CN113354853A - Biodegradable high-barrier antibacterial composite membrane and preparation method thereof - Google Patents
Biodegradable high-barrier antibacterial composite membrane and preparation method thereof Download PDFInfo
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- CN113354853A CN113354853A CN202110740912.2A CN202110740912A CN113354853A CN 113354853 A CN113354853 A CN 113354853A CN 202110740912 A CN202110740912 A CN 202110740912A CN 113354853 A CN113354853 A CN 113354853A
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- polylactic acid
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- antibacterial
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 239000012528 membrane Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 96
- 239000004626 polylactic acid Substances 0.000 claims abstract description 96
- 239000001913 cellulose Substances 0.000 claims abstract description 71
- 229920002678 cellulose Polymers 0.000 claims abstract description 71
- 238000007790 scraping Methods 0.000 claims abstract description 23
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 21
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 239000012754 barrier agent Substances 0.000 claims abstract description 11
- 230000004888 barrier function Effects 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000010345 tape casting Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000005266 casting Methods 0.000 claims description 39
- 239000002121 nanofiber Substances 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 30
- 238000009210 therapy by ultrasound Methods 0.000 claims description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- -1 polytetrafluoroethylene Polymers 0.000 claims description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 238000009423 ventilation Methods 0.000 claims description 15
- 229920001661 Chitosan Polymers 0.000 claims description 12
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims description 12
- 239000000341 volatile oil Substances 0.000 claims description 12
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- 238000000576 coating method Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
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- 229940093612 zein Drugs 0.000 claims description 11
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 7
- 235000019486 Sunflower oil Nutrition 0.000 claims description 7
- 108010046377 Whey Proteins Proteins 0.000 claims description 7
- 102000007544 Whey Proteins Human genes 0.000 claims description 7
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- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000002600 sunflower oil Substances 0.000 claims description 7
- 235000021119 whey protein Nutrition 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000010676 Ocimum basilicum Nutrition 0.000 claims description 6
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- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 claims description 4
- 244000269722 Thea sinensis Species 0.000 claims description 4
- 229940117916 cinnamic aldehyde Drugs 0.000 claims description 4
- KJPRLNWUNMBNBZ-UHFFFAOYSA-N cinnamic aldehyde Natural products O=CC=CC1=CC=CC=C1 KJPRLNWUNMBNBZ-UHFFFAOYSA-N 0.000 claims description 4
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 claims description 4
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 4
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 4
- 235000013824 polyphenols Nutrition 0.000 claims description 4
- 229940090181 propyl acetate Drugs 0.000 claims description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- 235000013628 Lantana involucrata Nutrition 0.000 claims description 3
- 235000006677 Monarda citriodora ssp. austromontana Nutrition 0.000 claims description 3
- 240000007673 Origanum vulgare Species 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- 235000002566 Capsicum Nutrition 0.000 claims description 2
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 claims description 2
- 239000006002 Pepper Substances 0.000 claims description 2
- 235000016761 Piper aduncum Nutrition 0.000 claims description 2
- 235000017804 Piper guineense Nutrition 0.000 claims description 2
- 244000203593 Piper nigrum Species 0.000 claims description 2
- 235000008184 Piper nigrum Nutrition 0.000 claims description 2
- 239000002981 blocking agent Substances 0.000 claims description 2
- 229940045110 chitosan Drugs 0.000 claims description 2
- 229940043350 citral Drugs 0.000 claims description 2
- 229940109262 curcumin Drugs 0.000 claims description 2
- 235000012754 curcumin Nutrition 0.000 claims description 2
- 239000004148 curcumin Substances 0.000 claims description 2
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 claims description 2
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- 229940071440 soy protein isolate Drugs 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 6
- 239000000835 fiber Substances 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 abstract description 3
- 238000004806 packaging method and process Methods 0.000 abstract description 3
- 229920001046 Nanocellulose Polymers 0.000 abstract description 2
- 229960001701 chloroform Drugs 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 4
- 150000004676 glycans Chemical class 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920001282 polysaccharide Polymers 0.000 description 4
- 239000005017 polysaccharide Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 108010073771 Soybean Proteins Proteins 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
