CN109294003A - A kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof - Google Patents
A kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof Download PDFInfo
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
Abstract
The invention discloses a kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof.Preparation method of the present invention is: using starch as dispersing agent and stabilizer, Zn (NO3)2·6H2O is zinc source, prepares ZnO nanoparticle；Chitosan is dissolved in 1% acetic acid solution, glycerol is added, chitosan film liquid is prepared, disperses deionized water for ZnO nanoparticle, sodium alginate and glycerol, stirring is added, ultrasonic disperse is stood, and ultrasonic degassing obtains sodium alginate film liquid；Dry by chitosan film liquid casting film-forming, later on its surface by sodium alginate film liquid casting film-forming, dry, finally again by chitosan film liquid casting film-forming, drying takes off film up to antimicrobial preservative film.CS/SA/SH-ZnO antimicrobial preservative film prepared by the present invention has lower water-soluble, vapor transmission coefficient, and anti-microbial property is good, can be avoided the excessive loss and microbial contamination of fruits and vegetables moisture in transport, storage and process.
Description
Technical field
The present invention relates to a kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof, belongs to fresh food
Product field of packaging material.
Background technique
In packaging industry, used material is mainly petroleum-based plastics material, such as polypropylene (PP), polyethylene
(PE) or polystyrene (PS), but it is difficult to degrade, therefore brings serious plastic wastes problem.With problem of environmental pollution day
Beneficial serious, there is an urgent need to the uses that other environment-friendly materials replace petroleum-based plastics material by people.Natural polysaccharide because its abundance,
Renewable, environmentally friendly, less toxic, biodegradable and biocompatibility and the concern for increasingly causing researcher.Past tens
Application of many polysaccharide in food packaging applications has been studied in Nian Zhong, such as starch, gelatin, cellulose, shell gather
Sugar, sodium alginate and its derivative.Compared with other polysaccharide, chitosan is selected as thin extensively due to its unique advantage
Membrane material.Chitosan is a kind of natural cationic polysaccharide, have good antibacterial activity, gas selective penetrated property, it is excellent at
Film ability and good resistance oxygen ability.However, the vapor water barriers performance and serious brittleness of difference limit it in food packaging
In direct application.Sodium alginate has good film forming, water-retaining property, but its soluble easily in water also limits it as packing timber
The application of material.
If can solve above-mentioned technical problem, chitosan and sodium alginate answering as food packaging will be effectively widened
Use range.
Summary of the invention
The present invention is intended to provide a kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof, overcomes
The vapor water barriers performance of chitosan film difference, the defects of serious brittleness and sodium alginate film water resistance are poor in the prior art.
In the present invention, sodium alginate is the by-product after extracting iodine and mannitol in the kelp or sargassum of brown algae
Object, molecule are keyed by beta-D-mannuronic acid and α-L- guluronic acid by (1 → 4), are a kind of natural polysaccharides, sweet
Electronegative carboxylic acid group can pass through electrostatic with amino positively charged on chitosan on dew uronic acid and guluronic units
Effect and hydrogen bond form the multilayer film combined closely.Due to sodium alginate good water-retaining property, the formation of multilayer film, which has, to be conducive to improve shell
The high defect of glycan film water vapor permeation coefficient.ZnO nanoparticle is added in multilayer film as inorganic crosslinking agent, can reinforce each group
/ tightness degree, further improve its mechanical property and vapor water barriers performance.
The present invention provides a kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film, including following components: ZnO, shell
Glycan, sodium alginate；Wherein, the mass ratio of ZnO and sodium alginate are as follows: 1 ~ 5:100；The mass ratio of chitosan and sodium alginate
Are as follows: 5 ~ 15:10.
The chitosan containing ZnO/sodium alginate antimicrobial preservative film preparation method that the present invention provides above-mentioned, including following step
It is rapid:
(1) preparation of ZnO nanoparticle:
First using starch as dispersing agent and stabilizer, Zn (NO3)2·6H2O is zinc source, prepares ZnO nanoparticle；
(2) prepared by chitosan film liquid:
Chitosan is dissolved in 1% acetic acid solution, glycerol is added, chitosan film liquid is prepared；
(3) prepared by sodium alginate film liquid:
Deionized water is dispersed by ZnO nanoparticle prepared by step (1), sodium alginate and glycerol, stirring, ultrasound point is added
It dissipates, stands, ultrasonic degassing 10-15min obtains sodium alginate film liquid；
(4) chitosan containing ZnO/sodium alginate antimicrobial preservative film preparation:
It first by chitosan film liquid casting film-forming, dries, later dries sodium alginate film liquid casting film-forming, finally on its surface
It is dry again by chitosan film liquid casting film-forming, film is taken off up to antimicrobial preservative film.
