CN115948032A - Biodegradable slow-release antibacterial preservative film and preparation method and application thereof - Google Patents
Biodegradable slow-release antibacterial preservative film and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a biodegradable slow-release antibacterial preservative film and a preparation method and application thereof. A biodegradable slow-release antibacterial preservative film comprises the following components in parts by mass: 50-80 parts of matrix resin, 1-5 parts of coupling agent, 1-10 parts of bacteriostatic agent, 5-30 parts of inorganic porous material and 1-5 parts of processing aid. The biodegradable slow-release antibacterial preservative film provided by the invention not only has the biodegradation performance, but also has the slow-release antibacterial performance, the using time of the antibacterial preservative film can be prolonged through the slow-release function, the shelf life of fruits, vegetables, food and the like is further prolonged, and the problem of white pollution can be solved by adopting compost degradation after the use.
Description
The technical field is as follows:
the invention relates to the technical field of freshness-retaining packaging materials, in particular to a biodegradable slow-release antibacterial freshness-retaining film and a preparation method and application thereof.
Background art:
with the increasing severity of the 'white pollution' problem worldwide, the governments of various countries have successively proposed the policy of plastic restriction and plastic prohibition, and the biodegradable material has great application potential as one of the potential materials capable of replacing the traditional plastic. At present, most of packaging materials applied to fruits, vegetables, foods and the like adopt packaging bags prepared from traditional plastics, and biodegradable packaging films with certain fresh-keeping and antibacterial functions are gradually popularized due to the fact that the shelf life of the foods can be prolonged and the commodity value can be improved. The bacteriostatic packaging material has a strong inhibiting effect on bacteria, fungi and the like, and can effectively ensure food safety, so that the bacteriostatic packaging material can well meet the requirements of packaging materials. However, the traditional antibacterial packaging material has the defect that the traditional antibacterial packaging material is not biodegradable and has no slow release function, so that the application of the traditional antibacterial packaging material is greatly limited.
Patent CN113583422A discloses a biodegradable plastic wrap with antibacterial function and its preparation method, which uses chitosan to wrap and supercritical fluid to disperse antibacterial agent to prepare degradable film material for antibacterial, and uses wrapping polymer transportation and supercritical fluid treatment to disperse antibacterial particles in polymer resin master batch relatively uniformly. The obtained antibacterial biodegradable film product is safe and environment-friendly when being used for food packaging. However, the preparation process is complex, the material preparation needs to be carried out under high pressure, the cost is high, and meanwhile, the bacteriostatic performance does not have a slow release function. Patent ZL201410385522.8 discloses a preparation method of a non-migration and degradable antibacterial polyester film, wherein the degradable antibacterial polyester film is prepared by utilizing a high-molecular antibacterial agent, thermoplastic starch and biodegradable polyester, the method avoids the migration problem caused by simple blending of raw materials by utilizing the hydrogen bond effect formed among starch, a plasticizer and the high-molecular antibacterial agent, but the binding capacity of the composite material prepared by utilizing intermolecular force is only slightly higher than that of direct blending, and the method still has the migration risk compared with a chemical modification method. Therefore, the development of a preparation method of a chemical grafting modified biodegradable slow-release antibacterial preservative film for slow-release antibacterial preservative packaging products and the application of the preservative packaging products in fruits, vegetables, foods and the like is urgently needed.
The invention content is as follows:
the biodegradable slow-release antibacterial preservative film provided by the invention not only has biodegradation performance, but also has slow-release antibacterial performance, can prolong the service life of the antibacterial preservative film through the slow-release function, further prolongs the shelf life of fruits, vegetables, food and the like, and can be degraded by adopting compost after being used, thereby solving the problem of white pollution.
The invention aims to provide a biodegradable slow-release antibacterial preservative film which comprises the following components in parts by mass: 50-80 parts of matrix resin, 1-5 parts of coupling agent, 1-10 parts of bacteriostatic agent, 5-30 parts of inorganic porous material and 1-5 parts of processing aid.
The biodegradable slow-release antibacterial preservative film provided by the invention is simple in raw materials and preparation process, green and safe, the slow-release characteristic can be endowed with the introduction of the inorganic porous material, and the bacteriostatic function can be endowed with the introduction of the bacteriostatic auxiliary agent. The invention provides a concept for preparing a biodegradable slow-release antibacterial preservative film by utilizing an inorganic porous material and a bacteriostatic agent, and has creativity and important application value.