- 229920006255 plastic film Polymers 0.000 description 3
- 235000019710 soybean protein Nutrition 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241001529744 Origanum Species 0.000 description 1
- 235000011203 Origanum Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920006381 polylactic acid film Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
Classifications
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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
-
- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
-
- 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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
-
- 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
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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
- C08J2405/08—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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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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
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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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
- C08J2489/00—Characterised by the use of proteins; 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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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
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Biological Depolymerization Polymers (AREA)
- Laminated Bodies (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention belongs to the technical field of food packaging, and particularly relates to a biodegradable high-barrier antibacterial composite film and a preparation method thereof, wherein the biodegradable high-barrier antibacterial composite film comprises the following raw materials in parts by weight: 100 parts of polylactic acid, 0.5-10 parts of nano cellulose fiber, 1-10 parts of plasticizer, 3-35 parts of barrier agent and 2-35 parts of antibacterial agent. The invention relates to a biodegradable high-barrier antibacterial composite film which is prepared by taking nano-cellulose composite polylactic acid as a base material, adding barrier substances, antibacterial substances and a plasticizer and adopting a tape casting or film scraping mode. The preparation method is simple and effective, and the prepared biodegradable high-barrier antibacterial composite membrane has the advantages of good barrier property, good mechanical property, obvious antibacterial property and biodegradability.
Description
Technical Field
The invention belongs to the technical field of food packaging, and particularly relates to a biodegradable high-barrier antibacterial composite film and a preparation method thereof.
Background
Polylactic acid is a novel and environment-friendly degradable aliphatic polyester polymer material, has better mechanical strength, excellent biocompatibility and degradability, is safe and nontoxic, can be composted and degraded, can not cause any pollution to the environment because the final degradation products after use are carbon dioxide and water, is easy to process and form, has high transparency and visibility, and has very wide market prospect. At present, food packaging bags, preservative films, lunch box appliances and the like which take polylactic acid as a base material are developed at home and abroad. Peroxide crosslinked biodegradable polylactic acid foam plastic and chain extender-containing biodegradable polylactic acid foam plastic are developed by the Changchun applied chemistry research institute of Chinese academy of sciences, and the like, have excellent physical properties and can be completely biodegraded after being used.
Although the polylactic acid material is simple and convenient to synthesize and easy to process into various products, the waste after being used can not cause harm to human bodies or environment in the aspect of waste treatment, and the polylactic acid material conforms to the trend of current social development. However, polylactic acid materials have poor gas barrier properties, poor thermal stability, poor ductility, and no antibacterial properties. These factors all limit the wide application of polylactic acid in food packaging materials to a certain extent.
Disclosure of Invention
In order to solve the problems of the existing polylactic acid film material, the invention provides a biodegradable high-barrier antibacterial composite film and a preparation method thereof, and the obtained biodegradable high-barrier plastic film material has the characteristics of good mechanical property, high barrier property, antibacterial property, good biodegradability and the like.
The invention relates to a biodegradable high-barrier antibacterial composite film which comprises the following raw materials in parts by weight: 100 parts of polylactic acid, 0.5-10 parts of cellulose nano-fiber, 1-10 parts of plasticizer, 3-35 parts of barrier agent and 2-45 parts of antibacterial agent.
The barrier agent is selected from polyvinyl alcohol or ethylene-vinyl alcohol copolymer or acrylic ester or pullulan polysaccharide or chitosan or soybean protein isolate or whey protein concentrate or zein or a mixture thereof. Wherein the pullulan and chitosan have certain antibacterial effect, and the polyvinyl alcohol has good biocompatibility, fragrance retention property and degradability.
The plasticizer is selected from glycerol or polyethylene glycol or acetyl tributyl citrate or span80 or epoxidized soybean oil or epoxidized sunflower oil.
