CN112662145B - Bacteriostatic degradable respiratory membrane with self-contraction performance, preparation method and application - Google Patents
Bacteriostatic degradable respiratory membrane with self-contraction performance, preparation method and application Download PDFInfo
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- CN112662145B CN112662145B CN202011519242.3A CN202011519242A CN112662145B CN 112662145 B CN112662145 B CN 112662145B CN 202011519242 A CN202011519242 A CN 202011519242A CN 112662145 B CN112662145 B CN 112662145B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
The invention belongs to the technical field of high polymer materials, and particularly relates to a bacteriostatic degradable respiratory membrane with self-contraction performance, a preparation method and application thereof. The completely degradable bacteriostatic breathing film provided by the invention has a bacteriostatic function and a self-generating air-conditioning function. Meanwhile, the invention has the characteristics of good toughness, difficult fracture, convenient production and use, high biodegradation speed and the like. The membrane material is prepared by blending multiple materials or all materials in poly terephthalic acid-adipic acid-butylene glycol ester (PBAT), L-polylactic acid (PLLA), poly Butylene Succinate (PBS), polycaprolactone (PCL), a chain extender, nano titanium dioxide, nano silicon dioxide, chitosan and calcium propionate.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a bacteriostatic degradable respiratory membrane with self-contraction performance, a preparation method and application thereof.
Background
The plastic film generally refers to a sheet-like or roll-like film having a thickness of 0.25mm or less and mainly made of a plastic material. The annual output of Chinese plastic films is about 1600 ten thousand tons, the recovery rate of waste plastic films is less than 30 percent every year, a large amount of waste plastic films are not effectively treated, and serious environmental pollution is caused. Although the latest version of "plastic restricted order" was released at 20.1.2020, 80% of businesses are currently using traditional plastic packaging, including many food manufacturers. Most enterprises lack advanced green packaging technology and environmental awareness, so that more and more plastic packaging wastes are generated, the environment is greatly influenced, and the prohibition and restriction of the state on the non-degradable plastics are not met.
The raw materials of the traditional plastic film are organic high molecular compounds, the structure of the traditional plastic film is stable, the traditional plastic film is not easily degraded by natural microorganisms, and the natural decay of a non-degradable plastic bag needs more than 200 years. If the waste plastic bags are not recycled, the waste plastic bags are mixed in the soil to cause soil hardening, which influences the nutrient and water absorption of crops and leads to crop yield reduction. Waste plastic bags discarded on land and in water bodies can be swallowed by animals, fishes and the like as food, so that the animals and the fishes die or the growth of the animals and the fishes is influenced.
At present, a plurality of non-degradable films are applied to fresh-keeping packaging of fresh foods in the market, and mainly comprise Low Density Polyethylene (LDPE), linear Low Density Polyethylene (LLDPE), high Density Polyethylene (HDPE), polypropylene (PP), polyvinylidene chloride (PVDC), nylon (PA) and the like. These materials have the advantages of high flexibility, chemical resistance, transparency, easy processing and the like, but have CO resistance 2 、O 2 Has poor barrier property and small gas selective permeation ratio, and is difficult to meet the packaging requirement of fresh food. Meanwhile, materials such as PE and PA have poor water vapor permeability, and dew condensation is likely to occur in the packaging bag, so that microorganisms are bred, and the packaging bag is deteriorated. Compared with common materials, the degradable material is healthy and harmless to people or the environment in the whole life cycle of the package. The common degradable materials applied to the modified atmosphere packaging of fresh foods in the current market are mainly modifiedThe subsequent polylactic acid (PLA), full starch polymer plastic, polycaprolactone (PCL) and the like. Different kinds of degradable materials have different superior properties, and the materials are separately used in modified atmosphere packaging of fruits and vegetables and have certain limitation. For example, polylactic acid has a good gas barrier property, so that it cannot be applied to packaging of fruits and vegetables with a high respiratory rate, and has mechanical properties similar to Polystyrene (PS), and is prone to brittle fracture. Therefore, the polymers are usually required to be blended and modified to change the mechanical properties and barrier properties, so that the polymers are applied to modified atmosphere packaging of fruits and vegetables.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a bacteriostatic degradable respiratory membrane with self-contraction performance, a preparation method and application thereof, and aims to solve part of problems in the prior art or at least alleviate part of problems in the prior art. The completely degradable bacteriostatic respiratory membrane provided by the invention has a bacteriostatic function and a self-regulating function. Meanwhile, the invention has the characteristics of good toughness, difficult fracture, convenient production and use, high biodegradation speed and the like.