Preferably, the biodegradable slow-release antibacterial preservative film comprises the following components in parts by mass: 60-80 parts of matrix resin, 2-4 parts of coupling agent, 2-6 parts of bacteriostatic agent, 10-30 parts of inorganic porous material and 2-4 parts of processing aid.
Further preferably, the biodegradable slow-release antibacterial preservative film comprises the following components in parts by mass: 70 parts of matrix resin, 3 parts of coupling agent, 3 parts of bacteriostatic agent, 20 parts of inorganic porous material and 3 parts of processing aid.
Preferably, the matrix resin is selected from one or more of polybutylene terephthalate-adipate (PBAT), polylactic acid (PLA) and Polyhydroxyalkanoate (PHA). The matrix resin is commercial resin.
Preferably, the coupling agent is selected from one or more of KH550, KH-560 and KH 570.
Preferably, the bacteriostatic agent is guanidine bacteriostatic agent. The guanidine bacteriostatic agent comprises polyhexamethylene biguanide hydrochloride, and the polyhexamethylene guanidine hydrochloride has the advantages of no toxicity, wide bacteriostatic range, high bacteriostatic rate and the like.
Preferably, the inorganic porous material is one or more selected from activated carbon, white carbon black and diatomite. The mesh number of the inorganic porous material is more than 300 meshes. The inorganic porous material has hot points such as strong loading capacity and stable performance, and can greatly improve the bacteriostatic slow-release performance of the film by being uniformly dispersed in the film.
Preferably, the processing aid comprises a plasticizer and an antioxidant. The plasticizer is glycerol, polyethylene glycol 200, etc., and the antioxidant is 1010 or 168 of Basff company. More preferably, the mass ratio of the plasticizer to the antioxidant is 5-9, and when the plasticizer is glycerol and polyethylene glycol 200, the mass ratio of the plasticizer to the antioxidant is 4-8.
The invention also provides a preparation method of the biodegradable slow-release antibacterial preservative film, which comprises the following steps:
s1, preparing a slow-release antibacterial agent loaded by a chemical grafting modified inorganic porous material: mixing an inorganic porous material and a coupling agent, heating, controlling the temperature to be 60-80 ℃, keeping the temperature, stirring for 1-5min, adding an antibacterial agent after heating, and stirring for 4-6min under the condition of keeping the temperature condition unchanged to obtain a slow-release antibacterial agent loaded on the chemical graft modified inorganic porous material;
s2, premixing raw materials: putting matrix resin, a processing aid and the slow-release antibacterial agent loaded on the chemical grafting modified inorganic porous material obtained in the step S1 into a high-speed mixer for premixing, controlling the stirring speed to be 500-1200r/min, and keeping the temperature at 60-80 ℃ for 1-5min to obtain a master batch;
s3, continuous banburying extrusion: adding the master batch obtained in the step S2 into a continuous banburying extruder, controlling the temperature to be 150-180 ℃, controlling the revolution to be 100-300rpm, and extruding and pelletizing to obtain uniform granules;
s4, extrusion film forming: and (4) feeding the granules obtained in the step (S3) into a film blowing machine, uniformly blowing and forming a film, wherein the outlet temperature of the film blowing machine is 160-190 ℃, and thus obtaining the biodegradable slow-release antibacterial preservative film.
Compared with the existing biodegradable antibacterial fresh-keeping packaging film, the preparation method of the invention is simple, and simultaneously, the packaging film has the functions of bacteriostasis, slow release and the like.
In step S1, the inorganic porous material and the coupling agent are heated first, a large number of epoxy groups can be grafted on the surface of the inorganic porous material, the antibacterial agent is added, and the antibacterial agent and the epoxy groups react and are successfully grafted to the porous material, so as to obtain the slow-release antibacterial agent loaded on the chemically grafted and modified inorganic porous material (as shown in fig. 1).
