CN114591525B - Active packaging film and preparation method thereof - Google Patents
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Abstract
The invention discloses an active packaging film and a preparation method thereof. The active packaging film comprises the following raw materials in percentage by mass: starch: 65% -74%; nano-cellulose: 3% -5%; nanoparticle: 3% -5%; plasticizer: 20% -25%; the nano particles comprise the following raw materials in percentage by mass: and (3) chitosan: 60% -65%; sodium tripolyphosphate: 20% -25%; tannin: 15 to 20 percent. The preparation method of the active packaging film comprises the following steps: 1) Preparing nanoparticles by an ionic gel method; 2) Preparing a packaging film; 3) And (3) dipping the packaging film into the nanoparticle dispersion liquid to obtain the active packaging film. The active packaging film can slowly release the natural antibacterial agent tannin encapsulated in the nano particles, has long-acting antibacterial and antioxidant effects, is high in strength, high in transparency and simple to prepare, and is suitable for large-scale production and application.
Description
Technical Field
The invention relates to the technical field of packaging films, in particular to an active packaging film and a preparation method thereof.
Background
The food is rotten and deteriorated under the influence of adverse factors such as microorganisms and oxygen in the process of storage and transportation, so that not only is the resource waste caused, but also the human health is endangered. The traditional packaging method has certain defects in the aspects of prolonging the shelf life of food and protecting the environment of materials, and is difficult to completely meet the requirements of practical application. Thus, active packaging comes in the wake of a new form of packaging that can extend the shelf life of food products by releasing antimicrobial or antioxidant agents while maintaining the quality of the food product.
Antimicrobial packaging is an active packaging form with broad application prospects, which inhibits pathogenic and spoilage microorganisms in food by diffusing one or more antimicrobial agents from the packaging material into the packaged product, thereby improving the safety and quality of the food. Currently, antimicrobial carriers used for forming films or coatings in antimicrobial packages include biodegradable materials such as proteins, polysaccharides, lipids, and the like, commonly used antimicrobial agents mainly include inorganic antimicrobial agents, organic synthetic antimicrobial agents, and natural antimicrobial agents, and the preparation methods often adopt co-mixing casting, extrusion molding, dipping, coating, and the like. The traditional antibacterial package is characterized in that an antibacterial agent is directly added into a packaging film to endow the packaging film with an antibacterial effect, the method can change the color and the sensory characteristics of the packaging film and influence food, and antibacterial active substances can be inactivated by reactions such as neutralization and hydrolysis with a food matrix, so that long-acting antibacterial is difficult to achieve and the ever-increasing actual requirements cannot be met.
Therefore, it is very important to develop a slow-release antibacterial package with long-acting antibacterial and antioxidant effects.
Disclosure of Invention
The invention aims to provide an active packaging film and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
an active packaging film comprises the following raw materials in percentage by mass:
starch: 65% -74%;
nano-cellulose: 3% -5%;
nanoparticle: 3% -5%;
plasticizer: 20% -25%;
the nano particles comprise the following raw materials in percentage by mass:
and (3) chitosan: 60% -65%;
sodium tripolyphosphate: 20 to 25 percent;
tannin: 15 to 20 percent.
Preferably, the starch is at least one of corn starch, tapioca starch and potato starch.
Further preferably, the starch is corn starch.
Preferably, the length of the nano-cellulose is 0.1-1.3 μm, and the diameter is 5-20 nm.
Preferably, the nanocellulose is at least one of softwood nanocellulose, hardwood nanocellulose and bagasse nanocellulose.
Preferably, the particle size of the nanoparticles is 50nm to 500nm.
Preferably, the mass ratio of the chitosan to the sodium tripolyphosphate is 1-6.
Preferably, the plasticizer is at least one of glycerol, sorbitol, polyethylene glycol and sucrose.
The preparation method of the active packaging film comprises the following steps:
1) Dispersing chitosan in an acetic acid solution, adding tannin and sodium tripolyphosphate, and preparing nanoparticles by an ion gel method;
2) Adding starch and a plasticizer into water for plasticizing, adding nano-cellulose to prepare a membrane casting solution, and casting the membrane to obtain a packaging membrane;
3) Dispersing the nanoparticles obtained in the step 1) in a solvent to prepare a dispersion liquid, immersing the packaging film obtained in the step 2) in the dispersion liquid, soaking, taking out the packaging film, and drying to obtain the active packaging film.
