dispersing by ultrasonic, adding 5g of chitosan and 2mL of glacial acetic acid, adding 2mL of plasticizer glycerol, and continuously stirring until the mixture is uniformly mixed to obtain a chitosan/nanocellulose composite solution;
2) Preparing a chitosan/nanocellulose/pectin composite solution: dissolving 5g of fruit gel in 25mL of deionized water, stirring until the fruit gel is completely dissolved, adding the mixture into a chitosan/nanocellulose composite solution, uniformly mixing the mixture, and adding 2mL of silicone oil defoamer to obtain a chitosan/nanocellulose/pectin composite solution;
3) Preparing a gelatin solution containing nano silver: adding 2g of gelatin into 40mL of deionized water, stirring to form a clear solution, adding 1mL of 0.01mol/L silver nitrate solution, uniformly mixing, and placing in an ultraviolet camera to react to form a brown solution to obtain a gelatin solution containing nano silver;
4) Adding 20mL of the nano silver gelatin solution in the step 3) into 20mL of the chitosan/nano cellulose/pectin composite solution in the step 2), and stirring until the mixture is uniform, thus obtaining a nano silver modified chitosan/nano cellulose/pectin composite coating;
5) And (3) taking 20mL of nano-silver modified chitosan/nano-cellulose/pectin composite coating film, and spraying the coating film on a tetrafluoroethylene plate to obtain a composite film.
Example 2: preparation method of nano-silver modified chitosan/nano-cellulose/guar gum antibacterial film
Reference example 1 was made with the difference that guar gum was added instead of pectin.
1) Preparing a chitosan/nanocellulose composite solution: taking 50g of nanocellulose in 1000mL of deionized water, uniformly dispersing by ultrasonic, adding 5g of chitosan and 2mL of glacial acetic acid, adding 2mL of plasticizer glycerol, and continuously stirring until the mixture is uniformly mixed to obtain a chitosan/nanocellulose composite solution;
2) Preparing a chitosan/nanocellulose/guar gum composite solution: taking 5g guar gum in 25mL deionized water, stirring until the guar gum is completely dissolved, adding the guar gum into a chitosan/nanocellulose composite solution, uniformly mixing, adding 2mL silicone oil, and continuously stirring until no bubble appears in the composite solution, thereby obtaining a chitosan/nanocellulose/pectin composite solution;
3) Preparing a gelatin solution containing nano silver: adding 2g of gelatin into 40mL of deionized water, stirring to form a clear solution, adding 1mL of 0.01mol/L silver nitrate solution, uniformly mixing, and placing in an ultraviolet camera to react to form a brown solution to obtain a gelatin solution containing nano silver;
4) Adding 20mL of the nano silver gelatin solution in the step 3) into 20mL of the chitosan/nano cellulose/pectin composite solution in the step 2), and stirring until the mixture is uniform, thus obtaining a nano silver modified chitosan/nano cellulose/pectin composite coating;
5) And (3) taking 20mL of nano-silver modified chitosan/nano-cellulose/guar gum composite coating film, and spraying the coating film on a tetrafluoroethylene plate to obtain a composite film.
The test results show that the addition of pectin in example 1 improves the barrier and mechanical properties of the composite film as compared to example 1.
Example 3: preparation method of nano-silver modified chitosan/bacterial cellulose/pectin antibacterial film
Reference example 1 was made with the difference that bacterial cellulose was added instead of nanocellulose.
The method comprises the following steps:
1) Preparing a chitosan/bacterial cellulose composite solution: taking 50g of bacterial cellulose in 1000mL of deionized water, uniformly dispersing by ultrasonic, adding 5g of chitosan and 2mL of glacial acetic acid, adding 2mL of plasticizer glycerol, and continuously stirring until the mixture is uniform to obtain a chitosan/bacterial cellulose composite solution;
2) Preparing a chitosan/nanocellulose/pectin composite solution: adding 5g pectin into 25mL deionized water, stirring until the pectin is completely dissolved, adding the pectin into the chitosan/nano cellulose composite solution, uniformly mixing, adding 2mL silicone oil, and continuously stirring until no bubbles appear to obtain the chitosan/bacterial cellulose/pectin composite solution;
3) Preparing a gelatin solution containing nano silver: adding 2g of gelatin into 40mL of deionized water, stirring to form a clear solution, adding 1mL of 0.01mol/L silver nitrate solution, uniformly mixing, and placing in an ultraviolet camera to react to form a brown solution to obtain a gelatin solution containing nano silver;
4) Adding 20mL of the nano silver gelatin solution in the step 3) into 20mL of the chitosan/bacterial cellulose/pectin composite solution in the step 2), and stirring until the mixture is uniform, thus obtaining a nano silver modified chitosan/nano cellulose/pectin composite coating;
5) And (3) taking 20mL of nano-silver modified chitosan/bacterial cellulose/pectin composite coating film, and spraying the coating film on a tetrafluoroethylene plate to obtain a composite film.
The test results show that the addition of nanocellulose in example 1 improves the barrier properties and mechanical properties of the composite film over bacterial cellulose, as compared to example 1.
Example 4: preparation method of nano-silica modified chitosan/bacterial cellulose/pectin antibacterial film
Reference example 1 was different in that nano-silica was used to modify the chitosan/bacterial cellulose/pectin bacteriostatic film instead of nano-silver.