The invention is realized in such a way that the bacteriostatic degradable respiratory membrane with self-contraction performance comprises the following components in parts by weight:
further, the PCL also comprises 5-10 parts.
Further, the nano titanium oxide powder also comprises 0.25-2.5 parts of nano titanium oxide.
Further, 0.25-2.5 parts of nano silicon oxide is also included.
Further, the feed also comprises 0.5-5 parts of calcium propionate.
PBAT, PLLA, PBS and PCL are all biodegradable materials, the tail end of the PBAT is provided with a reaction group, the PBAT can react with a chain extender under the melting condition, and the number average molecular weight of the PBAT, the PLLA, the PBS and the PCL ranges from 150000 to 250000.
The invention also provides a preparation method of the bacteriostatic degradable respiratory membrane with self-contraction performance, which comprises the following steps:
s1: stirring and mixing the dried PBAT, PLLA, PBS, PCL, a chain extender, nano titanium oxide and nano silicon oxide;
s2: adding the uniformly mixed materials into a granulator, extruding, bracing, cooling, shearing and granulating to obtain a special master batch capable of completely degrading the antibacterial breathing membrane;
s3: adding the special master batch of the completely degradable bacteriostatic breathing film into a double-screw casting extruder at a feeding port for casting extrusion, cooling and drawing, and rolling after or without secondary stretching to obtain the degradable breathing film;
s4: dissolving chitosan and calcium propionate in 0.1% acetic acid water solution, stirring uniformly, coating chitosan on the surface of the degradable respiratory membrane uniformly by using a coating machine, and naturally drying to obtain the completely degradable antibacterial respiratory membrane.
Further, the vacuum drying temperature of the materials is 60-80 ℃, and the drying time is 24-48h.
Further, a mixer is used for mixing in the step S1, the rotating speed of the mixer is 150-200rpm/min, and the mixing time is 5-10min.
Further, in the step S2, the temperature range of the granulator is 150-200 ℃, the temperature of the die head is 190-210 ℃, and the size of the granulated master batch is about 2-3mm; in the step S3, the heating temperature range of the twin-screw casting extruder is 160-220 ℃, the die head temperature is 200-220 ℃, and the film thickness is 25 +/-5 mu m.
The invention also provides application of the antibacterial degradable breathing film with self-contraction performance in preparation of the degradable antibacterial packaging and transporting paper-plastic box.
In summary, the advantages and positive effects of the invention are as follows:
the modified atmosphere packaging (EMAP) is characterized in that in the storage process, no manual operation is needed, the gas components in the packaging are completely regulated through the selective permeability of the film to gas and the respiration of fruits and vegetables, the dynamic balance is finally achieved, and the stable and proper atmosphere in the packaging is kept. The fresh fruit and vegetable fresh-keeping agent can effectively inhibit physiological metabolism of fresh fruits and vegetables and delay aging, is convenient to operate and obvious in fresh-keeping effect, and can be used for prolonging shelf life and keeping flavor and nutrient substances to a greater extent. At present, in the fields of food packaging and transportation and the like, the packaging material is urgently expected to have good antibacterial performance, inhibit the growth and the propagation of microorganisms in the package and prolong the fresh-keeping period of fresh fruits and vegetables. And no such products are currently available on the market.
