CN115477776A - Starch-based degradable antibacterial preservative film and preparation method and application thereof - Google Patents
Starch-based degradable antibacterial preservative film and preparation method and application thereof Download PDFInfo
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- CN115477776A CN115477776A CN202211191645.9A CN202211191645A CN115477776A CN 115477776 A CN115477776 A CN 115477776A CN 202211191645 A CN202211191645 A CN 202211191645A CN 115477776 A CN115477776 A CN 115477776A
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- essential oil
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- 229920002472 Starch Polymers 0.000 title claims abstract description 98
- 239000008107 starch Substances 0.000 title claims abstract description 98
- 235000019698 starch Nutrition 0.000 title claims abstract description 98
- 239000003755 preservative agent Substances 0.000 title claims abstract description 70
- 230000002335 preservative effect Effects 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 230000000844 anti-bacterial effect Effects 0.000 title claims description 26
- 239000000341 volatile oil Substances 0.000 claims abstract description 67
- 239000002245 particle Substances 0.000 claims abstract description 63
- 230000003385 bacteriostatic effect Effects 0.000 claims abstract description 48
- 238000009920 food preservation Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- 229920000881 Modified starch Polymers 0.000 claims description 24
- 239000004368 Modified starch Substances 0.000 claims description 24
- 235000019426 modified starch Nutrition 0.000 claims description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 19
- 229920001896 polybutyrate Polymers 0.000 claims description 17
- 238000005469 granulation Methods 0.000 claims description 16
- 230000003179 granulation Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000004014 plasticizer Substances 0.000 claims description 9
- 238000005266 casting Methods 0.000 claims description 8
- 238000010096 film blowing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 240000002943 Elettaria cardamomum Species 0.000 claims description 7
- 244000166124 Eucalyptus globulus Species 0.000 claims description 7
- 235000005300 cardamomo Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- -1 fatty acid ester Chemical class 0.000 claims description 7
- 239000004970 Chain extender Substances 0.000 claims description 6
- 244000223760 Cinnamomum zeylanicum Species 0.000 claims description 6
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 6
- 235000017803 cinnamon Nutrition 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 5
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 5
- 239000000600 sorbitol Substances 0.000 claims description 5
- 235000012424 soybean oil Nutrition 0.000 claims description 5
- 239000003549 soybean oil Substances 0.000 claims description 5
- 229940037312 stearamide Drugs 0.000 claims description 5
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- ITCAUAYQCALGGV-XTICBAGASA-M sodium;(1r,4ar,4br,10ar)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylate Chemical compound [Na+].C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C([O-])=O ITCAUAYQCALGGV-XTICBAGASA-M 0.000 claims description 4
- 239000004250 tert-Butylhydroquinone Substances 0.000 claims description 4
- 235000019281 tert-butylhydroquinone Nutrition 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- VBICKXHEKHSIBG-UHFFFAOYSA-N beta-monoglyceryl stearate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 125000005442 diisocyanate group Chemical group 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- MRBKEAMVRSLQPH-UHFFFAOYSA-N 3-tert-butyl-4-hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1 MRBKEAMVRSLQPH-UHFFFAOYSA-N 0.000 claims description 2
- 230000002085 persistent effect Effects 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 238000002834 transmittance Methods 0.000 abstract description 2
- 239000002361 compost Substances 0.000 abstract 1
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000004200 microcrystalline wax Substances 0.000 description 2
- 235000019808 microcrystalline wax Nutrition 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 1
- 241000228197 Aspergillus flavus Species 0.000 description 1
- 239000004255 Butylated hydroxyanisole Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000019282 butylated hydroxyanisole Nutrition 0.000 description 1
- 229940043253 butylated hydroxyanisole Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000013311 vegetables 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
- A23B7/154—Organic compounds; Microorganisms; Enzymes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- 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
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
-
- 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
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Zoology (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Botany (AREA)
- Nutrition Science (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a starch-based degradable bacteriostatic preservative film and a preparation method and application thereof, wherein the method comprises the following steps: 1) Preparing starch-based biodegradable particles; 2) Preparing microencapsulated essential oil particles; 3) The preparation method of the starch-based degradable bacteriostatic preservative film is simple in steps and easy to operate, the prepared preservative film can be subjected to industrial compost degradation within 6 months, the degradation can be completed, the environmental pressure caused by plastic products can be relieved, the persistent bacteriostatic effect is good, the food preservation performance is excellent, the preservative film has the performances of high light transmittance, low haze, high tensile strength, high puncture resistance and the like, and the starch-based degradable bacteriostatic preservative film is very suitable for the field of food preservation.