Preferably, the temperature in the step S1 is 70 ℃, the stirring time is 4min, the antibacterial agent is added, and the stirring is continued for 5min under the condition that the temperature condition is kept unchanged; the stirring speed of the step S2 is 800r/min, and the temperature is kept at 70 ℃ for 4min; the temperature is controlled to be 160 ℃ in the step S3, and the revolution is controlled to be 200rpm; and the outlet temperature of the film blowing machine in the step S4 is 170 ℃.
The invention also protects the application of the biodegradable slow-release antibacterial preservative film in fruit and vegetable preservative packaging or food preservative packaging.
Compared with the prior art, the invention has the following advantages:
1. the biodegradable slow-release antibacterial preservative film disclosed by the invention is prepared by selecting one or more of biodegradable terephthalic acid-butanediol adipate (PBAT), polylactic acid (PLA) and Polyhydroxyalkanoate (PHA) as matrix resin and adopting a silane coupling agent, a bacteriostatic agent and an inorganic porous material as raw materials to prepare the slow-release antibacterial agent loaded on the inorganic porous material by utilizing a chemical grafting modification and coupling method, so that the slow-release antibacterial agent is endowed with bacteriostatic and slow-release functions.
2. The preparation process is simple and convenient, most of prepared raw materials are environment-friendly green materials, the bacteriostatic performance and the slow release performance of the film are regulated and controlled by controlling the adding amount of the bacteriostatic agent and the inorganic porous material, so that the defects that the traditional bacteriostatic packaging material is non-biodegradable, easy to precipitate and free of slow release function are overcome, and the antibacterial film can be widely applied to various fields.
Description of the drawings:
FIG. 1 is a reaction schematic diagram of a slow-release antibacterial agent loaded on a chemical grafting modified inorganic porous material;
FIG. 2 is a flow chart of the preparation of the biodegradable slow-release antibacterial preservative film.
The specific implementation mode is as follows:
the following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention. Unless otherwise specified, the experimental materials and reagents used herein are all conventional commercial products in the art.
Example 1
A biodegradable slow-release antibacterial preservative film comprises 500g of PBAT, 40g of glycerol, 200g of polyethylene glycol, 1010 g of antioxidant, 50g of KH550, 100g of polyhexamethylene biguanide hydrochloride and 300g of activated carbon.
As shown in fig. 1, the preparation method of the biodegradable slow-release antibacterial preservative film comprises the following steps:
s1, heating activated carbon and KH550, controlling the temperature at 70 ℃, keeping the temperature and stirring for 4min, adding polyhexamethylene biguanide hydrochloride, and stirring for 5min under the condition of continuously keeping the temperature condition unchanged to obtain a slow-release antibacterial agent loaded by the activated carbon;
s2, putting the PBAT, the glycerol, the polyethylene glycol 200, the antioxidant 1010 and the slow-release antibacterial agent loaded by the inorganic porous material prepared in the step S1 into a high-speed mixer, controlling the stirring speed to be 800r/min, and keeping the temperature at 70 ℃ for 4min to obtain a master batch;
s3, adding the master batch obtained in the step S2 into a continuous banburying extruder, controlling the temperature at 160 ℃, controlling the revolution at 200rpm, and extruding and pelletizing to obtain uniform granules;
and S4, feeding the granules obtained in the step S3 into a film blowing machine, uniformly blowing and forming a film, wherein the outlet temperature of the film blowing machine is 170 ℃, and thus obtaining the biodegradable slow-release antibacterial preservative film.
Example 2
A biodegradable slow-release antibacterial preservative film comprises PBAT 400g, PLA100 g, glycerin 40g, polyethylene glycol 200g, antioxidant 1010 5g, KH550 50g, polyhexamethylene biguanide hydrochloride 100g and white carbon black 300g.
The preparation method of the biodegradable antibacterial preservative film is the same as that of the example 1.
Example 3
A biodegradable slow-release antibacterial preservative film comprises PBAT 600g, PHA100g, glycerol 20g, polyethylene glycol 2005g, an antioxidant 1010 5g, KH560 30g, polyhexamethylene biguanide hydrochloride 40g and white carbon black 200g.