The degradable material commonly used in the market at present, such as polybutylene terephthalate-adipate terephthalate (PBAT), is a completely biodegradable material, and the white pollution can be resisted and the harm to the environment can be reduced by using the PBAT. PBAT has good ductility and elongation at break, but has high toughness and viscosity after film forming, is easy to adhere to each other, has influence on use, and needs to be modified.
Materials like poly (L-lactic acid) (PLLA), poly (butylene succinate) (PBS), polycaprolactone (PCL), etc. also have the following advantages: the PLLA and the PCL have good biocompatibility and biodegradability, but the crystallinity and the glass transition temperature of the PLLA and the PCL are lower, meanwhile, the materials have large brittleness and poor processability, and the PLLA and the PCL are generally used by blending and modifying with other materials.
Drawings
FIG. 1 is a design drawing of a paper-plastic box body;
FIG. 2 is a graph showing the change in the total number of colonies before and after storage of a sample;
FIG. 3 is a graph showing the change of oxygen in the packaging before and after the kiwi fruit is packaged and stored;
FIG. 4 is a graph of the change of carbon dioxide in the packaging before and after the kiwi fruit is packaged and stored;
FIG. 5 is a graph showing the change in oxygen in the package before and after storage of the mango package;
FIG. 6 is a graph showing the change in carbon dioxide in the package before and after storage of the mango package;
FIG. 7 is a graph showing the change of oxygen in the package before and after the strawberry is packaged and stored;
FIG. 8 is a graph showing the change in carbon dioxide in the package before and after packaging and storage of strawberries;
FIG. 9 shows the tensile properties of the products of the examples.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the apparatuses and reagents used in the examples and test examples are commercially available without specific reference. The specific embodiments described herein are merely illustrative of the invention and do not delimit the invention.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
For a better understanding of the invention, without limiting the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques. In the present invention, "about" means within 10%, preferably within 5% of a given value or range.
The invention discloses a preparation method and application of a bacteriostatic degradable respiratory membrane with self-contraction performance. The details are shown in the following examples.
Example 1 preparation of degradable bacteriostatic respiratory membranes
70 parts of PBAT,20 parts of PLLA,10 parts of PBS and 0.2 part of chain extender are prepared into the degradable respiratory membrane. Stirring a mixer: 150rpm/min, 5min, twin screw extruder barrel temperature: cartridge 1:180 ℃, cartridge 2:185 ℃, barrel 3:190 ℃, barrel 4-5:200 ℃, cartridge 6-9:210 ℃, quick change zone: 210 ℃ C: die head 123: at 210 ℃. And extruding, cooling, drawing and rolling to obtain the degradable breathing membrane.
Dissolving 2 parts of chitosan in 1000 parts of 0.1% acetic acid aqueous solution, uniformly stirring, uniformly coating the chitosan on the surface of the degradable breathing membrane by using a film coating machine, and naturally drying to obtain the completely degradable antibacterial breathing membrane.
Example 2 preparation of degradable bacteriostatic respiratory membranes
60 parts of PBAT,28 parts of PLLA,10 parts of PBS,2 parts of PCL,0.1 part of chain extender and 0.25 part of nano silicon oxide are prepared into the degradable respiratory membrane. Stirring a mixer: 180rpm/min, 5min, twin screw extruder barrel temperature: cartridge 1:170 ℃, cartridge 2:180 ℃, cartridge 3:190 ℃, cartridge 4:200 ℃, cartridge 5:210 ℃, cartridge 6-9:220 ℃, quick change zone: 220 ℃ C: die head 123: at 220 deg.c. And extruding, cooling, drawing and rolling to obtain the degradable respiratory membrane.
Dissolving 2 parts of chitosan into 1000 parts of 0.1% acetic acid aqueous solution, uniformly stirring, uniformly coating the chitosan on the surface of the degradable breathing membrane by using a coating machine, and naturally drying to obtain the completely degradable antibacterial breathing membrane.