The method comprises the following steps:
1) Preparing a chitosan/nanocellulose composite solution: taking 50g of nanocellulose in 1000mL of deionized water, uniformly dispersing by ultrasonic, adding 5g of chitosan and 2mL of glacial acetic acid, adding 2mL of plasticizer glycerol, and continuously stirring until the mixture is uniformly mixed to obtain a chitosan/nanocellulose composite solution;
2) Preparing a chitosan/nanocellulose/pectin composite solution: taking 5g of pectin in 25mL of deionized water, stirring until the pectin is completely dissolved, adding the pectin into a chitosan/nanocellulose composite solution, adding 2mL of silicone oil, and uniformly mixing to obtain a chitosan/nanocellulose/pectin composite solution;
3) Adding 2g of silicon dioxide into the chitosan/nanocellulose/pectin composite solution, and stirring until the mixture is uniform to obtain a nano silicon dioxide modified chitosan/nanocellulose/pectin composite coating;
5) And (3) taking 20mL of nano silicon dioxide modified chitosan/nano cellulose/pectin composite coating film, and spraying the coating film on a tetrafluoroethylene plate to obtain a composite film.
Test results show that compared with the example 1, the addition of the nano silver silicone oil in the example 1 improves the antibacterial performance of the composite film compared with the silicon dioxide.
Example 5: performance testing
The films prepared in examples 1-4 were subjected to performance testing.
1. Water vapor transmission rate test
Cutting the film into 6-7cm diameter discs, and tightly fitting the discs with dry anhydrous CaCl 2 Is placed on a vial cup (diameter 5 cm). The film was covered on top of the vial and secured with wax. The cup was placed in a storage tank containing a saturated solution (RH 75%) at 25±1 ℃ and the mass of the cup was weighed after 24 hours. The test results are shown in FIG. 1.
Wherein the WVP of the film is calculated as follows:
WVP＝w/t×(l/A·ΔP)
w/t is a linear regression of mass and time, l is the film thickness, A is the film area, and ΔP is the partial pressure difference across the film at 25 ℃ (3169 Pa).
2. Oxygen transmission rate test
An automatic oxygen permeation instrument is adopted for testing. The results are shown in FIG. 2.
3. Mechanical property test
The test was performed using an automatic stretcher. The results are shown in FIG. 3.
5. Bacteriostasis test
Adopting Escherichia coli and Staphylococcus aureus as simulative bacteria, respectively diluting 0.1mL to 10 7 cfu/mL of escherichia coli and staphylococcus aureus suspension are respectively added into a sterile agar culture medium, so that the sterile agar culture medium is fully and uniformly mixed, a bacteriostatic film wafer with the diameter of 10mm is paved on the surface of the culture medium, the bacteriostatic effect of the film is detected, the film is cultured for 24 hours at 37 ℃, and the diameter of a bacteriostatic ring of the film is observed and recorded. The results are shown in Table 1.
TABLE 1
As can be seen from comparison of examples 1 and examples 2-4, the nano-silver modified chitosan/nano-cellulose/pectin composite film has good barrier property and antibacterial property, and is used for preserving fruits and vegetables, prolonging the shelf life of the fruits and vegetables and reducing the waste of the fruits and vegetables.
Claims (9)
1. The preparation method of the nano-silver modified chitosan-nano-cellulose antibacterial film is characterized by comprising the following steps of:
1) Dissolving nano cellulose in deionized water, uniformly dispersing by ultrasonic, adding chitosan and glacial acetic acid, adding plasticizer glycerol, and continuously stirring until the mixture is uniform to obtain a chitosan/nano cellulose composite solution;
2) Dissolving pectin in deionized water, stirring to dissolve completely, adding into chitosan/nanocellulose composite solution, mixing well, adding defoamer silicone oil, and continuing stirring until no bubbles appear to obtain chitosan/nanocellulose/pectin composite solution;
3) Dissolving gelatin in deionized water, stirring to form a clear solution, adding silver nitrate solution, uniformly mixing, and placing in an ultraviolet camera to react to form a brown solution to obtain a gelatin solution containing nano silver;
4) Adding the nano silver gelatin solution obtained in the step 3) into the chitosan/nano cellulose/pectin composite solution obtained in the step 2), and stirring until the mixture is uniform, thus obtaining a nano silver modified chitosan/nano cellulose/pectin composite coating;
5) And (3) spraying the nano-silver modified chitosan/nano-cellulose/pectin composite coating film obtained in the step (4) on a tetrafluoroethylene plate to obtain a composite film.
2. The preparation method according to claim 1, wherein the mass ratio of nanocellulose to chitosan is 10:1-20:1.
3. The preparation method according to claim 1, wherein the mass concentration of the nanocellulose is 5wt%.
4. The preparation method according to claim 1, wherein the mass concentration of pectin is 10-30wt%.
5. The method of claim 1, wherein the volume ratio of pectin solution to chitosan/nanocellulose is 1:1.
6. The method according to claim 1, wherein the concentration of silver nitrate is 0.005M to 0.01M.
7. The preparation method according to claim 1, wherein the mass concentration of the gelatin is 5wt%.
8. The method of claim 1, wherein the volume ratio of the nanosilver gelatin solution to the chitosan/nanocellulose/pectin composite solution is 1:1.
9. The application of the nano-silver modified chitosan/nano-cellulose/pectin antibacterial film obtained by the preparation method of claim 1, which is characterized by being applied to the field of fruit and vegetable fresh-keeping.
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