Description
Technical Field
The invention relates to the field of food packaging materials, in particular to a starch-based degradable antibacterial preservative film and a preparation method and application thereof.
Background
The preservative film is a daily consumable in life, and the currently used preservative film mainly has two problems: firstly, the degradability is poor, and the problem of environmental pollution caused by the use of the preservative film generally exists; secondly, the bacteriostatic property is poor, the vegetables and foods are easy to mildew after daily contact, the main reason of the mildew is mildew, the bacteriostatic preservative film needs to be selected, namely, bacteriostatic components are added into the preservative film to prevent the mildew, but the safety and the durability of the bacteriostatic components of the existing bacteriostatic preservative film in the actual use process cannot be guaranteed, so that the applicant carries out deep research on the problems of environmental pollution, bacteriostatic property and the like of the preservative film.
Disclosure of Invention
The first technical problem to be solved by the invention is as follows: the preparation method of the starch-based degradable antibacterial preservative film is simple in steps and easy to operate, and the prepared preservative film solves the problems that the existing preservative film is difficult to degrade, environment pollution is easy to cause, and the persistent antibacterial performance is poor.
The second technical problem to be solved by the invention is: the starch-based degradable bacteriostatic preservative film solves the problems that the existing preservative film is difficult to degrade and has poor bacteriostatic performance continuity.
The third technical problem to be solved by the invention is: an application of a starch-based degradable bacteriostatic preservative film in food preservation.
In order to solve the first technical problem, the technical scheme of the invention is as follows: a preparation method of a starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 45-70 parts of PBAT, 25-40 parts of modified starch, 0.3-1.4 parts of chain extender, 0.4-0.7 part of dispersant and 0.03-0.09 part of antioxidant according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 135-140 ℃ to prepare starch-based biodegradable particles;
2) Preparing microencapsulated essential oil particles: uniformly dispersing 15-35 parts of bacteriostatic essential oil, 1.5-3 parts of O/W emulsifier and 10-20 parts of starch in water, heating 10-15 parts of PBAT and 30-40 parts of PLA at 180 ℃ for 20-30 min to be in a molten state, spraying the heated and molten liquid into the dispersed liquid by using high-pressure gas in a gun head with the diameter of 0.54-1.0 mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at a low temperature of 50 ℃ to dry;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 75 to 89 portions of starch-based biodegradable particles and 11 to 25 portions of microencapsulated essential oil particles are uniformly mixed and added into film forming equipment such as a film blowing machine or a casting machine to form a film, and the operation temperature is 135 to 140 ℃.
Preferably, the preparation method of the modified starch comprises the following steps: adding starch and a plasticizer into a high-speed mixer, wherein the mass ratio of the starch to the plasticizer is 100: (8-12), plasticizing at 60-80 ℃, and keeping for 10-30 min to obtain the modified starch.
Preferably, the plasticizer is one or more of glycerol, epoxidized soybean oil, epoxidized rapeseed oil, citrate and the like.
Preferably, the bacteriostatic essential oil is one or more of cardamom essential oil, cinnamon essential oil and eucalyptus essential oil.
Preferably, the O/W emulsifier is one or more of Ma Juyang ethylene fatty amine, polyethylene glycol fatty acid ester, sodium oleate, sodium abietate, tween 80 and the like.
Preferably, the chain extender is one or more of maleic anhydride, diisocyanate, 1,4-butanediol, sorbitol and the like.
Preferably, the dispersing agent is one or more of stearamide, stearic acid monoglyceride, microcrystalline paraffin, zinc stearate and the like.
Preferably, the antioxidant is one or more of 2,6-di-tert-butyl-p-cresol, tert-butyl hydroquinone, citric acid and butyl hydroxy anisol.