Example 3 preparation of degradable bacteriostatic respiratory membranes
Preparing 60 parts of PBAT,28 parts of PLLA,10 parts of PBS,2 parts of PCL,0.1 part of chain extender, 0.25 part of nano silicon oxide and 0.25 part of nano titanium oxide into the degradable respiratory membrane. Stirring a mixer: 180rpm/min, 5min, twin screw extruder barrel temperature: cartridge 1:170 ℃, cartridge 2:180 ℃, cartridge 3:190 ℃, cartridge 4:200 ℃, cartridge 5:210 ℃, cartridge 6-9:220 ℃, quick change zone: 220 ℃ of: die head 123: at 220 ℃. And extruding, cooling, drawing and rolling to obtain the degradable breathing membrane.
Dissolving 2 parts of chitosan in 1000 parts of 0.1% acetic acid aqueous solution, uniformly stirring, uniformly coating the chitosan on the surface of the degradable breathing membrane by using a film coating machine, and naturally drying to obtain the completely degradable antibacterial breathing membrane.
Example 4 preparation of degradable bacteriostatic respiratory membranes
Preparing 60 parts of PBAT,28 parts of PLLA,10 parts of PBS,2 parts of PCL,0.1 part of chain extender, 0.25 part of nano silicon oxide and 0.25 part of nano titanium oxide into the degradable respiratory membrane. Stirring a mixer: 180rpm/min, 5min, twin screw extruder barrel temperature: cartridge 1:170 ℃, cartridge 2:180 ℃, cartridge 3:190 ℃, cartridge 4:200 ℃, cartridge 5:210 ℃, cartridge 6-9:220 ℃, quick change zone: 220 ℃ C: die head 123: at 220 ℃. The degradable respiratory membrane is obtained by extrusion, cooling, traction and rolling.
Dissolving 2 parts of chitosan and 2 parts of calcium propionate in 1000 parts of 0.1% acetic acid aqueous solution, uniformly stirring, uniformly coating the chitosan on the surface of the degradable respiratory membrane by using a coating machine, and naturally drying to obtain the completely degradable antibacterial respiratory membrane.
Example 5 preparation of completely degradable bacteriostatic respiratory film paper-plastic box
The method specifically comprises the following steps:
the step (1) designs and produces a corrugated case with the volume of 10.5L, the size of the case body is (35 cm multiplied by 20cm multiplied by 15 cm), and the corrugated paper sheet is punched and formed on a punch by utilizing the whole piece of corrugated paper. The carton body layout is shown in fig. 1.
Cutting the prepared degradable antibacterial breathing membrane into a proper size, bonding the membrane with a corrugated case by using glue, and then airing to prepare the degradable antibacterial breathing paper-plastic composite board.
And (3) folding and bonding the degradable antibacterial respiratory paper-plastic composite board into a paper-plastic box, adhering the paper-plastic box hermetically, only reserving one surface for packaging fresh fruits and vegetables, sealing the fresh fruits and vegetables after packaging the fresh fruits and vegetables, and sealing the whole box without reserving gaps.
Application example 1
Selecting mango, strawberry and kiwi fruit as experimental objects, and selecting, precooling, bagging and refrigerating three selected fruits. The selected fruits were divided into 5 groups. Group 1 was unpacked (exposed directly to air and placed in a freezer along with the control group) and group 4 was packed as four examples, with group 5 experimental fruits placed in a freezer at 4 ℃ and 85-90% humidity, the results are shown in FIGS. 2-8. Wherein the paper-plastic case was the case prepared in example 5 and the film prepared in example 4 was used; examples 2-4 were cut to size, the edges of the film were sealed with a heat sealer to leave a single side open, and the opening was heat sealed with a heat sealer after the fruit and vegetable were packaged to leave a relatively sealed environment inside the package.