Preferably, the preparation method of the active packaging film comprises the following steps:
1) Adding chitosan into an acetic acid solution, stirring for dissolving, adjusting the pH value of the solution to 3.5-5.5, adding a tannin solution, stirring uniformly, dropwise adding a sodium tripolyphosphate solution while stirring, continuously stirring for a crosslinking reaction after the addition is finished, centrifuging, taking a precipitate, and washing to prepare nanoparticles;
2) Adding starch and a plasticizer into water, plasticizing, adding nanocellulose to prepare a membrane casting solution, casting the membrane casting solution on a polytetrafluoroethylene plate, and then carrying out vacuum degassing and drying to obtain a packaging membrane;
3) Dispersing the nanoparticles obtained in the step 1) in a solvent to prepare a dispersion liquid, immersing the packaging film obtained in the step 2) in the dispersion liquid, soaking, taking out the packaging film, and drying to obtain the active packaging film.
Preferably, the time of the crosslinking reaction in the step 1) is 20min to 40min.
Preferably, the vacuum degassing in the step 2) is performed under the condition that the vacuum degree is 0.01MPa to 0.02MPa, and the degassing time is 10min to 20min.
Preferably, the plasticizing in the step 2) is carried out at 70-80 ℃, and the plasticizing time is 30-40 min.
Preferably, the drying in step 3) is performed at a temperature of 40 ℃ to 60 ℃ and a relative humidity of 60% to 80%.
The beneficial effects of the invention are: the active packaging film can slowly release the natural antibacterial agent tannin encapsulated in the nano particles, has long-acting antibacterial and antioxidant effects, is high in strength, high in transparency and simple to prepare, and is suitable for large-scale production and application.
Drawings
FIG. 1 is an AFM image of nanoparticles of example 1.
Figure 2 is a digital photograph of the active packaging film, the pure corn starch film, and the softwood nanocellulose-corn starch film of example 1.
FIG. 3 is a graph of the tensile strength and elongation at break test results for the activated packaging film, the pure corn starch film, and the softwood nanocellulose-corn starch film of example 1.
Fig. 4 is a graph of the results of the zone of inhibition tests for the active packaging film, the pure corn starch film, and the softwood nanocellulose-corn starch film of example 1.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
an active packaging film, the raw material composition of which is shown in the following table:
TABLE 1 composition of raw materials for an active packaging film
Note: the raw material composition of the nanoparticles is shown in the following table:
table 2 raw material composition table of nanoparticles
| Raw materials | Mass percent (%) |
| Chitosan | 60 |
| Sodium tripolyphosphate | 25 |
| Tannin | 15 |
The preparation method of the active packaging film comprises the following steps:
1) Adding chitosan into an acetic acid solution with the mass fraction of 1%, stirring and dissolving to obtain a chitosan-acetic acid solution, adjusting the pH of the chitosan-acetic acid solution to 4 by using a NaOH solution with the concentration of 0.04g/mL, adding tannin into a solution with the concentration of 0.01g/mL, adding the solution into the chitosan-acetic acid solution, stirring for 30min, adding sodium tripolyphosphate into a solution with the concentration of 0.015g/mL, dropwise adding the solution into the stirred chitosan-acetic acid solution through a separating funnel, continuously stirring for 40min after the solution is added, centrifuging, wherein the rotating speed of a centrifugal machine is 9000r/min, the centrifuging time is 40min, taking a supernatant, measuring the tannin concentration by using an ultraviolet spectrophotometer, taking a precipitate, washing and centrifuging for 3 times, and preparing nanoparticles;
2) Adding corn starch into deionized water, wherein the mass ratio of the corn starch to the deionized water is 1;
3) Adding water into the nanoparticles obtained in the step 1) to prepare a dispersion liquid with the mass fraction of 1%, immersing the packaging film obtained in the step 2) into the dispersion liquid for 15min, taking out the packaging film, and drying the packaging film in a constant-temperature and constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 70% to obtain the active packaging film (marked as BNC/TPS/CS NPs).