After the first technical scheme is adopted, the invention has the effects that: a preparation method of a starch-based degradable bacteriostatic preservative film comprises the following steps: 1) Preparing starch-based biodegradable particles; 2) Preparing microencapsulated essential oil particles; 3) The preparation method of the starch-based degradable antibacterial preservative film is simple in steps and easy to operate, the prepared preservative film can be industrially composted and degraded within 6 months, the environmental pressure caused by plastic products can be relieved, the antibacterial effect is good in persistence, the food preservation performance is excellent, and the preservative film has the performances of high light transmittance, low haze, high tensile strength, high puncture resistance and the like. The microencapsulated essential oil particles in the application can bear high temperature to a certain extent, so that the loss of essential oil in the processing process is reduced, the microencapsulated essential oil particles carry out microencapsulation treatment on edible bacteriostatic essential oil, the bacteriostatic essential oil can be slowly released along with the degradation of wall materials of the microencapsulated essential oil particles, the bacteriostatic function is lasting, and the defect of poor bacteriostatic effect of the existing preservative film in the later period can be well overcome.
And as the bacteriostatic essential oil is one or more of cardamom essential oil, cinnamon essential oil, eucalyptus essential oil and the like, the cardamom essential oil, the cinnamon essential oil and the eucalyptus essential oil can well inhibit the propagation of mould and belong to grease which can be contacted with food, so that the safety of the preservative film can be guaranteed.
In order to solve the two technical problems, the technical scheme of the invention is as follows: a starch-based degradable antibacterial preservative film is prepared by the preparation method.
After the two technical schemes are adopted, the invention has the effects that: the starch-based degradable antibacterial preservative film can be completely biodegraded, can effectively relieve the environmental pressure caused by plastic products, and has good persistent antibacterial effect and excellent food preservation performance.
In order to solve the third technical problem, the technical scheme of the invention is as follows: an application of a starch-based degradable bacteriostatic preservative film in food preservation.
Detailed Description
The present invention is described in further detail below with reference to specific examples.
A preparation method of a starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 45-70 parts of PBAT, 25-40 parts of modified starch, 0.3-1.4 parts of chain extender, 0.4-0.7 part of dispersant and 0.03-0.09 part of antioxidant according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 135-140 ℃ to prepare starch-based biodegradable particles;
2) Preparing microencapsulated essential oil particles: uniformly dispersing 15-35 parts of bacteriostatic essential oil, 1.5-3 parts of O/W emulsifier and 10-20 parts of starch in water, heating 10-15 parts of PBAT and 30-40 parts of PLA at 180 ℃ for 20-30 min to be in a molten state, spraying the heated and molten liquid into the dispersed liquid by using high-pressure gas in a gun head with the diameter of 0.54-1.0 mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at the low temperature of 50 ℃ to dry, wherein the high-pressure gas can be clean air and the air pressure is 4-5 MPa;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 75 to 89 portions of starch-based biodegradable particles and 11 to 25 portions of microencapsulated essential oil particles are mixed uniformly and added into film forming equipment such as a film blowing machine or a casting machine to form a film, the operation temperature is 135 to 140 ℃, and the mixing process can adopt manual mixing or a high-speed mixer.
The preparation method of the modified starch comprises the following steps: adding starch and a plasticizer into a high-speed mixer, wherein the mass ratio of the starch to the plasticizer is 100: (8-12), plasticizing at 60-80 ℃, and keeping for 10-30 min to obtain the modified starch.
The plasticizer is one or more of glycerol, epoxidized soybean oil, epoxidized rapeseed oil, citrate and the like, the bacteriostatic essential oil is one or more of cardamom essential oil, cinnamon essential oil, eucalyptus essential oil and the like, the O/W emulsifier is one or more of Ma Juyang ethylene fatty amine, polyethylene glycol fatty acid ester, sodium oleate, sodium abietate, tween 80 and the like, the chain extender is one or more of maleic anhydride, diisocyanate, 1,4-butanediol, sorbitol and the like, the dispersant is one or more of stearamide, stearic acid monoglyceride, microcrystalline wax, zinc stearate and the like, and the antioxidant is one or more of 2,6-di-tert-butyl-p-cresol, tert-butyl hydroquinone, citric acid, butyl hydroxy anisole and the like.
