CN109776869A - A kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, preparation method and application - Google Patents
A kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, preparation method and application Download PDFInfo
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- CN109776869A CN109776869A CN201811642398.3A CN201811642398A CN109776869A CN 109776869 A CN109776869 A CN 109776869A CN 201811642398 A CN201811642398 A CN 201811642398A CN 109776869 A CN109776869 A CN 109776869A
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Abstract
The present invention discloses a kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane and preparation method thereof.The present invention uses grape seed extract to prepare nano silver for reducing agent, and oxidation nanometer cellulose is the fixed nano silver of template, and the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer is prepared；Then using oxidation nanometer cellulose as film forming matrix, grape seed extract is antioxidant, and glycerol is plasticiser, mixes with the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer, the composite membrane is made.The preparation of nano silver in composite membrane obtained is 0.6-6wt%, can be applied to food packaging, and will not reveal, be overflowed into food as the nano-Ag particles of antibacterial action, greatly reduces its toxicity and potential hazard in food applications；And the composite membrane possesses antioxidation, can prevent the oxidative rancidity of the food such as lipid, meets the requirement of modern food active packing.
Description
Technical field
The present invention relates to packaging material for food fields, and in particular to the food packaging cellulose fixed nanometer of oxidation nanometer
Silver/grape seed extract antibacterial, anti-oxidant composite membrane and the preparation method and application thereof.
Background technique
In recent years, people have been devoted to find that a kind of antibacterial, antioxidant activity is high, barrier property is strong and environmentally friendly food
Product packaging material, to meet the requirement of modern food active packing, thus helping to extend the food storage phase, improving food storage
The pollution to environment can be reduced while hiding environment.
Cellulose is a kind of natural polysaccharide with designability, nontoxic, degradable, in Living Packaging Materials in Foodstuff field
It has potential application, is especially received through being aoxidized obtained by the oxidation of 2,2,6,6- tetramethyl piperidine nitrogen oxides (TEMPO)
Rice cellulose.The oxidation nanometer cellulose membrane transparency is high, intensity is good and has good thermal stability, but there is nothings
Disadvantage anti-oxidant, antibacterial activity is poor is not able to satisfy the requirement of modern food active packing, and application is by a degree of limit
System.
Silver nano-grain is a kind of broad spectrum activity antibacterial material, has very strong antibacterial activity, can be used as reinforcing agent and be added to
In oxidation nanometer cellulose composite membrane, enhance the antibacterial activity of composite membrane.But there is researcher to find nano silver to the person in recent years
Body has certain potential cumulative toxicity.When nano silver is added in packaging film as antibacterial agent, people are big in use
The leakage of the free silver nano-grain of amount, can cause to damage to human body.
In recent years, various bioactive substances are used for anti-oxidant reinforcing agent.The biology extracted from agricultural wastes is living
Property ingredient in active food packaging application receive the extensive concern of people, such as grape seed extract.It is reported that annual Portugal
A large amount of grape pip leftover bits and pieces is generated in grape liquor industry, and in these substances anthocyanidin or Polyphenols activity rich at
Point.The active component has very strong antioxidation, can be used in food storage, to prevent the oxidation of food from declining
It loses.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to a kind of food packaging multifunctional composite film is provided,
It is specially nontoxic and have antibacterial, antioxidant activity, the cellulose fixed nano silver of oxidation nanometer oxidation nanometer cellulose multiple
Close film.