The preparation method of the biodegradable antibacterial preservative film is the same as that of the embodiment 1, and is characterized in that: step S1, keeping the temperature unchanged, continuing stirring for 6min, wherein the temperature is 60 ℃, and the stirring time is 5min; s2, keeping the stirring speed at 500r/min and keeping the temperature at 60 ℃ for 5min; s3, controlling the temperature to be 150 ℃ and controlling the revolution number to be 300rpm; and S4, setting the outlet temperature of the film blowing machine to be 160 ℃.
Example 4
A biodegradable slow-release antibacterial preservative film comprises PBAT 600g, PLA 100g, glycerol 20g, polyethylene glycol 2005g, an antioxidant 1010 5g, KH570 30g, polyhexamethylene biguanide hydrochloride 40g and diatomite 200g.
The preparation method of the biodegradable antibacterial preservative film is the same as that of the embodiment 1, and is characterized in that: s1, keeping the temperature unchanged, and continuing stirring for 4min, wherein the temperature is 80 ℃, and the stirring time is 1min; s2, keeping the stirring speed at 1200r/min and keeping the temperature at 80 ℃ for 1min; s3, controlling the temperature to be 180 ℃ and the revolution to be 100rpm; and S4, setting the outlet temperature of the film blowing machine to be 190 ℃.
Example 5
A biodegradable slow-release antibacterial preservative film comprises PBAT 600g, PLA 100g, glycerol 20g, polyethylene glycol 2005g, an antioxidant 1010 5g, KH550 30g, polyhexamethylene biguanide hydrochloride 40g and active carbon 200g.
The preparation method of the biodegradable antibacterial preservative film is the same as that of the example 1.
Example 6
A biodegradable slow-release antibacterial preservative film comprises PBAT 600g, PLA 200g, glycerol 40g, polyethylene glycol 2005g, an antioxidant 1010 5g, KH560 30g, polyhexamethylene biguanide hydrochloride 40g and white carbon black 80g.
The preparation method of the biodegradable antibacterial preservative film is the same as that of the example 1.
Comparative example 1
An antibacterial preservative film comprises PBAT 600g, PLA200 g, glycerol 40g, polyethylene glycol 200g, antioxidant 5g, polyhexamethylene biguanide hydrochloride 70g and white carbon black 80g.
The preparation method of the antibacterial preservative film is the same as that of the embodiment 1, except that: s1, heating white carbon black, controlling the temperature at 70 ℃, adding polyhexamethylene biguanide hydrochloride, and stirring for 4min under heat preservation to obtain the antibacterial agent loaded with white carbon black.
Comparative example 2
An antibacterial preservative film comprises PBAT 600g, PLA100 g, glycerol 40g, polyethylene glycol 200g, antioxidant 1010 g, KH560 30g and diatomite 220g.
The preparation method of the antibacterial preservative film is the same as that of the embodiment 1, except that: s1, heating diatomite and KH560 at 70 ℃, and stirring for 4min under heat preservation to obtain the modified inorganic porous material.
Comparative example 3
An antibacterial preservative film comprises PBAT 600g, PHA200 g, glycerol 40g, polyethylene glycol 200g, antioxidant 1010 g, KH570 50g and polyhexamethylene biguanide hydrochloride 100g.
The preparation method of the antibacterial preservative film is the same as that of the embodiment 1, except that: s1, heating KH570 and polyhexamethylene biguanide hydrochloride, controlling the temperature at 70 ℃, keeping the temperature and stirring for 4min, and then drying and grinding at 100 ℃ into powder for later use.
Comparative example 4
An antibacterial preservative film comprises PBAT 600g, PLA 200g, glycerol 40g, polyethylene glycol 2005g, antioxidant 1010 5g and polyhexamethylene biguanide hydrochloride 70g.
The preparation method of the antibacterial preservative film comprises the following steps:
s1, weighing each component consisting of PBAT, PLA, glycerol, polyethylene glycol 200, an antioxidant 1010 and polyhexamethylene biguanide hydrochloride, putting the raw materials into a high-speed mixer, controlling the stirring speed to be 800r/min, and keeping the temperature at 70 ℃ for 4min to obtain a master batch;
s2, adding the master batch obtained in the step S1 into a continuous banburying extruder, controlling the temperature at 160 ℃, controlling the revolution at 200rpm, and extruding and pelletizing to obtain uniform granules;
and S3, feeding the granules obtained in the step S2 into a film blowing machine, uniformly blowing and forming a film, wherein the outlet temperature of the film blowing machine is 170 ℃, and thus obtaining the antibacterial preservative film.