The antibacterial agent comprises a natural antibacterial agent and an inorganic metal antibacterial agent; wherein the natural antibacterial agent is selected from chitosan or sodium alginate or cinnamaldehyde or tea polyphenols or oregano essential oil or basil essential oil or pepper flower essential oil or thymol or citral or curcumin or their mixture; the inorganic metal antibacterial agent is selected from Nano-TiO2Or Nano-ZnO or Nano-Ag or a mixture thereof. When the natural antibacterial agent and the inorganic metal antibacterial agent are used together, the effect is better, and preferably, the natural antibacterial agent comprises the following components in percentage by mass: the inorganic metal antibacterial agent is 20: 1-5: 1.
The cellulose nanofiber has the diameter of 3-30 nm, the length of 300 nm-micron, the crystallinity of 70-95%, the elastic modulus of 135-150 GPa, the purity of more than 99.9% and the pH value of 6-7.
The method for preparing the biodegradable high-barrier antibacterial composite film comprises the steps of taking the cellulose nanofiber composite polylactic acid as a base material, adding the barrier agent, the antibacterial agent and the plasticizer, and preparing the biodegradable high-barrier antibacterial composite film in a tape casting or film scraping mode.
The method comprises the following specific steps:
(1) adding a solvent into polylactic acid, cellulose nanofiber and a plasticizer, stirring for dissolving, performing ultrasonic treatment, performing vacuum defoaming, adding a blocking agent and an antibacterial agent into the mixture, and uniformly stirring to obtain a nano-cellulose polylactic acid membrane casting solution;
(2) taking a nano cellulose fiber polylactic acid casting solution, and uniformly coating the surface of a polytetrafluoroethylene plate on a casting polytetrafluoroethylene mold or a film scraping machine;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
The solvent is selected from dichloromethane or trichloromethane or N, N-dimethylformamide or dimethyl sulfoxide or ethyl formate or ethyl acetate or butyl acetate or propyl acetate or a mixture thereof.
The thickness of the biodegradable high-barrier antibacterial composite film is 5-400 mu m
The Cellulose Nanofiber (CNF) is a fiber with physical properties, can keep the fiber form, is not dissolved in water but is in a dispersed state, keeps the crystal structure of the fiber and has the function of improving the mechanical properties. The cellulose nanofibers need to be dispersed before addition. The Cellulose Nanofibers (CNF) according to the present invention were purchased from the North century (Jiangsu) cellulose materials Co.
According to the invention, the polylactic acid is hydrophobic, and the barrier agent is hydrophilic, so that the bonding property between the polylactic acid and the barrier agent is poor, and the polylactic acid and the barrier agent can be well bonded through blending in different proportions, so that the finally obtained composite film has good barrier property under the action of the plasticizer.
The invention takes biodegradable polylactic acid as a matrix, and adopts cellulose nanofiber as a modifying substance to enhance the mechanical property of the polylactic acid; polyvinyl alcohol, ethylene-vinyl alcohol copolymer, acrylic ester, pullulan polysaccharide, chitosan, soy protein isolate, whey protein concentrate and zein are used as a barrier agent to enhance the barrier property of polylactic acid; natural antibacterial substances and inorganic metal antibacterial substances are adopted as antibacterial substances to enhance the antibacterial performance of the polylactic acid; adopting glycerol, polyethylene glycol, acetyl tributyl citrate, span80, epoxidized soybean oil and epoxidized sunflower oil as plasticizers to enhance the toughness of the polylactic acid; the biodegradable high-barrier plastic film material prepared by the invention has the characteristics of good mechanical property, high barrier property, antibacterial property, good biodegradability and the like.