The object of the invention is also to provide a kind of cellulose fixed nano silver of oxidation nanometer/grape pips to extract
The preparation method of object antibacterial, anti-oxidant composite membrane.The preparation method uses grape seed extract to prepare nano silver for reducing agent, warp
The oxidation nanometer cellulose that TEMPO is aoxidized is the fixed nano silver of template, and nano silver composite antibacterial agent is prepared；Then with
Oxidation nanometer cellulose is film forming matrix, and grape seed extract is film properties reinforcing agent, and glycerol is plasticiser, compound with nano silver
Antibacterial agent mixing, prepares oxidation nanometer cellulose/grape seed extract/nano silver composite antibacterial, oxidation resistanct fresh-keeping film.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation side of the cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane
Method, TEMPO aoxidize to obtain oxidation nanometer cellulose, molten using grape seed extract reduction-oxidation nano-cellulose solution and silver-colored ammonia
The mixed liquor of liquid, prepares the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer, then with grape seed extract solution, glycerol
And the mixing of oxidation nanometer cellulose mixed solution, prepare oxidation nanometer cellulose base that is nontoxic and having antibacterial, antioxidant activity
Composite membrane specifically comprises the following steps:
(1) firstly, being aoxidized referring to Denilson et al. (Biomacromolecules, 2003,4,1417-1425) with TEMPO
Carboxyl-content is obtained as the oxidation nanometer cellulose of 0.93mmol/g, under stirring condition, it is fine that oxidation nanometer is added in silver ammino solution
It ties up and is uniformly mixed in plain solution, obtain oxidation nanometer cellulose-silver ammonia mixed solution；
(2) at room temperature, grape pip is added into oxidation nanometer cellulose described in step (1)-silver ammonia mixed solution to mention
Take object solution, reacted, by the obtained cellulose fixed nano-ag composite of oxidation nanometer of reaction with ultrapure water dialyse to
Inspection does not measure silver ion, obtains the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer；
(3) under agitation, glycerol and grape seed extract solution are added into oxidation nanometer cellulose solution, adds step
Suddenly the cellulose fixed nano silver composite antibacterial agent of (1) described oxidation nanometer is uniformly mixed, drying and forming-film；
(4) film is taken off, the food packaging oxidation nanometer cellulose/grape seed extract/immobilization nanometer silver antimicrobial is obtained, resists
Oxidation compound film.
Further, in step (1), the concentration of the silver ammino solution is 0.01-1 mol/L.
Further, in step (1), the concentration of the oxidation nanometer cellulose solution is 0.5-30 g/L.
Further, in step (1), the mixed volume ratio of the silver ammino solution and oxidation nanometer cellulose solution is 1:4-
1:40。
Further, in step (2), the concentration of the grape seed extract solution is 0.5-10 g/L.
Further, in step (2), the additional amount of the grape seed extract solution is the 1%- for accounting for reaction total volume
10%。
Further, in step (2), the time of the reaction is 5-60 min.
Further, in step (3), in the oxidation nanometer cellulose solution, the mass fraction of oxidation nanometer cellulose
For 0.2-4%.
Further, in step (3), the grape seed extract is relative to the mass fraction of oxidation nanometer cellulose
0.1-10%。
Further, in step (3), the glycerol is 20-30% relative to the mass fraction of oxidation nanometer cellulose.
Further, in step (3), matter of the immobilization nano silver composite antibacterial agent relative to oxidation nanometer cellulose
Amount score is 0.1-2%.
Further, in step (3), the temperature of the drying and forming-film is 30-60 DEG C.
Cellulose fixed nano silver/the grape seed extract of the oxidation nanometer as made from above-mentioned preparation method is multi-functional compound
In film, the releasing ratio of nano silver is 0.6-6 wt%.
The present invention is using nano silver as antibacterial agent, and antibacterial effect is good, range is wide, solves oxidation nanometer cellulose packaging film
Antibacterial activity is weak, the unstable problem of effect；There is carboxylic group abundant on oxidation nanometer cellulose molecular chain, is received using oxidation
The chelation of rice cellulose and metal ion effectively solves free so that metal ion is fixed on cellulose skeleton surface
The problem of silver nano-grain causes potential hazard to human body；Using grape seed extract antioxidation, it is fine to solve oxidation nanometer
The problem of composite membrane is without antioxidant activity is tieed up, and can be used as the green reducing agent in nano silver synthesis process；Have composite membrane
Have a unique physical and chemical performance and excellent biological antibiotic, antioxidant activity, expand oxidation nanometer cellulose food fresh keeping antibacterial,
The application of anti-oxidation field.
The cellulose fixed nano silver of the oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane can be applied to
In food packaging.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) oxidation nanometer cellulose and grape seed extract that the present invention uses, source is wide, at low cost, safe and non-toxic, and performance
Stablize；
(2) present invention is acted on using oxidation nanometer cellulose adsorption of immobilization, fixed nano-Ag particles, then fine with oxidation nanometer
The prepared oxidation nanometer cellulose/grape seed extract/nano silver composite membrane of dimension element mixing for food packaging, it is fresh-keeping in
When, the preparation of the nano-Ag particles as antibacterial action is only 0.6-6wt%, will not largely reveal, overflow into food
In product, its toxicity in food applications is greatly reduced, reduces and human body is caused potentially hazardous, expanded nano silver work
The application for being antibacterial agent in food fresh keeping；Grape seed extract as antioxidation has strong antioxidant effect, and
Antioxidant activity is lasting, meets the requirement of modern food active packing；
(3) preparation method simple process of the present invention, raw material sources are wide, and low energy consumption, are conducive to large-scale industrial production；
(4) the cellulose fixed nano silver of oxidation nanometer of the invention/grape pip antibacterial, in anti-oxidant composite membrane, nano silver
Preparation is only 0.6-6wt%, and has good antibacterial, antioxidant effect, be can be applied in food packaging.