The starch-based degradable antibacterial preservative film is applied to the fields of food preservation and the like.
Example 1
The preparation method of the starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 55 parts of PBAT, 30 parts of modified starch, 1.4 parts of maleic anhydride, 0.5 part of stearamide and 0.05 part of 2,6-di-tert-butyl-p-cresol according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 135 ℃ to prepare starch-based biodegradable particles;
the preparation method of the modified starch comprises the following steps: adding starch and glycerol into a high-speed mixer, wherein the mass ratio of the starch to the glycerol is 100: and 8, plasticizing at the temperature of 60 ℃, and keeping for 20min to obtain the modified starch.
2) Preparing microencapsulated essential oil particles: uniformly dispersing 25 parts by weight of cardamom essential oil, 2.5 parts by weight of polyoxyethylene fatty amine and 15 parts by weight of starch in water, heating 13 parts by weight of PBAT and 36 parts by weight of PLA at 180 ℃ for 30min to be in a molten state, spraying the heated and molten liquid into the water by utilizing high-pressure gas in a gun head with the diameter of 1.0mm to form microencapsulated essential oil particles, and placing the microencapsulated essential oil particles at 50 ℃ for low-temperature airing, wherein the high-pressure gas is clean air and has the air pressure of 4MPa;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 80 portions of starch-based biodegradable particles and 20 portions of microencapsulated essential oil particles are mixed uniformly and added into film forming equipment such as a film blowing machine or a casting machine to prepare the starch-based degradable antibacterial preservative film, wherein the operation temperature is 135 ℃.
Example 2
The preparation method of the starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 60 parts of PBAT, 25 parts of modified starch, 1.4 parts of maleic anhydride, 0.5 part of microcrystalline paraffin and 0.05 part of citric acid according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 140 ℃ to obtain starch-based biodegradable particles;
the preparation method of the modified starch comprises the following steps: adding starch and epoxidized soybean oil into a high-speed mixer, wherein the mass ratio of the starch to the epoxidized soybean oil is 10:1, plasticizing at the temperature of 80 ℃ for 30min to prepare modified starch;
2) Preparing microencapsulated essential oil particles: uniformly dispersing 29 parts of cardamom essential oil, 3 parts of polyethylene glycol fatty acid ester and 18 parts of starch in water, heating 14 parts of PBAT and 35 parts of PLA for 30min at 180 ℃ to enable the PBAT and the PLA to be in a molten state, spraying the heated and molten liquid into the water by utilizing high-pressure gas in a gun head with the diameter of 1.0mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at low temperature of 50 ℃ in the air, wherein the high-pressure gas is clean air and the air pressure is 5MPa;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 81 portions of starch-based biodegradable particles and 19 portions of microencapsulated essential oil particles are mixed uniformly and added into film forming equipment such as a film blowing machine or a casting machine to prepare the starch-based degradable antibacterial preservative film, wherein the operation temperature is 135 ℃.
Example 3
The preparation method of the starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 63 parts of PBAT, 27 parts of modified starch, 0.7 part of sorbitol, 0.7 part of stearamide and 0.03 part of butylated hydroxyanisole according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 138 ℃ to obtain starch-based biodegradable particles;
the preparation method of the modified starch comprises the following steps: adding starch and citric acid ester into a high-speed mixer, wherein the mass ratio of the starch to the citric acid ester is 10:1, plasticizing at70 ℃ and keeping for 10min to prepare the modified starch.
2) Preparing microencapsulated essential oil particles: uniformly dispersing 35 parts of eucalyptus essential oil, 3 parts of sodium oleate and 17 parts of starch in water, heating 14 parts of PBAT and 30 parts of PLA at 180 ℃ for 30min to be in a molten state, spraying the heated and molten liquid into the water by using high-pressure gas in a gun head with the diameter of 0.54mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at a low temperature of 50 ℃ in the air, wherein the high-pressure gas is clean air and has the air pressure of 4MPa;
3) Preparing a starch-based degradable antibacterial preservative film: according to parts by weight, 75 parts of starch-based biodegradable particles and 25 parts of microencapsulated essential oil particles are uniformly mixed and added into film forming equipment such as a film blowing machine or a casting machine to prepare the starch-based degradable antibacterial preservative film, wherein the operating temperature is 140 ℃.