Further, in the preparation of step (1) ZnO nanoparticle, soluble starch is dissolved in 80 ~ 95 DEG C of water, is stirred
To being completely dissolved, Zn (NO is added3)2·6H2O stirs 20-40min, and NaOH solution is added dropwise, and after stirring 1 ~ 3h, is centrifuged, washing,
It is dry, obtain ZnO nanoparticle；Wherein, soluble starch and Zn (NO3)2·6H2The mass ratio of O is 1:0.25-2；Solubility is formed sediment
The mass ratio of powder and water is 1:80-120.
Further, the concentration of NaOH solution is 0.1-0.3M, Zn (NO3)2·6H2The molar ratio of O and NaOH is 0.5-1.
Further, in the preparation step of the ZnO nanoparticle, dry temperature is 50-80 DEG C, time 18-24
Hour.
Further, in the preparation of step (2) chitosan film liquid, 1mL glacial acetic acid is added dropwise in 100mL deionized water, is stirred
10 ~ 30min is mixed, the acetic acid solution that volumetric concentration is 1% is formed, weighs chitosan and be dissolved in acetic acid solution, glycerol is added, stir,
Ultrasonic disperse is stood, ultrasonic degassing 10-15min；Wherein, the mass ratio of glycerol and chitosan is 1:1-4.
Further, in the preparation of step (3) sodium alginate film liquid, ZnO nanoparticle is added in deionized water, is then surpassed
Sound is uniformly mixed, and adds sodium alginate and glycerol；The mass ratio of ZnO nanoparticle and sodium alginate is 1:20-200, glycerol
Mass ratio with sodium alginate is 1:1-4.
Further, ultrasound condition is that Probe Ultrasonic Searching power is 200-500W in step (2) and (3), ultrasonic 2-4s,
Have a rest 1-3s.
Further, in the preparation of chitosan of the step (4) containing ZnO/sodium alginate antimicrobial preservative film, 5mL chitosan is taken
Film liquid is in 12 × 12cm2Casting film-forming on glass plate, is dried in an oven, adds 10mL sodium alginate film on its surface later
Liquid, casting film-forming is dry in baking oven, finally takes 5mL chitosan film liquid casting film-forming again, dry, takes off film；
The mass ratio of sodium alginate and chitosan is 1:0.5 ~ 1.5.
Further, in step (4), dry temperature is 30-50 DEG C, time 30-120min.
The method of chitosan containing ZnO/sodium alginate antimicrobial preservative film provided by the invention limits the shell containing ZnO
In glycan/sodium alginate antimicrobial preservative film preparation step, dry temperature is 30-50 DEG C, time 30-120min.It limits
In the preparation step of the ZnO nanoparticle, dry temperature is 50-80 DEG C, and the time is 18-24 hours.This is because: containing
In the chitosan of ZnO/sodium alginate antimicrobial preservative film preparation step, if drying temperature is excessively high, polysaccharide structures can be destroyed, and
In the preparation step of ZnO nanoparticle, drying temperature is too low, is not easy to be dehydrated, and drying time can extend, and is formed simultaneously hydroxide
Zinc rather than zinc oxide nano-particle.
Beneficial effects of the present invention:
The method of chitosan containing ZnO/sodium alginate antimicrobial preservative film provided by the invention, this method is simple, quick, does not add
Add any noxious material, preservative film obtained is transparent, has lower water-soluble and vapor transmission coefficient, higher antibiotic property
Energy.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of SH-ZnO nanoparticle prepared by embodiment 1；
Fig. 2 is the surface sweeping electron microscope of SH-ZnO nanoparticle prepared by embodiment 1；
Fig. 3 is the water-soluble figure of antimicrobial preservative film prepared by embodiment 1-3 and comparative example 1,2；
Fig. 4 is the anti-microbial property figure of antimicrobial preservative film prepared by embodiment 1-3 and comparative example 1,2.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art described routine experiment
The operation of step or condition can carry out.Reagents or instruments used without specified manufacturer, being can be by commercially available acquisition
Conventional reagent product.