Detailed Description
Example 1
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) taking 4g of polylactic acid, adding cellulose nanofiber and glycerol, adding 200ml of ethyl acetate, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding polyvinyl alcohol and chitosan, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the glycerol are respectively 2% and 4% of the weight of the polylactic acid, and the addition amounts of the polyvinyl alcohol and the chitosan are respectively 9% and 8% of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a film scraping machine, wherein the specification of a metering rod is 30 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 2
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) adding cellulose nanofiber and polyethylene glycol into 8g of polylactic acid, adding 100ml of N, N-dimethylformamide, stirring for dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding zein and thymol, stirring uniformly, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the polyethylene glycol are respectively 1.5 percent and 6 percent of the weight of the polylactic acid, and the addition amounts of the zein and the thymol are respectively 13 percent and 23 percent of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a film scraping machine, wherein the specification of a metering rod is 60 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 3
The biodegradable high-barrier antibacterial composite membrane is prepared by adopting a tape casting mode and comprises the following steps:
(1) adding 7.5g of polylactic acid into cellulose nanofiber and span80, adding 50ml of dimethyl sulfoxide, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding ethylene-vinyl alcohol copolymer and Nano-TiO2, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a Nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the span80 are respectively 2% and 5% of the weight of the polylactic acid, and the addition amounts of the ethylene-vinyl alcohol copolymer and the Nano-TiO2 are respectively 30% and 3% of the weight of the polylactic acid;
(2) casting the nano-cellulose polylactic acid casting solution on the surface of a polytetrafluoroethylene plate in a flow manner, wherein the thickness of the nano-cellulose polylactic acid casting solution is 170 micrometers;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 4
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) taking 10g of polylactic acid, adding cellulose nanofiber and glycerol, adding 50ml of dichloromethane, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding acrylate and cinnamaldehyde, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the glycerol are respectively 6% and 5% of the weight of the polylactic acid, and the addition amounts of the acrylate and the cinnamaldehyde are respectively 3% and 2.5% of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid membrane casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a membrane scraping machine, wherein the distance between the scrapers is 95 microns;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 5
The biodegradable high-barrier antibacterial composite membrane is prepared by adopting a tape casting mode and comprises the following steps:
(1) adding 18g of polylactic acid into cellulose nanofiber and acetyl tributyl citrate, adding 300ml of chloroform, stirring for dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding pullulan polysaccharide and tea polyphenol, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nano-fiber and the acetyl tributyl citrate are respectively 3% and 1.5% of the weight of the polylactic acid, and the addition amounts of the pullulan polysaccharide and the tea polyphenol are respectively 17% and 15% of the weight of the polylactic acid;
(2) casting the nano-cellulose polylactic acid casting solution on the surface of a polytetrafluoroethylene plate in a casting way, wherein the thickness of the nano-cellulose polylactic acid casting solution is 135 micrometers;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 6
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) taking 13g of polylactic acid, adding cellulose nanofiber and polyethylene glycol, adding 100ml of ethyl formate, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding polyvinyl alcohol and origanum essential oil, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the polyethylene glycol are respectively 2.5 percent and 2 percent of the weight of the polylactic acid, and the addition amounts of the polyvinyl alcohol and the oregano essential oil are respectively 20 percent and 33 percent of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid membrane casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a membrane scraping machine, wherein the distance between the scrapers is 200 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 7
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) adding cellulose nanofiber and epoxidized soybean oil into 5.25g of polylactic acid, adding 75ml of N, N-dimethylformamide, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding soybean protein isolate and Nano-ZnO, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a Nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the epoxidized soybean oil are respectively 2% and 4% of the weight of the polylactic acid, and the addition amounts of the soybean protein isolate and the Nano-ZnO are respectively 25% and 4% of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid membrane casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a membrane scraping machine, wherein the distance between the scrapers is 150 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 8