Comparative example 5
An antibacterial preservative film comprises PBAT 600g, PLA 200g, glycerol 40g, polyethylene glycol 2005g, antioxidant 1010 5g and white carbon black 80g.
The preparation method of the antibacterial preservative film comprises the following steps:
s1, weighing various components consisting of raw materials, namely PBAT, PLA, glycerol, polyethylene glycol 200, an antioxidant 1010 and white carbon black, putting the raw materials into a high-speed mixer, controlling the stirring speed to be 800r/min, and keeping the temperature at 70 ℃ for 4min to obtain a master batch;
s2, adding the master batch obtained in the step S1 into a continuous internal mixing extruder, controlling the temperature at 160 ℃, controlling the revolution at 200rpm, and extruding and granulating to obtain uniform granules;
and S3, feeding the granules obtained in the step S2 into a film blowing machine, uniformly blowing and forming a film, wherein the outlet temperature of the film blowing machine is 170 ℃, and thus obtaining the antibacterial preservative film.
The ratio of the amounts of the components of examples 1 to 6 and comparative examples 1 to 5 is shown in Table 1:
TABLE 1
Experimental example 1 characterization of the properties of the temperature responsive coatings of examples 1-6
1. Experimental methods
And (3) testing mechanical properties:
the method for testing the tensile property of the plastic film is based on the GB/T13022-1991 test method, and the test method is carried out by adopting a universal tensile machine and comprises the following steps:
the plastic film was cut with a die cutter to prepare specimens of size 10mm × 100mm.
And testing the thickness of the sample strip to be tested by using a thickness tester, then installing the sample strip in a tensile machine testing area, inputting the thickness for testing, and automatically obtaining data such as tensile strength, elongation at break and the like.
And (3) testing the antibacterial performance: and (3) testing the bacteriostatic circle of the sample by taking GB/T39101-2020 as a standard, and judging the antibacterial effect according to the size of the bacteriostatic circle. And then, the test sample is taken off and cleaned, the bacteriostatic zone test is repeated for two times, and the bacteriostatic slow-release performance of the test sample is tested.
2. Results of the experiment
The results of the performance tests for each sample are shown in table 2.
TABLE 2
Comprehensive mechanical property, antibacterial property and antibacterial slow-release property are sequentially ranked as follows: example 5 > 3 > 4 > 6 > 2 > 1. Comparative examples 1 and 2 show that introduction of PLA can reduce elongation at break of the film and has little influence on the bacteriostatic performance, and comparative examples 1-6 show that addition of a bacteriostatic agent can improve the bacteriostatic performance of the film, but addition of a bacteriostatic agent increases the cost on one hand, and easily causes precipitation of the bacteriostatic agent on the other hand, and comparative examples 3-5 show that the most excellent bacteriostatic slow-release performance is activated carbon, and then white carbon black and diatomite are added, so that the overall performance is considered, and the addition proportion in example 5 is the optimum addition proportion.
Comparative example 1 shows that the addition of the coupling agent can enable the bacteriostatic agent to be better loaded on the porous material and endow the film with bacteriostatic slow-release performance, comparative example 2 shows that the addition of the bacteriostatic auxiliary agent can endow the film with bacteriostatic performance, comparative example 3 shows that the bacteriostatic slow-release performance of the film after the porous material is improved, but the bacteriostatic slow-release functional effect is not as good as that in examples 1-5 when a small amount of the porous material is added in comparative example 1, comparative examples 4 and 5 show that the bacteriostatic performance of the film after grafting without chemical reaction can not be kept stable, the size of a bacteriostatic zone is sharply reduced after multiple tests, and meanwhile, compared with comparative examples 1, 4, 5 and examples, the chemical grafting modification can ensure that the prepared film can keep excellent bacteriostatic performance and can keep long-acting bacteriostatic.
The above embodiments are only for the purpose of helping understanding the technical solution of the present invention and the core idea thereof, and it should be noted that those skilled in the art can make several improvements and modifications to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims (10)
1. The biodegradable slow-release antibacterial preservative film is characterized by comprising the following components in parts by mass: 50-80 parts of matrix resin, 1-5 parts of coupling agent, 1-10 parts of bacteriostatic agent, 5-30 parts of inorganic porous material and 1-5 parts of processing aid.