And (3) performance testing:
1) An Atomic Force Microscope (AFM) image of the nanoparticle in this example is shown in fig. 1.
As can be seen from fig. 1: the shape of the nano particles is close to spherical, and the diameter is 150 nm-500 nm.
2) The digital photographs of the active packaging film, the pure corn starch film (denoted as TPS) with the same thickness, and the softwood nanocellulose-corn starch film (the amount of the softwood nanocellulose added is the same as that of the active packaging film in this example, and denoted as BNC/TPS) in this example are shown in fig. 2 (a is the pure corn starch film, b is the softwood nanocellulose-corn starch film, and c is the active packaging film), the tensile strength and elongation at break test results are shown in fig. 3, and the zone of inhibition test (using escherichia coli as the antibacterial test object, using the agar diffusion method to evaluate the antibacterial performance of the film sample, the specific steps are carried outThe method comprises the following steps: cutting the film sample into circular pieces with diameter of 1cm, sterilizing under ultraviolet irradiation for 30min, and sterilizing 10 8 Pouring the suspension of the escherichia coli with the CFU/mL concentration into an autoclaved solid culture medium according to the volume ratio of 1.
As can be seen from fig. 2: the transparency of the active packaging film of the embodiment is greatly improved compared with that of a pure corn starch film with the same thickness and a softwood nano-cellulose-corn starch film with the same thickness.
As can be seen from fig. 3: the addition of the softwood nanocellulose improves the tensile strength of the corn starch film by about 4 times, the tensile strength reaches about 10 times of the corn starch film after the nanoparticles are continuously added, and meanwhile, the elongation at break is reduced to some extent after the softwood nanocellulose and the nanoparticles are added.
As can be seen from fig. 4: the pure corn starch film and the needle wood nano cellulose-corn starch film have no antibacterial effect on escherichia coli, and the active packaging film containing the nano particles has an inhibitory effect on the escherichia coli, so that the active packaging film has a certain non-diffusible antibacterial property.
Example 2:
an active packaging film, the raw material composition of which is shown in the following table:
TABLE 3 composition of raw materials for an active packaging film
Note: the raw material composition of the nanoparticles is shown in the following table:
table 4 raw material composition table of nanoparticles
| Raw materials | Mass percent (%) |
| |
60 |
| |
20 |
| |
20 |
The preparation method of the active packaging film comprises the following steps:
1) Adding chitosan into an acetic acid solution with the mass fraction of 1%, wherein the mass ratio of chitosan to the acetic acid solution is 1;
2) Adding corn starch into deionized water, wherein the mass ratio of the corn starch to the deionized water is 1;
3) Adding water into the nanoparticles obtained in the step 1) to prepare a dispersion liquid with the mass fraction of 1%, immersing the packaging film obtained in the step 2) into the dispersion liquid for 15min, taking out the packaging film, and drying the packaging film in a constant-temperature constant-humidity drying oven with the temperature of 40 ℃ and the relative humidity of 70% to obtain the active packaging film.
Performance testing (test method as in example 1):
1) AFM test shows that: the shape of the nano particles in the embodiment is close to spherical, and the diameter is 50 nm-180 nm;
2) Displaying the digital photo: compared with a pure corn starch film with the same thickness and a hardwood nanocellulose-corn starch film with the same thickness, the transparency of the active packaging film in the embodiment is greatly improved;
3) The tensile strength and elongation at break test results show: the addition of the hardwood nanocellulose improves the tensile strength of the corn starch film by about 3 times, the tensile strength reaches about 9 times of the corn starch film after the nanoparticles are continuously added, and meanwhile, the elongation at break is reduced after the hardwood nanocellulose and the nanoparticles are added;
4) The test of the inhibition zone shows that: the pure corn starch film and the broadleaf wood nano cellulose-corn starch film have no antibacterial effect on escherichia coli, and the active packaging film containing the nano particles has an inhibitory effect on the escherichia coli, so that the active packaging film has a certain non-diffusible antibacterial property.