Embodiment 1 (SA/SH-ZnO-1)
The chitosan containing ZnO/sodium alginate antimicrobial preservative film preparation method that the present embodiment provides a kind of, comprising the following steps:
Starch-ZnO nanoparticle is prepared in situ first, prepares chitosan film liquid later, and prepared ZnO is uniformly added into alginic acid
Sodium alginate film liquid is made in sodium solution, chitosan film liquid stream is prolonged on glass plate, is dried, then sodium alginate film liquid is covered
Above, casting film-forming is dry, is eventually adding chitosan film liquid, casting film-forming.Specific step is as follows:
1g soluble starch is dissolved in 100ml deionized water, 90 DEG C of stirring 30min are warming up in magnetic stirring apparatus to complete
Dissolution；By 0.595g Zn (NO3)2·6H2O is added in above-mentioned solution and stirs 30min；50ml 0.2M NaOH is added dropwise later
Solution after stirring 2h, is centrifuged, and washing, drying for 24 hours, obtains ZnO nanoparticle in 50 DEG C of baking ovens；
X-ray diffraction and scanning electron microscope analysis, concrete outcome such as Fig. 1 and Fig. 2 are carried out to prepared ZnO nanoparticle.From Fig. 1
In it can be seen that the characteristic peak of ZnO nanoparticle is overlapped with JCPDS 76-0704 standard card characteristic peak, and not miscellaneous peak out
It is existing, suggest the formation of pure ZnO particle.As can be seen from Figure 2 starch-ZnO nanoparticle is formed by irregular
Spheric granules, partial size 200-300nm, uniform particle diameter.
1mL glacial acetic acid is dissolved in 100mL deionized water, is added 2g chitosan and 1g glycerol, stirring 1h is made to uniform
Chitosan film liquid.The zinc oxide nano-particle of the above-mentioned preparation of 0.01g is added in 100ml deionized water, Probe Ultrasonic Searching, probe is super
Acoustical power is 500W, ultrasonic 3s, and interval 2s is stirred evenly；2g sodium alginate and 1g glycerol are added later and stirs 1h to uniform；It will
5mL chitosan film liquid is poured on glass plate, casting film-forming, dry.10mL sodium alginate film liquid is covered in its surface later, is flowed
Prolong film forming, it is dry, 5mL chitosan film liquid is finally covered in surface, glass plate is put into 50 DEG C of baking ovens dry by casting film-forming
Chitosan/sodium alginate/starch-ZnO(CS/SA/SH-ZnO can be obtained in 60min) antimicrobial preservative film.
Embodiment 2 (CS/SA/SH-ZnO-2)
The chitosan containing ZnO/sodium alginate antimicrobial preservative film preparation method that the present embodiment provides a kind of, the specific steps are as follows:
0.5g soluble starch is dissolved in 100ml deionized water, 90 DEG C of stirring 30min are warming up in magnetic stirring apparatus to complete
Fully dissolved；By 0.595g Zn (NO3)2·6H2O is added in above-mentioned solution and stirs 30min；50ml 0.3M is added dropwise later
NaOH solution, after stirring 2h, is centrifuged, and washing is dried for 24 hours in 70 DEG C of baking ovens；
1mL glacial acetic acid is dissolved in 100mL deionized water, 2g chitosan and 0.5g glycerol, stirring 1h to uniform, obtained shell is added
Glycan film liquid.The zinc oxide nano-particle of the above-mentioned preparation of 0.05g is added in 100ml deionized water, Probe Ultrasonic Searching, Probe Ultrasonic Searching
Power is 300W, ultrasonic 3s, and interval 2s is stirred evenly, and 2g sodium alginate and 0.5g glycerol are added later and stirs 1h to uniform；It will
5mL chitosan film liquid is poured on glass plate, casting film-forming, dry.10mL sodium alginate film liquid is covered in its surface later, is flowed
Prolong film forming, it is dry, 5mL chitosan film liquid is finally covered in surface, glass plate is put by casting film-forming, is done in 40 DEG C of baking ovens
Chitosan/sodium alginate/starch-ZnO(CS/SA/SH-ZnO can be obtained in dry 90min) antimicrobial preservative film.