2. The biodegradable slow-release antibacterial preservative film according to claim 1, characterized by comprising the following components in parts by mass: 60-80 parts of matrix resin, 2-4 parts of coupling agent, 2-6 parts of bacteriostatic agent, 10-30 parts of inorganic porous material and 2-4 parts of processing aid.
3. The biodegradable slow-release antibacterial preservative film according to claim 2, characterized by comprising the following components in parts by mass: 70 parts of matrix resin, 3 parts of coupling agent, 3 parts of bacteriostatic agent, 20 parts of inorganic porous material and 3 parts of processing aid.
4. The biodegradable slow-release antibacterial preservative film according to any one of claims 1 to 3, wherein the matrix resin is one or more selected from the group consisting of butylene terephthalate-adipate, polylactic acid and polyhydroxyalkanoate.
5. The biodegradable slow-release antibacterial preservative film according to any one of claims 1 to 3, wherein the coupling agent is selected from one or more of KH550, KH-560 and KH 570.
6. The biodegradable slow-release antibacterial preservative film according to any one of claims 1 to 3, wherein the bacteriostatic agent is a guanidine bacteriostatic agent.
7. The biodegradable slow-release antibacterial preservative film according to any one of claims 1 to 3, wherein the inorganic porous material is one or more selected from activated carbon, white carbon black and diatomite.
8. The biodegradable slow-release antibacterial plastic wrap according to any one of claims 1-3, wherein said processing aid comprises a plasticizer and an antioxidant.
9. The method for preparing the biodegradable slow-release antibacterial preservative film according to any one of claims 1 to 8, characterized by comprising the steps of:
s1, preparing a slow-release antibacterial agent loaded by a chemical grafting modified inorganic porous material: mixing an inorganic porous material and a coupling agent, heating, controlling the temperature to be 60-80 ℃, keeping the temperature, stirring for 1-5min, adding an antibacterial agent after heating, and stirring for 4-6min under the condition of keeping the temperature condition unchanged to obtain a slow-release antibacterial agent loaded on the chemical graft modified inorganic porous material;
s2, premixing raw materials: putting matrix resin, a processing aid and the slow-release antibacterial agent loaded on the chemical grafting modified inorganic porous material obtained in the step S1 into a high-speed mixer for premixing, controlling the stirring speed to be 500-1200r/min, and keeping the temperature at 60-80 ℃ for 1-5min to obtain a master batch;
s3, continuous banburying extrusion: adding the master batch obtained in the step S2 into a continuous banburying extruder, controlling the temperature to be 150-180 ℃, controlling the revolution to be 100-300rpm, and extruding and pelletizing to obtain uniform granules;
s4, extrusion film forming: and (4) feeding the granules obtained in the step (S3) into a film blowing machine, uniformly blowing and forming a film, wherein the outlet temperature of the film blowing machine is 160-190 ℃, and thus the biodegradable slow-release antibacterial preservative film is obtained.
10. The use of the biodegradable slow-release antibacterial preservative film according to any one of claims 1 to 8 in fruit and vegetable freshness-retaining packaging or food freshness-retaining packaging.
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| CN113121841A (en) * | 2021-04-21 | 2021-07-16 | 上海玉城高分子材料股份有限公司 | Inorganic composite guanidine salt polymer antibacterial agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101836655A (en) * | 2010-04-20 | 2010-09-22 | 华南理工大学 | Functionalization inorganic antibiosis material and preparation method thereof |
| CN108752884A (en) * | 2018-05-31 | 2018-11-06 | 广东轻工职业技术学院 | A kind of high antibiotic property PLA/PBAT materials and the preparation method and application thereof |
| CN109438937A (en) * | 2018-09-29 | 2019-03-08 | 万卓（武汉）新材料有限公司 | A kind of antimicrobial form PLA base degradable food packaging material and preparation method thereof |
| CN110835457A (en) * | 2019-11-15 | 2020-02-25 | 上海海洋大学 | Full-biomass porous material slow-release antibacterial active preservative film and preparation method thereof |
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