CN104861598A - Antioxidant activity polylactic acid packing material and preparation method thereof - Google Patents
Antioxidant activity polylactic acid packing material and preparation method thereof Download PDFInfo
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- CN104861598A CN104861598A CN201510234625.9A CN201510234625A CN104861598A CN 104861598 A CN104861598 A CN 104861598A CN 201510234625 A CN201510234625 A CN 201510234625A CN 104861598 A CN104861598 A CN 104861598A
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- lactic acid
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- oxidant activity
- polycaprolactone
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 70
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000012856 packing Methods 0.000 title abstract description 10
- 239000004626 polylactic acid Substances 0.000 title abstract description 8
- 229920001610 polycaprolactone Polymers 0.000 claims abstract description 26
- 239000004632 polycaprolactone Substances 0.000 claims abstract description 25
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 7
- -1 poly(lactic acid) Polymers 0.000 claims description 127
- 238000005469 granulation Methods 0.000 claims description 12
- 230000003179 granulation Effects 0.000 claims description 12
- 238000005096 rolling process Methods 0.000 claims description 11
- 235000009392 Vitis Nutrition 0.000 claims description 8
- 241000219095 Vitis Species 0.000 claims description 8
- 229940092258 rosemary extract Drugs 0.000 claims description 8
- 235000020748 rosemary extract Nutrition 0.000 claims description 8
- 239000001233 rosmarinus officinalis l. extract Substances 0.000 claims description 8
- 210000000582 semen Anatomy 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- 235000013305 food Nutrition 0.000 abstract description 17
- 239000003963 antioxidant agent Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 6
- 230000002292 Radical scavenging effect Effects 0.000 description 5
- 239000012620 biological material Substances 0.000 description 5
- 239000004310 lactic acid Substances 0.000 description 5
- 235000014655 lactic acid Nutrition 0.000 description 5
- 239000005022 packaging material Substances 0.000 description 5
- 235000006708 antioxidants Nutrition 0.000 description 4
- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000009456 active packaging Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- YBWLLZXSRMTNCI-UHFFFAOYSA-N 1-phenyl-1-(2,4,6-trinitrophenyl)hydrazine Chemical compound [O-][N+](=O)C=1C=C([N+]([O-])=O)C=C([N+]([O-])=O)C=1N(N)C1=CC=CC=C1 YBWLLZXSRMTNCI-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- JBFHTYHTHYHCDJ-UHFFFAOYSA-N gamma-caprolactone Chemical group CCC1CCC(=O)O1 JBFHTYHTHYHCDJ-UHFFFAOYSA-N 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical group CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000622 polydioxanone Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Abstract
The invention discloses an antioxidant activity polylactic acid packing material and a preparation method thereof. The antioxidant activity packing material comprises the following components in parts by weight: 80-100 parts of matrix resin and 2-8 parts of natural antioxidant, wherein the matrix resin is the blends of the polylactic acid and polycaprolactone; when in preparation, the components are added into a double-screw extruder for blending and pelleting, and the novel antioxidant activity polylactic acid packing material is prepared by a calendar. The antioxidant activity polylactic acid packing material is non-toxic and innocent, the product is healthy and safe, biont is completely degraded, and the production process is simple; the obtained packing material has certain tensile strength and elongation at break, as well as excellent antioxidant activity, and can be applied to packing foods rich in oil.
Description
Technical field
The present invention relates to a kind of poly(lactic acid) anti-oxidant activity wrapping material and preparation method thereof, belong to technical field of polymer materials.
Background technology
Along with the development of science and technology, biomaterial is in the sight of people more and more frequently, biodegradable and eco-friendly requirement, impels biomaterial to intelligent and multifunction future development.In order to meet the growth requirement in food safety, biological environmental production field, new polymkeric substance is constantly included into the research category of biomaterial, new performance also constantly examine by biomaterial investigator closely, the relation between biomaterial Structure and Properties is also constantly re-recognized.
In prior art, existing several Biodegradable material is applied, and comprises the materials such as poly(lactic acid), polycaprolactone, PTMC and poly-dioxanone.Poly(lactic acid) (PLA) be a kind of with the carbohydrate such as starch, Mierocrystalline cellulose for raw material, through hydrolysis, fermentation, purifying and the polyester that is polymerized, its raw material sources are extensive, renewable, can complete biodegradable, having and processing characteristics like conventional polyolefins resin-phase, is a kind of novel green packaging material for food.Poly(lactic acid) has extraordinary mechanical property, and its tensile strength can reach about 60MPa, and main manifestations is for firm and crisp, but its fragility limits the subject matter of poly(lactic acid) in food packaging industry widespread use at present.Polycaprolactone (PCL) has good biocompatibility and biodegradable, its second-order transition temperature and melt temperature are far below poly(lactic acid), there is excellent kindliness and processibility, be widely used in totally biodegradable environment-friendly materials and medical material.Polylactic acid and caprolactone blend effectively can improve the mechanical property of poly(lactic acid) packing film.