Example 3:
an active packaging film, the raw material composition of which is shown in the following table:
TABLE 5 composition of raw materials for an active packaging film
Note: the raw material composition of the nanoparticles is shown in the following table:
TABLE 6 raw Material composition of nanoparticles
The preparation method of the active packaging film comprises the following steps:
1) Adding chitosan into an acetic acid solution with the mass fraction of 1%, stirring and dissolving to obtain a chitosan-acetic acid solution, adjusting the pH of the chitosan-acetic acid solution to 3.8 by using a NaOH solution with the concentration of 0.04g/mL, adding tannin into a solution with the concentration of 0.15g/mL, stirring for 30min, adding sodium tripolyphosphate into a solution with the concentration of 0.02g/mL, dropwise adding the solution into the stirred chitosan-acetic acid solution through a separating funnel, continuously stirring for 30min after adding, centrifuging at the rotation speed of 9000r/min for 30min, taking the supernatant, measuring the tannin concentration by using an ultraviolet spectrophotometer, and washing and centrifuging the precipitate for 3 times to obtain nanoparticles;
2) Adding corn starch into deionized water, wherein the mass ratio of the corn starch to the deionized water is 1;
3) Adding water into the nanoparticles obtained in the step 1) to prepare a dispersion liquid with the mass fraction of 1%, immersing the packaging film obtained in the step 2) into the dispersion liquid for 15min, taking out the packaging film, and drying the packaging film in a constant-temperature constant-humidity drying oven with the temperature of 40 ℃ and the relative humidity of 70% to obtain the active packaging film.
Performance testing (test method as in example 1):
1) AFM test shows that: the shape of the nano particles in the embodiment is close to spherical, and the diameter is 100 nm-460 nm;
2) Displaying the digital photo: compared with a pure corn starch film with the same thickness and a bagasse nano cellulose-corn starch film with the same thickness, the transparency of the active packaging film in the embodiment is greatly improved;
3) The tensile strength and elongation at break test results are shown in the figure: the addition of the bagasse nanocellulose improves the tensile strength of the corn starch film by about 2 times, the tensile strength reaches about 9 times of the corn starch film after the nanoparticles are continuously added, and meanwhile, the elongation at break is reduced after the bagasse nanocellulose and the nanoparticles are added;
4) The test of the inhibition zone shows that: the pure corn starch film and the bagasse nano-cellulose-corn starch film have no antibacterial effect on escherichia coli, and the active packaging film containing the nano-particles has an inhibitory effect on the escherichia coli, which shows that the active packaging film has a certain non-diffusible antibacterial property.
Example 4:
an active packaging film, the raw material composition of which is shown in the following table:
TABLE 7 raw material composition table of an active packaging film
Note: the raw material composition of the nanoparticles is shown in the following table:
TABLE 8 raw Material composition Table of nanoparticles
| Raw materials | Mass percent (%) |
| |
60 |
| |
20 |
| |
20 |
The preparation method of the active packaging film comprises the following steps:
1) Adding chitosan into an acetic acid solution with the mass fraction of 1%, stirring and dissolving to obtain a chitosan-acetic acid solution, adjusting the pH of the chitosan-acetic acid solution to 4.2 by using a NaOH solution with the concentration of 0.04g/mL, adding tannin into a solution with the concentration of 0.02g/mL, stirring for 30min, adding sodium tripolyphosphate into a solution with the concentration of 0.005g/mL, dropwise adding the solution into the stirred chitosan-acetic acid solution through a separating funnel, continuously stirring for 30min after adding, centrifuging at the rotation speed of 9000r/min for 30min, taking the supernatant, measuring the tannin concentration by using an ultraviolet spectrophotometer, and washing and centrifuging the precipitate for 3 times to obtain nanoparticles;
2) Adding corn starch into deionized water, wherein the mass ratio of the corn starch to the deionized water is 1;
3) Adding water into the nanoparticles obtained in the step 1) to prepare a dispersion liquid with the mass fraction of 1%, then soaking the packaging film obtained in the step 2) into the dispersion liquid for 15min, taking out the packaging film, and drying the packaging film in a constant-temperature and constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 70% to obtain the active packaging film.