Embodiment 3 (CS/SA/SH-ZnO-3)
The chitosan containing ZnO/sodium alginate antimicrobial preservative film preparation method that the present embodiment provides a kind of, the specific steps are as follows:
2g soluble starch is dissolved in 100ml deionized water, 90 DEG C of stirring 30min are warming up in magnetic stirring apparatus to complete
Dissolution；By 0.595g Zn (NO3)2·6H2O is added in above-mentioned solution and stirs 30min；50ml 0.1M NaOH is added dropwise later
Solution, after stirring 2h, is centrifuged, and washing is dried for 24 hours in 80 DEG C of baking ovens；
1mL glacial acetic acid is dissolved in 100mL deionized water, is added 2g chitosan and 2g glycerol, it is poly- that shell is made to uniform in stirring 1h
Sugared film liquid.The zinc oxide nano-particle of the above-mentioned preparation of 0.1g is added in 100ml deionized water, Probe Ultrasonic Searching, Probe Ultrasonic Searching function
Rate is 400W, ultrasonic 4s, and interval 1s is stirred evenly, and 2g sodium alginate and 2g glycerol are added later and stirs 1h to uniform；By 5mL
Chitosan film liquid is poured on glass plate, casting film-forming, dry.10mL sodium alginate film liquid is covered in its surface later, is cast
Film forming, it is dry, 5mL chitosan film liquid is finally covered in surface, glass plate is put into 30 DEG C of baking ovens dry by casting film-forming
Chitosan/sodium alginate/starch-ZnO(CS/SA/SH-ZnO can be obtained in 120min) antimicrobial preservative film.
Comparative example 1 (CS)
This example provides a kind of preparation method of pure chitosan preservative film, the specific steps are as follows:
1mL glacial acetic acid is dissolved in 100mL deionized water, is added 2g chitosan and 2g glycerol, it is poly- that shell is made to uniform in stirring 1h
Sugared film liquid.20mL chitosan film liquid is poured on glass plate, casting film-forming, glass plate is put into 50 DEG C of baking ovens dry 60min,
Chitosan (CS) antimicrobial preservative film can be obtained.
Comparative example 2(CS/SA)
This example provides a kind of preparation method of chitosan/sodium alginate, the specific steps are as follows:
1mL glacial acetic acid is dissolved in 100mL deionized water, is added 2g chitosan and 1g glycerol, it is poly- that shell is made to uniform in stirring 1h
Sugared film liquid.2g sodium alginate and 1g glycerol are added in 100mL deionized water, stirring 1h is to uniform；5mL chitosan film liquid is fallen
On a glass, casting film-forming, it is dry.10mL sodium alginate film liquid is covered in its surface later, casting film-forming is dry, most
5mL chitosan film liquid is covered in surface afterwards, glass plate is put into 30 DEG C of baking ovens dry 120min, can obtained by casting film-forming
To chitosan/sodium alginate (CS/SA) antimicrobial preservative film.
Performance test
1, the measuring mechanical property of film uses the standard of GB13022-91 " stretched plastic film performance test method ", by omnipotent examination
It tests machine (Jiangdu Ren Heng machinery plant, RH-10KN electronic universal tester) and tests its tensile strength and elongation at break, the thickness of film
(Thickness) is spent to be measured by calibrator (Shanghai Bang Te test apparatus device fabrication Co., Ltd).
Tensile strength (TS) is by maximum pull (Fmax) with obtained by the ratio calculation of cross-sectional area,
TS=Fmax/ (L × W)
TS indicates tensile strength (Mpa), FmaxIt is the maximum pull born when film fracture, L indicates that the width of film, W indicate film
Thickness.
Elongation at break (EB%) calculates gained by following formula,
EB%=(L-L0)/L0
L indicates the initial length (mm) of film, L0Indicate the length (mm) after film stretching.
2, the preservative film after measurement is dry soaks the percentage of front and back Mass lost in water to represent the water solubility (WR) of film.
WR=[(Wa-Wb)/Wa]×100%
WaFor the quality of initial sample, WbFor the dissolved quality of film.
Fig. 3 is the water-soluble figure of antimicrobial preservative film prepared by 1-3 of the embodiment of the present invention and comparative example 1,2；With SH-
The increase of ZnO content, it is water-soluble constantly to reduce, this is because the hydrogen bond action between SH-ZnO and chitosan, sodium alginate
Polysaccharide molecule dissolution is limited into aqueous solution.