Detailed description of the invention
Accumulation of the nano silver under condition of different pH in the oxidation nanometer cellulose base composite membrane that Fig. 1 obtains for embodiment 2
Release rate result figure.
Fig. 2 is that the oxidation nanometer cellulose base composite membrane that embodiment 2 obtains is anti-to staphylococcus aureus and Escherichia coli
The diameter data figure of the experiment inhibition zone of bacterium.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiments and drawings, but the present invention is implemented
Example and protection scope are without being limited thereto.
Embodiment 1
The preparation of the cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, specific steps are such as
Under:
(1) oxidation nanometer cellulose is obtained using TEMPO oxidation nanometer cellulose, configuration concentration is the oxidation nanometer of 0.5 g/L
It is molten that the silver-colored ammonia that 1 mL concentration is 0.01 mol/L is added in cellulose solution into 40 mL oxidation nanometer cellulose solutions under stirring
Liquid is uniformly mixed；
(2) at room temperature, in the mixed solution obtained to step (1), the totality that 1%(is added relative to reaction solution is integrated
Number) grape seed extract solution that concentration is 0.5 g/L, the reaction was continued 5 min fix obtained oxidation nanometer cellulose
Change nano-ag composite, which is dialysed, does not measure silver ion to inspection, obtains the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer；
(3) extraction of 0.1% grape pip is added in the oxidation nanometer cellulose solution that configuration quality score is 0.2% thereto under stirring
Object solution and 20% glycerol plasticiser (mass fraction relative to oxidation nanometer cellulose)；
(4) the cellulose fixed nano silver composite antibacterial agent of 0.1% oxidation nanometer is added into mixed solution obtained by (3) under stirring
(mass fraction relative to oxidation nanometer cellulose) is uniformly mixed, and drying and forming-film at 30 DEG C takes off film, obtains oxidation nanometer fibre
Tie up plain immobilization nano silver/grape seed extract antibacterial, anti-oxidant composite membrane.
Embodiment 2
The preparation of the cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, specific steps are such as
Under:
(1) oxidation nanometer cellulose is obtained using TEMPO oxidation nanometer cellulose, configuration concentration is the oxidation nanometer of 2.5 g/L
It is molten that the silver-colored ammonia that 2 mL concentration are 0.5 mol/L is added in cellulose solution into 40 mL oxidation nanometer cellulose solutions under stirring
Liquid is uniformly mixed；
(2) at room temperature, in the mixed solution obtained to step (1), total volume of the 7.5%(relative to reaction solution is added
Score) grape seed extract solution that concentration is 1 g/L, the reaction was continued 30 min fix obtained oxidation nanometer cellulose
Change nano-ag composite, which is dialysed, does not measure silver ion to inspection, obtains the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer；
(3) the oxidation nanometer cellulose solution that configuration quality score is 1%, it is molten to be added 5% grape seed extract thereto under stirring
Liquid and 25% glycerol plasticiser (mass fraction relative to oxidation nanometer cellulose)；
(4) the cellulose fixed nano silver composite antibacterial agent of 0.5% oxidation nanometer is added into mixed solution obtained by (3) under stirring
(mass fraction relative to oxidation nanometer cellulose) is uniformly mixed, and drying and forming-film at 45 DEG C takes off film, obtains oxidation nanometer fibre
Tie up plain immobilization nano silver/grape seed extract antibacterial, anti-oxidant composite membrane.
Nano silver is tired in the cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane
Product release rate result figure, as shown in Figure 1.As shown in Figure 1, it is discharged 14 days under the conditions of pH 4, pH 6.9,9.2 pH, oxidation is received
The release rate of nano silver is lower in the cellulose fixed nano silver/grape seed extract composite membrane of rice, respectively only 5.77%,
3.62%, 3.11%, illustrate that oxidation nanometer cellulose has good immobilization efficiency to nano silver, overflowing for nano silver can be prevented
Out, it leaks.
The cellulose fixed nano silver of the oxidation nanometer of preparation/grape seed extract antibacterial, anti-oxidant composite membrane are to golden yellow
The diameter data figure of the experiment inhibition zone of color staphylococcus and Escherichia coli antibacterial, as shown in Figure 2.As shown in Figure 2, prepared
The cellulose fixed nano silver of oxidation nanometer/grape seed extract composite membrane to staphylococcus aureus and Escherichia coli have compared with
Good antibacterial effect, illustrating the cellulose fixed nano silver of oxidation nanometer, there is no the antibacterial effects for reducing nano silver；Without
The composite membrane of addition immobilization nano silver does not show antibacterial effect.