Performance testing (test method as in example 1):
1) AFM test shows that: the shape of the nano particles in the embodiment is close to spherical, and the diameter is 70 nm-230 nm;
2) Displaying the digital photos: compared with a pure corn starch film with the same thickness and a softwood nanocellulose-corn starch film with the same thickness, the transparency of the active packaging film in the embodiment is greatly improved;
3) The tensile strength and elongation at break test results are shown in the figure: the addition of the softwood nanocellulose improves the tensile strength of the corn starch film by about 2 times, the tensile strength reaches about 6 times of the corn starch film after the nanoparticles are continuously added, and meanwhile, the elongation at break is reduced after the softwood nanocellulose and the nanoparticles are added;
4) The test of the inhibition zone shows that: the pure corn starch film and the needle wood nano cellulose-corn starch film have no antibacterial effect on escherichia coli, and the active packaging film containing the nano particles has an inhibitory effect on the escherichia coli, so that the active packaging film has a certain non-diffusible antibacterial property.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (9)
1. The active packaging film is characterized by comprising the following raw materials in percentage by mass:
starch: 65% -74%;
nano-cellulose: 3% -5%;
nanoparticle: 3% -5%;
plasticizer: 20 to 25 percent;
the nano particles comprise the following raw materials in percentage by mass:
and (3) chitosan: 60% -65%;
sodium tripolyphosphate: 20% -25%;
tannin: 15% -20%;
the active packaging film is prepared by a preparation method comprising the following steps of: 1) Dispersing chitosan in an acetic acid solution, adding tannin and sodium tripolyphosphate, and preparing nanoparticles by an ion gel method; 2) Adding starch and a plasticizer into water, plasticizing, adding nano-cellulose to prepare a membrane casting solution, and casting to form a membrane to obtain a packaging membrane; 3) Dispersing the nanoparticles obtained in the step 1) in a solvent to prepare a dispersion liquid, immersing the packaging film obtained in the step 2) in the dispersion liquid, soaking, taking out the packaging film, and drying to obtain the active packaging film.
2. The active packaging film of claim 1, wherein: the starch is at least one of corn starch, cassava starch and potato starch.
3. The active packaging film of claim 1, wherein: the length of the nano-cellulose is 0.1-1.3 mu m, and the diameter is 5-20 nm.
4. The active packaging film of claim 1, wherein: the nano-cellulose is at least one of coniferous wood nano-cellulose, hardwood nano-cellulose and bagasse nano-cellulose.
5. The active packaging film according to any one of claims 1 to 4, characterized in that: the particle size of the nano particles is 50 nm-500 nm.
6. The active packaging film according to any one of claims 1 to 4, characterized in that: the mass ratio of the chitosan to the sodium tripolyphosphate is 1-6.
7. An active packaging film according to any one of claims 1 to 4, characterized in that: the plasticizer is at least one of glycerol, sorbitol, polyethylene glycol and sucrose.
8. The active packaging film of claim 1, wherein: and 2) plasticizing is carried out at 70-80 ℃, and the plasticizing time is 30-40 min.
9. Active packaging film according to claim 1 or 8, characterized in that: the drying in the step 3) is carried out at the temperature of 40-60 ℃ and the relative humidity of 60-80%.
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| CN103254471A (en) * | 2013-05-29 | 2013-08-21 | 江南大学 | Edible membrane with chitosan-sodium tripolyphosphate nanoparticles as matrix and preparation method of edible membrane |
| CN108041405A (en) * | 2017-11-08 | 2018-05-18 | 广西大学 | A kind of preparation process of essential oil microcapsules edible film |
| 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 |
| WO2021168581A1 (en) * | 2020-02-28 | 2021-09-02 | Impactful Health Research And Development Inc. | Compostable anti-microbial film and method of applying film to packaging |
| CN112753759A (en) * | 2020-12-30 | 2021-05-07 | 江苏大学 | Preparation method and application of composite fresh-keeping film coating agent for relieving browning of fresh-cut apples |
| CN113383882A (en) * | 2021-07-05 | 2021-09-14 | 青岛农业大学 | Degradable antibacterial composite preservative film and preparation method and application thereof |
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