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) adding cellulose nanofiber and span80 into 10g of polylactic acid, adding 250ml of trichloromethane, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding chitosan and Nano-TiO2, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a Nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the span80 are respectively 1% and 3.5% of the weight of the polylactic acid, and the addition amounts of the chitosan and the Nano-TiO2 are respectively 10% and 7% of the weight of the polylactic acid;
(2) uniformly coating the rice cellulose polylactic acid casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a film scraping machine, wherein the distance between the scrapers is 80 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 9
The biodegradable high-barrier antibacterial composite membrane is prepared by adopting a tape casting mode and comprises the following steps:
(1) adding 11.5g of polylactic acid into cellulose nanofiber and acetyl tributyl citrate, adding 60ml of propyl acetate, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding whey protein concentrate and basil essential oil, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nano-fiber and the acetyl tributyl citrate are respectively 8% and 9% of the weight of the polylactic acid, and the addition amounts of the whey protein concentrate and the basil essential oil are respectively 33% and 41% of the weight of the polylactic acid;
(2) casting the nano-cellulose polylactic acid casting solution on a polytetrafluoroethylene plate die with the thickness of 380 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 10
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) taking 18g of polylactic acid, adding cellulose nanofiber and epoxy sunflower oil, adding 150ml of chloroform, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum deaeration, adding zein and Nano-Ag, stirring uniformly, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum deaeration to obtain a Nano-cellulose polylactic acid casting solution; the addition amounts of the added cellulose nanofiber and the added epoxy sunflower oil are respectively 10% and 7% of the weight of the polylactic acid, and the addition amounts of the zein and the Nano-Ag are respectively 5% and 2% of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid membrane casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a membrane scraping machine, wherein the distance between the scrapers is 270 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 11
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) taking 15g of polylactic acid, adding cellulose nanofiber and epoxy sunflower oil, adding 200ml of chloroform, stirring and dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum deaeration, adding zein, chitosan and Nano-Ag, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum deaeration to obtain a Nano-cellulose polylactic acid casting solution; the addition amounts of the added cellulose nanofiber and the added epoxy sunflower oil are respectively 10% and 7% of the weight of the polylactic acid, and the addition amounts of the zein, the chitosan and the Nano-Ag are respectively 5%, 10% and 2% of the weight of the polylactic acid;
(2) uniformly coating the nano-cellulose polylactic acid membrane casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a membrane scraping machine, wherein the distance between the scrapers is 270 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 12
The biodegradable high-barrier antibacterial composite membrane is prepared by adopting a tape casting mode and comprises the following steps:
(1) adding cellulose nanofiber and acetyl tributyl citrate into 11.5g of polylactic acid, adding 75ml of propyl acetate, stirring for dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum defoaming, adding whey protein concentrate, basil essential oil and Nano-TiO2Stirring uniformly in an ultrasonic processorPerforming medium-ultrasonic treatment for 5min, and performing vacuum defoaming to obtain a nano-cellulose polylactic acid membrane casting solution; the addition amounts of the cellulose Nano-fiber and the acetyl tributyl citrate are respectively 8% and 9% of the weight of the polylactic acid, the whey protein concentrate, the basil essential oil and the Nano-TiO2The addition amounts of (A) and (B) are respectively 33%, 41% and 4% of the weight of the polylactic acid;
(2) casting the nano-cellulose polylactic acid casting solution on a polytetrafluoroethylene plate die with the thickness of 380 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
Example 13
The biodegradable high-barrier antibacterial composite membrane is prepared in a membrane scraping mode and comprises the following steps:
(1) adding cellulose nanofiber and polyethylene glycol into 8g of polylactic acid, adding 100ml of N, N-dimethylformamide, stirring for dissolving, performing ultrasonic treatment for 5min in an ultrasonic processor, performing vacuum deaeration, adding zein, thymol and Nano-ZnO, uniformly stirring, performing ultrasonic treatment for 5min in the ultrasonic processor, and performing vacuum deaeration to obtain a Nano-cellulose polylactic acid casting solution; the addition amounts of the cellulose nanofiber and the polyethylene glycol are respectively 1.5 percent and 6 percent of the weight of the polylactic acid, and the addition amounts of the zein, the thymol and the Nano-ZnO are respectively 13 percent, 24 percent and 1.2 percent of the weight of the polylactic acid;
(1) uniformly coating the nano-cellulose polylactic acid casting solution on the surface of a polytetrafluoroethylene plate by using a scraper on a film scraping machine, wherein the specification of a metering rod is 60 mu m;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
The biodegradable high barrier antibacterial composite films prepared in examples 1-13 were subjected to performance tests.