The antioxygen of the cellulose fixed nano silver of the oxidation nanometer of preparation/grape seed extract antibacterial, anti-oxidant composite membrane
Change activity experimental data table, as shown in table 1.As shown in Table 1, the cellulose fixed nano silver/grape of prepared oxidation nanometer
Seed extract composite membrane is the every milliequivalent ascorbic acid of 6.87 μ g to DPPH free radical capture ability and catches to TRAP free radical
Capacitation power is the every milliequivalent watermiscible vitamin E of 82.67 μ g, illustrates that prepared composite membrane has good anti-oxidant work
Property.
The anti-oxidant work of the cellulose fixed nano silver of 1 oxidation nanometer of table/grape seed extract antibacterial, anti-oxidant composite membrane
Property
| DPPH ( μg Vc/mg dw) | TRAP (μg Trolox/mg dw) | |
| Oxidation nanometer cellulose/grape seed extract/nano silver composite membrane | 6.87±0.04 | 82.67±0.93 |
Embodiment 3
The preparation of the cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, specific steps are such as
Under:
(1) oxidation nanometer cellulose is obtained using TEMPO oxidation nanometer cellulose, the oxidation nanometer that configuration concentration is 10 g/L is fine
Plain solution is tieed up, the silver ammino solution that 5 mL concentration are 0.6 mol/L is added under stirring into 40 mL oxidation nanometer cellulose solutions,
It is uniformly mixed；
(2) at room temperature, in the mixed solution obtained to step (1), the totality that 9%(is added relative to reaction solution is integrated
Number) grape seed extract solution that concentration is 5 g/L, the reaction was continued 40 min are cellulose fixed by obtained oxidation nanometer
Nano-ag composite, which is dialysed, does not measure silver ion to inspection, obtains the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer；
(3) the oxidation nanometer cellulose solution that configuration quality score is 2%, it is molten to be added 8% grape seed extract thereto under stirring
Liquid and 28% glycerol plasticiser (mass fraction relative to oxidation nanometer cellulose)；
(4) the cellulose fixed nano silver composite antibacterial agent of 1.5% oxidation nanometer is added into mixed solution obtained by (3) under stirring
(mass fraction relative to oxidation nanometer cellulose) is uniformly mixed, and drying and forming-film at 50 DEG C takes off film, obtains oxidation nanometer fibre
Tie up plain immobilization nano silver/grape seed extract antibacterial, anti-oxidant composite membrane.
Embodiment 4
The preparation of the cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, specific steps are such as
Under:
(1) oxidation nanometer cellulose is obtained using TEMPO oxidation nanometer cellulose, the oxidation nanometer that configuration concentration is 30 g/L is fine
Plain solution is tieed up, the silver ammino solution that 10 mL concentration are 1 mol/L is added under stirring into 40 mL oxidation nanometer cellulose solutions, mixes
It closes uniform；
(2) at room temperature, in the mixed solution obtained to step (1), total volume of the 10%(relative to reaction solution is added
Score) grape seed extract solution that concentration is 10 g/L, the reaction was continued 60 min consolidate obtained oxidation nanometer cellulose
Surely change nano-ag composite, which is dialysed, does not measure silver ion to inspection, obtains the cellulose fixed nano silver composite antibacterial of oxidation nanometer
Agent；
(3) the oxidation nanometer cellulose solution that configuration quality score is 4%, it is molten to be added 10% grape seed extract thereto under stirring
Liquid and 30% glycerol plasticiser (mass fraction relative to oxidation nanometer cellulose)；
(4) the cellulose fixed nano silver composite antibacterial agent (phase of 2% oxidation nanometer is added into mixed solution obtained by (3) under stirring
For the mass fraction of oxidation nanometer cellulose), it is uniformly mixed, drying and forming-film at 60 DEG C takes off film, obtains oxidation nanometer cellulose
Immobilization nano silver/grape seed extract antibacterial, anti-oxidant composite membrane.
Above embodiments are only preferrred embodiment of the present invention, for explaining only the invention, are not intended to limit the present invention, this
Field technical staff should belong to guarantor of the invention without departing from change made under spirit of the invention, replacement, modification etc.
Protect range.