Example 4
The preparation method of the starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 70 parts of PBAT, 35 parts of modified starch, 0.3 part of maleic anhydride, 0.7 part of zinc stearate and 0.09 part of citric acid in parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 135 ℃ to obtain starch-based biodegradable particles;
the preparation method of the modified starch comprises the following steps: adding starch and glycerol into a high-speed mixer, wherein the mass ratio of the starch to the glycerol is 100: and (12) plasticizing at the temperature of 80 ℃ for 30min to obtain the modified starch.
2) Preparing microencapsulated essential oil particles: uniformly dispersing 15 parts of cinnamon essential oil, 1.5 parts of tween 80 and 20 parts of starch in water, heating 15 parts of PBAT and 38 parts of PLA at 180 ℃ for 20min to be in a molten state, spraying the heated and molten liquid into the water by using high-pressure gas in a gun head with the diameter of 1.0mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at the low temperature of 50 ℃ under the condition that the high-pressure gas is clean air and the air pressure is 4MPa;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 83 portions of starch-based biodegradable particles and 17 portions of microencapsulated essential oil particles are mixed uniformly and added into film forming equipment such as a film blowing machine or a casting machine to prepare the starch-based degradable antibacterial preservative film, wherein the operation temperature is 135 ℃.
Example 5
The preparation method of the starch-based degradable bacteriostatic preservative film comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 45 parts of PBAT, 40 parts of modified starch, 1 part of sorbitol, 0.4 part of microcrystalline wax and 0.06 part of tert-butyl hydroquinone according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 135 ℃ to obtain starch-based biodegradable particles;
the preparation method of the modified starch comprises the following steps: adding starch and epoxy rapeseed oil into a high-speed mixer, wherein the mass ratio of the starch to the epoxy rapeseed oil is 100: and (12) plasticizing at the temperature of 80 ℃, and keeping for 20min to obtain the modified starch.
2) Preparing microencapsulated essential oil particles: uniformly dispersing 25 parts of eucalyptus essential oil, 2 parts of sodium abietate and 10 parts of starch in water, heating 10 parts of PBAT and 40 parts of PLA at 180 ℃ for 25min to be in a molten state, spraying the heated and molten liquid into the water by using high-pressure gas in a gun head with the diameter of 0.54mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at a low temperature of 50 ℃ in the air, wherein the high-pressure gas is clean air and the air pressure is 5MPa;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 89 portions of starch-based biodegradable particles and 11 portions of microencapsulated essential oil particles are uniformly mixed and added into film forming equipment such as a film blowing machine or a casting machine to prepare the starch-based degradable antibacterial preservative film, wherein the operation temperature is 138 ℃.
The performance requirements of the preservative film in GB10457 are detected, and the experimental results are shown in the following table 1:
the table shows that the preservative film of the invention meets the national standard, the starch-based degradable bacteriostatic preservative film in the embodiments 1 to 5 has high light transmission, low haze, high tensile strength and high puncture resistance, and completely meets the performance requirements of the preservative film in the national standard.
And (3) testing the antibacterial performance:
the test method comprises the following steps: the inhibition capacity and the time of the preservative film to the mould are detected by adopting a diffusion method.
The samples in the examples 1 to 5 are respectively cut into appropriate circular sizes at time points of 1 day, 3 days, 7 days, 30 days, 60 days, 90 days, 120 days, 150 days and 180 days, the circular sizes are uniformly placed on the surface of agar full of mold bacterial liquid at intervals, the size of a bacteriostatic circle is observed after 6 to 10 hours, 3 times of repetition are set for each sample, and the average value of the experimental results is obtained.
Aspergillus flavus (scientific name) is adopted as the mould strain.
The following table 2 shows the size of the inhibition zone of the preservative film at different time points.