1. The water resistance of the composite film was measured according to GB/T1540-2002 test for Water absorption of paper and paperboard (Ke Bo method), and the average value was obtained after 5 measurements.
2. The oxygen barrier performance of the composite membrane is measured according to GBT1038-2000 plastic membrane and thin sheet gas permeability test method.
3. The tensile strength and the elongation at break of the composite film are measured according to GB13022-91 'Plastic film tensile property test method'.
4. Antibacterial test of the composite membrane detects the antibacterial performance of the composite membrane to Escherichia coli and staphylococcus aureus according to QB/T2591-2003 'antibacterial plastic antibacterial performance test method and antibacterial effect'.
The results are shown in Table 1.
TABLE 1
Claims (9)
1. A biodegradable high-barrier antibacterial composite film is characterized by comprising the following raw materials in parts by weight: 100 parts of polylactic acid, 0.5-10 parts of cellulose nano-fiber, 1-10 parts of plasticizer, 3-35 parts of barrier agent and 2-45 parts of antibacterial agent.
2. A biodegradable high barrier antibacterial composite film according to claim 1, wherein said barrier agent is selected from polyvinyl alcohol or ethylene-vinyl alcohol copolymer or acrylate or pullulan or chitosan or soy protein isolate or whey protein concentrate or zein or their mixture.
3. The biodegradable high-barrier antibacterial composite film according to claim 1, wherein the plasticizer is selected from glycerol or polyethylene glycol or acetyl tributyl citrate or span80 or epoxidized soybean oil or epoxidized sunflower oil.
4. The biodegradable high-barrier antibacterial composite film according to claim 1,characterized in that the antibacterial agent comprises a natural antibacterial agent and an inorganic metal antibacterial agent; wherein the natural antibacterial agent is selected from chitosan or sodium alginate or cinnamaldehyde or tea polyphenols or oregano essential oil or basil essential oil or pepper flower essential oil or thymol or citral or curcumin or their mixture; the inorganic metal antibacterial agent is selected from Nano-TiO2Or Nano-ZnO or Nano-Ag or a mixture thereof.
5. The biodegradable high-barrier antibacterial composite film according to claim 1, wherein the cellulose nanofibers have a diameter of 3-30 nm and a length of 300 nm-micron, a crystallinity of 70-95%, an elastic modulus of 135-150 GPa, a purity of 99.9% or more, and a pH value of 6-7.
6. The method for preparing the biodegradable high-barrier antibacterial composite film according to any one of claims 1 to 5, wherein the biodegradable high-barrier antibacterial composite film is prepared by taking the cellulose nanofiber composite polylactic acid as a base material, adding a barrier agent, an antibacterial agent and a plasticizer and performing tape casting or film scraping.
7. The method for preparing a biodegradable high-barrier antibacterial composite film according to claim 6,
the method comprises the following specific steps:
(1) adding a solvent into polylactic acid, cellulose nanofiber and a plasticizer, stirring for dissolving, performing ultrasonic treatment, performing vacuum defoaming, adding a blocking agent and an antibacterial agent into the mixture, and uniformly stirring to obtain a nano-cellulose polylactic acid membrane casting solution;
(2) taking a nano-cellulose polylactic acid casting solution, and uniformly coating the surface of a polytetrafluoroethylene plate on a casting polytetrafluoroethylene die or a film scraping machine;
(3) the obtained film is placed in a ventilation position for airing, and the film is uncovered, so that the uniform biodegradable high-barrier antibacterial composite film can be obtained.
8. The method for preparing a biodegradable high-barrier antibacterial composite membrane according to claim 7, wherein the solvent is selected from dichloromethane or chloroform or N, N-dimethylformamide or dimethyl sulfoxide or ethyl formate or ethyl acetate or butyl acetate or propyl acetate or their mixture; the addition amount of the solvent is 3 times of the weight of the polylactic acid.
9. The method for preparing the biodegradable high-barrier antibacterial composite film according to claim 7, wherein the thickness of the biodegradable high-barrier antibacterial composite film is 5-400 μm.
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