Claims (8)
1. a kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, the preparation method of anti-oxidant composite membrane,
It is characterized by comprising the following steps:
(1) under stirring condition, it is equal that mixing in the oxidation nanometer cellulose solution aoxidized through TEMPO is added in silver ammino solution
It is even, obtain oxidation nanometer cellulose-silver ammonia mixed solution；
(2) at room temperature, grape pip is added into oxidation nanometer cellulose described in step (1)-silver ammonia mixed solution to mention
Object solution is taken, is reacted, the cellulose fixed nano-ag composite of oxidation nanometer is obtained, it is dialysed with ultrapure water to detection
Do not go out silver ion, obtains the cellulose fixed nano silver composite antibacterial agent of oxidation nanometer；
(3) under agitation, glycerol and grape seed extract solution are added into oxidation nanometer cellulose solution, adds step
Suddenly the cellulose fixed nano silver composite antibacterial agent of (2) described oxidation nanometer is uniformly mixed, drying and forming-film；
(4) film is taken off, the oxidation nanometer cellulose/grape seed extract/immobilization nanometer silver antimicrobial, anti-oxidant compound is obtained
Film.
2. preparation method according to claim 1, which is characterized in that in step (1), the concentration of the silver ammino solution is
0.01-1 mol/L；The concentration of the oxidation nanometer cellulose solution is 0.5-30 g/L；The silver ammino solution and oxidation nanometer
The mixed volume ratio of cellulose solution is 1:4-1:40.
3. preparation method according to claim 1, which is characterized in that in step (2), the grape seed extract solution
Concentration is 0.5-10 g/L；The additional amount of the grape seed extract solution accounts for the 1%-10% of reaction total volume.
4. preparation method according to claim 1, which is characterized in that in step (2), the time of the reaction is 5-60
min。
5. preparation method according to claim 1, which is characterized in that in step (3), the oxidation nanometer cellulose solution
In, the mass fraction of oxidation nanometer cellulose is 0.2-4%.
6. preparation method according to claim 1, which is characterized in that in step (3), the glycerol is relative to oxidation nanometer
The mass fraction of cellulose is 20-30%；The grape seed extract is 0.1- relative to the mass fraction of oxidation nanometer cellulose
10%；The cellulose fixed nano silver composite antibacterial agent of oxidation nanometer is relative to the mass fraction of oxidation nanometer cellulose
0.1-2%；The temperature of the drying and forming-film is 30-60 DEG C.
7. the cellulose fixed nano silver/grape of the oxidation nanometer as made from preparation method described in any one of claims 1-6
Seed extract antibacterial, anti-oxidant composite membrane, which is characterized in that the preparation of nano silver is 0.6-6wt%.
8. the cellulose fixed nano silver of oxidation nanometer as claimed in claim 7/grape seed extract antibacterial, anti-oxidant composite membrane
Application in food packaging.
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| CN201811642398.3A CN109776869A (en) | 2018-12-29 | 2018-12-29 | A kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, preparation method and application |
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ID=66499562
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112662014A (en) * | 2020-11-30 | 2021-04-16 | 华南理工大学 | High-barrier antibacterial composite film based on nano-cellulose/MXene immobilized nano-silver and preparation method and application thereof |
| CN115926257A (en) * | 2023-01-04 | 2023-04-07 | 齐鲁工业大学(山东省科学院) | Preparation method and application of silver-loaded TEMPO oxidized nano-cellulose/chitosan antibacterial preservative film for fruit and vegetable packaging |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662014A (en) * | 2020-11-30 | 2021-04-16 | 华南理工大学 | High-barrier antibacterial composite film based on nano-cellulose/MXene immobilized nano-silver and preparation method and application thereof |
| CN112662014B (en) * | 2020-11-30 | 2022-09-20 | 华南理工大学 | High-barrier antibacterial composite film based on nano-cellulose/MXene immobilized nano-silver and preparation method and application thereof |
| CN115926257A (en) * | 2023-01-04 | 2023-04-07 | 齐鲁工业大学(山东省科学院) | Preparation method and application of silver-loaded TEMPO oxidized nano-cellulose/chitosan antibacterial preservative film for fruit and vegetable packaging |
| WO2024012609A3 (en) * | 2023-01-04 | 2024-03-07 | 齐鲁工业大学(山东省科学院) | Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof |
| GB2622753A (en) * | 2023-01-04 | 2024-03-27 | Univ Qilu Technology | Preparation method for silver-loaded tempo oxidized nanocellulose/chitosan antibacterial preservative film for fruit and vegetable packaging, and use thereof |
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