TABLE 2 example sample inhibition zone size (mm) at different times
As can be seen from the data in table 2, the preservative films prepared in examples 1 to 5 have stable bacteriostatic effects at a plurality of time points, and have good persistent bacteriostatic effects.
The above-mentioned embodiments are merely descriptions of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and alterations made to the technical solution of the present invention without departing from the spirit of the present invention are intended to fall within the scope of the present invention defined by the claims.
Claims (10)
1. A preparation method of a starch-based degradable bacteriostatic preservative film is characterized by comprising the following steps: the method comprises the following steps:
1) Preparing starch-based biodegradable particles: respectively weighing 45-70 parts of PBAT, 25-40 parts of modified starch, 0.3-1.4 parts of chain extender, 0.4-0.7 part of dispersant and 0.03-0.09 part of antioxidant according to parts by weight, uniformly mixing in a high-speed mixer, and then putting into a double-screw extruder for granulation at the granulation temperature of 135-140 ℃ to prepare starch-based biodegradable particles;
2) Preparing microencapsulated essential oil particles: uniformly dispersing 15-35 parts of bacteriostatic essential oil, 1.5-3 parts of O/W emulsifier and 10-20 parts of starch in water, heating 10-15 parts of PBAT and 30-40 parts of PLA at 180 ℃ for 20-30 min to be in a molten state, spraying the heated and molten liquid into the dispersed liquid by using high-pressure gas in a gun head with the diameter of 0.54-1.0 mm to form microencapsulated essential oil particles, and drying the microencapsulated essential oil particles at a low temperature of 50 ℃ to dry;
3) Preparing a starch-based degradable antibacterial preservative film: according to the weight portion, 75 to 89 portions of starch-based biodegradable particles and 11 to 25 portions of microencapsulated essential oil particles are uniformly mixed and added into film forming equipment such as a film blowing machine or a casting machine to form a film, and the operation temperature is 135 to 140 ℃.
2. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 1, which is characterized by comprising the following steps: the preparation method of the modified starch comprises the following steps: adding starch and plasticizer into a high-speed mixer, wherein the mass ratio of the starch to the plasticizer is 100: (8-12), plasticizing at 60-80 ℃, and keeping for 10-30 min to obtain the modified starch.
3. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 2, which is characterized by comprising the following steps of: the plasticizer is one or more of glycerol, epoxidized soybean oil, epoxidized rapeseed oil, citrate and the like.
4. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 1, which is characterized by comprising the following steps: the antibacterial essential oil is one or more of cardamom essential oil, cinnamon essential oil, eucalyptus essential oil and the like.
5. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 1, which is characterized by comprising the following steps: the O/W emulsifier is one or more of Ma Juyang ethylene fatty amine, polyethylene glycol fatty acid ester, sodium oleate, sodium abietate, tween 80 and the like.
6. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 1, which is characterized by comprising the following steps: the chain extender is one or more of maleic anhydride, diisocyanate, 1,4-butanediol, sorbitol and the like.
7. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 1, which is characterized by comprising the following steps: the dispersing agent is one or more of stearamide, stearic acid monoglyceride, microcrystalline paraffin, zinc stearate and the like.
8. The preparation method of the starch-based degradable bacteriostatic preservative film according to claim 1, which is characterized by comprising the following steps: the antioxidant is one or more of 2,6-di-tert-butyl-p-cresol, tert-butyl hydroquinone, citric acid, butyl hydroxy anisol and the like.
9. A starch-based degradable bacteriostatic preservative film is characterized in that: the starch-based degradable bacteriostatic preservative film is prepared by the preparation method of the starch-based degradable bacteriostatic preservative film according to any one of the claims 1 to 8.
10. The use of the starch-based degradable bacteriostatic preservative film according to claim 9 in food preservation.
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| CN114410078A (en) * | 2022-01-26 | 2022-04-29 | 上海海洋大学 | Slow-release degradable antibacterial preservative film and preparation method thereof |
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| CN114410078A (en) * | 2022-01-26 | 2022-04-29 | 上海海洋大学 | Slow-release degradable antibacterial preservative film and preparation method thereof |
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