As can be seen from the figure, the degradable antibacterial breathing film prepared by the invention can prolong the fruit fresh-keeping period, effectively inhibit fruit respiration and inhibit bacterial growth.
Application example 2
Selecting mango, strawberry and kiwi fruit as experimental objects, and selecting, precooling, bagging, refrigerating and storing at normal temperature for three selected fruits. The selected fruits were divided into 2 groups. One group is a non-packaging group, the other group is a paper-plastic box packaging group, and the commercial package is made of PE materials. The experimental fruits of each group were placed in a freezer at 4 ℃ and 85-90% humidity, and the results are shown in FIGS. 2-8.
As can be seen from the figure, the degradable antibacterial breathing film paper-plastic box prepared by the invention can prolong the fruit fresh-keeping period, effectively inhibit fruit respiration and inhibit bacterial growth.
The results of measuring the tensile properties of the films prepared in the respective examples are shown in FIG. 9. As can be seen from the figure, the film prepared by the invention has better tensile property, the packaging capacity is determined by the tensile property of the material, and the better the tensile property is, the more excellent the packaging performance is.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A preparation method of a bacteriostatic degradable respiratory membrane with self-contraction performance is characterized by comprising the following steps:
s1: stirring and mixing 60 parts of dried PBAT,28 parts of PLLA,10 parts of PBS,2 parts of PCL,0.1 part of chain extender, 0.25 part of nano silicon oxide and 0.25 part of nano titanium oxide;
s2: adding the uniformly mixed materials into a granulator, extruding, bracing, cooling, and shearing for granulation to obtain a special master batch capable of completely degrading the antibacterial breathing membrane;
s3: adding the special master batch of the completely degradable antibacterial breathing membrane into a double-screw casting extruder at a feeding port for casting extrusion, cooling and drawing, and rolling to obtain the degradable breathing membrane;
s4: dissolving 2 parts of chitosan and 2 parts of calcium propionate in 1000 parts of 0.1% acetic acid aqueous solution, uniformly stirring, uniformly coating the chitosan on the surface of the degradable respiratory membrane by using a coating machine, and naturally drying to obtain the completely degradable antibacterial respiratory membrane;
wherein, the temperature of the twin-screw casting extruder is as follows: cartridge 1:170 ℃, cartridge 2:180 ℃, cartridge 3:190 ℃, cartridge 4:200 ℃, cartridge 5:210 ℃, cartridge 6-9:220 ℃, quick change zone: 220 ℃, die head 123: at 220 ℃.
2. The method for preparing the bacteriostatic degradable respiratory membrane with the self-contraction performance according to the claim 1, wherein the method comprises the following steps: the vacuum drying temperature of the material is 60-80 ℃, and the drying time is 24-48h.
3. The method for preparing the bacteriostatic degradable respiratory membrane with the self-contraction performance according to the claim 1, wherein the method comprises the following steps: in the step S1, a mixer is used for mixing materials, the rotating speed of the mixer is 150-200rpm/min, and the mixing time is 5-10min.
4. The method for preparing the bacteriostatic degradable respiratory membrane with self-contraction property according to claim 1, wherein the method comprises the following steps: in the step S2, the temperature range of the granulator is 150-200 ℃, the temperature of the die head is 190-210 ℃, and the size of the granulated master batch is about 2-3mm; the thickness of the film in step S3 is 25 +/-5 μm.
5. Use of the bacteriostatic degradable respiratory film with self-shrinking property of any one of claims 1-4 in the preparation of degradable bacteriostatic packaging and transporting paper-plastic boxes.
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| CN113248880A (en) * | 2021-05-23 | 2021-08-13 | 贵州省材料产业技术研究院 | Biodegradable gas-regulating film for prolonging shelf life of fruits and preparation method thereof |
| CN115710409A (en) * | 2022-08-12 | 2023-02-24 | 武汉轻工大学 | Bio-based antibacterial packaging film and preparation method thereof |
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