3, vapor transmission coefficient test uses GB1307-88 " plastic film and sheet material water vapor permeability test method-cup
Formula method " weight method test.Be added in moisture vapor transmission cup it is dry after anhydrous calcium chloride, apart from bottleneck 5mm, bottleneck is with prepared fresh-keeping
Film is tightened and is sealed with paraffin, is placed it in bottom and is filled in saturated sodium chloride solution drier, takes out claim at regular intervals
Measuring bottle weighing until when front and back quality incrementss twice are differed less than 5%, weighs three times, calculates average value, as a result with
Δ m is indicated, calculates the moisture-vapor transmission of composite membrane.
Calculation formula is WVP=Δ m × d/ (A × Δ t × Δ p)
Wherein, WVP indicates vapor transmission coefficient [gmm/ (m2·h·kPa)]；The thickness (mm) of d expression composite membrane；Δ
M indicates the quality incrementss (g) after stablizing；A indicates the area (m of the film of clip2), the experiment area phase of composite membrane in experiment
It together, is 572mm2；Δ t indicates the time interval (h) between measurement every time, is divided into 12h between measurement when experiment；Δ p indicates compound
The fixed vapor pressure difference (kPa) in film two sides, due to testing at 25 DEG C, relative humidity keeps 75%, therefore Δ p takes 2.37 kPa.
The preparation condition and its mechanical performance and vapor transmission coefficient of 1 antimicrobial preservative film of table
The mechanical performance and vapor that table 1 is antimicrobial preservative film prepared by 1-3 of the embodiment of the present invention and comparative example 1,2 are through system
Number；It can be found that increasing with SH-ZnO, the tensile strength of film increases therewith, and elongation at break reduces.This is because SH-ZnO
Addition, increase the interior friction of chitosan film matrix, so that tensile strength increases, and it destroys chitosan/sodium alginate
It is acted in membrane molecule with intermolecular hydrogen bonding, SH-ZnO and chitosan, sodium alginate form new hydrogen bond action, hinder molecule
Movement, therefore elongation at break is caused to reduce.
4, the anti-microbial property of film is tested by the method for plate culture count, takes 100 μ L 105CFU/mL bacterial suspension is added dropwise anti-
The bacterium preservative film surface (having a size of 2cm × 2cm) simultaneously coats uniformly, is placed in 37 ± 1 DEG C, the interior culture 4h of 95% incubator of humidity >.So
It is immersed in the centrifuge tube of 20mLPBS buffer afterwards, shakes 10min on 37 ± 1 DEG C of constant-temperature tables, make to attach to film surface
Bacterium is eluted in PBS buffer solution, and buffer is diluted 10 times.PBS buffer solution after drawing 60 μ L dilution is applied to agar
It on culture medium flat plate, is cultivated at 37 ± 1 DEG C for 24 hours, every group is repeated 3 times.Not add the bacterial suspension of preservative film as control group.
Fig. 4 is the anti-microbial property figure of antimicrobial preservative film prepared by 1-3 of the embodiment of the present invention and comparative example 1,2.With SH-
The increase of ZnO content, anti-microbial property are continuously increased, this is because the increase of SH-ZnO content improves SH-ZnO and bacterium
Touch opportunity, antibacterial material is positively charged, and bacterial cell surface is negatively charged, and when the two is in contact, current potential is neutralized, and charge occurs
Transfer, makes cell membrane surface protein qualitative change, the Zn for destroying bacterial metabolism to sterilize, and dissolving out2+Amount is continuously increased,
Zn2+It can react with the part functional group of protein, nucleic acid, be reacted, hindered with biological enzyme even into microbial cell
Hinder the normal biochemical action of bacterium and physiological function, to kill bacterium.
Claims (10)
1. a kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film, it is characterised in that: including following components: ZnO, shell are poly-
Sugar, sodium alginate；Wherein, the mass ratio of ZnO and sodium alginate are as follows: 1 ~ 5:100；The mass ratio of chitosan and sodium alginate are as follows: 5
~15:10。
2. a kind of preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film described in claim 1, feature exist
In: the following steps are included:
(1) preparation of ZnO nanoparticle:
First using starch as dispersing agent and stabilizer, Zn (NO3)2·6H2O is zinc source, prepares ZnO nanoparticle；
(2) prepared by chitosan film liquid:
Chitosan is dissolved in 1% acetic acid solution, glycerol is added, chitosan film liquid is prepared；
(3) prepared by sodium alginate film liquid:
Deionized water is dispersed by ZnO nanoparticle prepared by step (1), sodium alginate and glycerol, stirring, ultrasound point is added
It dissipates, stands, ultrasonic degassing 10-15min obtains sodium alginate film liquid；
(4) chitosan containing ZnO/sodium alginate antimicrobial preservative film preparation:
It first by chitosan film liquid casting film-forming, dries, later dries sodium alginate film liquid casting film-forming, finally on its surface
It is dry again by chitosan film liquid casting film-forming, film is taken off up to antimicrobial preservative film.
3. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 2, feature exist
In: in the preparation of step (1) ZnO nanoparticle, soluble starch is dissolved in 80 ~ 95 DEG C of water, stirring is added to being completely dissolved
Zn(NO3)2·6H2O stirs 20-40min, and NaOH solution is added dropwise, and after stirring 1 ~ 3h, is centrifuged, washs, dry, obtains ZnO nano grain
Son；Wherein, soluble starch and Zn (NO3)2·6H2The mass ratio of O is 1:0.25-2；The mass ratio of soluble starch and water is
1:80-120。
4. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 3, feature exist
In: the concentration of NaOH solution is 0.1-0.3M, Zn (NO3)2·6H2The molar ratio of O and NaOH is 0.5-1.
5. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 3, feature exist
In: in the preparation step of the ZnO nanoparticle, dry temperature is 50-80 DEG C, and the time is 18-24 hours.
6. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 2, feature exist
In: in the preparation of step (2) chitosan film liquid, 1mL glacial acetic acid is added dropwise in 100mL deionized water, stirs 10 ~ 30min, shape
The acetic acid solution for being 1% at volumetric concentration, weighs chitosan and is dissolved in acetic acid solution, and glycerol is added, and stirs, and ultrasonic disperse is quiet
It sets, ultrasonic degassing 10-15min；Wherein, the mass ratio of glycerol and chitosan is 1:1-4.
7. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 2, feature exist
In: in the preparation of step (3) sodium alginate film liquid, ZnO nanoparticle is added in deionized water, then ultrasonic mixing is uniform, then
Sodium alginate and glycerol is added；The mass ratio of ZnO nanoparticle and sodium alginate is 1:20-200, the matter of glycerol and sodium alginate
Amount is than being 1:1-4.
8. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 6 or 7, feature
Be: ultrasound condition is in step (2) and (3), and Probe Ultrasonic Searching power is 200-500W, ultrasonic 2-4s, interval 1-3s.
9. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 2, feature exist
In: in the preparation of chitosan of the step (4) containing ZnO/sodium alginate antimicrobial preservative film, take 5mL chitosan film liquid in 12 × 12cm2
Casting film-forming on glass plate, is dried in an oven, adds 10mL sodium alginate film liquid, casting film-forming, baking oven on its surface later
Middle drying finally takes 5mL chitosan film liquid casting film-forming again, dry, takes off film；
The mass ratio of sodium alginate and chitosan is 1:0.5 ~ 1.5.
10. the preparation method of the chitosan containing ZnO/sodium alginate antimicrobial preservative film according to claim 2, feature exist
In: in step (4), dry temperature is 30-50 DEG C, time 30-120min.
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| CN110558376A (en) * | 2019-10-10 | 2019-12-13 | 上海海洋大学 | Preparation method and application of chitosan-Zn composite nanoparticle preservative film |
| CN110643078A (en) * | 2019-09-03 | 2020-01-03 | 广西科技师范学院 | Low-moisture-permeability edible composite preservative film and preparation method thereof |
| CN110833093A (en) * | 2019-11-27 | 2020-02-25 | 武汉轻工大学 | Antibacterial preservative film and application thereof in duck meat preservation |
| CN112280067A (en) * | 2019-07-24 | 2021-01-29 | 南京理工大学 | Preparation method of edible antibacterial film |
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| CN114044943A (en) * | 2021-12-16 | 2022-02-15 | 成都大学 | Edible chilled meat antibacterial preservative film and preparation method and application thereof |
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| CN114044943A (en) * | 2021-12-16 | 2022-02-15 | 成都大学 | Edible chilled meat antibacterial preservative film and preparation method and application thereof |
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| CN114591542B (en) * | 2022-04-25 | 2022-11-18 | 江南大学 | Sodium alginate-based antioxidant antibacterial bioactive composite membrane added with IRMOF-3/carvacrol and preparation method thereof |
| CN115302934A (en) * | 2022-08-12 | 2022-11-08 | 武汉轻工大学 | Full-biodegradable double-layer antibacterial composite film and preparation method thereof |
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