Along with people are to food safety, the improving constantly of organoleptic property and Food Quality, the active packing of food arises at the historic moment.In conventional methods where, polyphenoils is all directly add in food.And the interpolation of polyphenoils can affect to flavour of food products.Anti-oxidant packing film is the one of Active Packaging Materials, it mainly with natural macromolecular material for carrier, add certain polyphenoils and the film made.Antioxidant is added in food product pack, what be prepared into has the impact that anti-oxidant activity composite membrane not only can reduce polyphenoils confrontation flavour of food products, the antioxidation property of composite membrane can be increased simultaneously, thus the characteristic of antioxidant and composite membrane can be given full play to, effectively extend the storage period of food.Wherein, tea-polyphenol, Pericarpium Granati extract, rosemary extract or Semen Vitis viniferae extract are taken from plant, have good anti-oxidant activity, are natural antioxidantss.
Although domestic and international many scholars have the report prepared about poly(lactic acid) anti-oxidant activity wrapping material, but do not mention with polylactic acid and caprolactone intermingling material as base material, add natural anti-reflecting oxide, preparation has the research of the food oxydating resistance Active Packaging Materials of anti-oxidant activity and excellent mechanical property.
Summary of the invention
In order to solve the deficiency of current anti-oxidant activity wrapping material, the invention provides that a kind of anti-oxidant activity is high, intensity is high, the novel poly(lactic acid) anti-oxidant activity wrapping material of good toughness, fully biodegradable, described poly(lactic acid) anti-oxidant activity wrapping material are made up of matrix resin and natural anti-reflecting oxide, wherein matrix resin 80 ~ 100 weight part, natural anti-reflecting oxide 2 ~ 8 weight part.
Described matrix resin is the blend of poly(lactic acid) and polycaprolactone, and poly(lactic acid) and polycaprolactone mix by weight the ratio of 6:4 ~ 9:1.
Described natural anti-reflecting oxide is the one in commercially available tea-polyphenol, Pericarpium Granati extract, rosemary extract, Semen Vitis viniferae extract.
Another object of the present invention is to the preparation method that described poly(lactic acid) anti-oxidant activity wrapping material are provided, poly(lactic acid), polycaprolactone and natural anti-reflecting oxide are mixed, add twin screw extruder to extrude and granulation, with rolling press 150 ~ 180 DEG C, pressure under being 1 ~ 3 MPa condition obtained thickness be 100 ~ 250 μm of poly(lactic acid) anti-oxidant activity wrapping material, the time is 20 ~ 60 s; The Freshkeeping Packaging of oil-rich food can be directly applied to.
Poly(lactic acid) of the present invention, polycaprolactone and natural anti-reflecting oxide compound particles need repeat melting, extrude, granulation 2 ~ 3 times, and poly(lactic acid), polycaprolactone and natural anti-reflecting oxide three are fully mixed.
Poly(lactic acid) of the present invention is market is supplied or is obtained through polycondensation or rac-Lactide ring-opening polymerization by lactic acid, and its weight average molecular weight is 100,000 ~ 300,000, and water content is less than 0.02%.
Polycaprolactone of the present invention is market is supplied or is obtained by 6-caprolactone ring-opening polymerization, and its weight average molecular weight is 100,000 ~ 200,000, and water content is less than 0.02%.
Compared with prior art, tool has the following advantages in the present invention:
(1) the anti-oxidant activity wrapping material that the present invention obtains have good processing characteristics, can carry out extruding, granulation in traditional plastic processing machinery, and roll film forming;
(2) working temperature of rolling press of the present invention controls at 150 ~ 180 DEG C, effectively prevent the too high impact on natural anti-reflecting oxide activity of processing temperature, has ensured the anti-oxidant activity of material;
(3) the anti-oxidant activity wrapping material that prepared by the present invention have that intensity is high, the feature of good toughness, found by test, tensile strength of material is 15 ~ 30MPa, elongation at break is 100 ~ 180%, wherein, adding of natural anti-reflecting oxide, play good plastification, greatly improve the mechanical property of wrapping material; Compared with polylactic acid and caprolactone intermingling material, the tensile strength adding the matrix material of natural anti-reflecting oxide reduces by 10 ~ 30%, and elongation at break improves 5 ~ 30%, and can meet the requirement of some packaging materials for food, range of application is more extensive;
(4) the anti-oxidant activity wrapping material that prepared by the present invention have certain antioxidant property, found by test, the natural anti-reflecting oxide that the present invention selects comprises tea-polyphenol, Pericarpium Granati extract, rosemary extract or Semen Vitis viniferae extract, after adding polymer blending material, DPPH(1,1-phenylbenzene picryl phenylhydrazine) radical scavenging activity is 15 ~ 95%, showed good antioxidant property;
(5) production technique of the present invention is simple, used starting material are nontoxic, wherein, poly(lactic acid) and polycaprolactone are Biodegradable material, and it is extract from crude substance to obtain that natural anti-reflecting oxide comprises tea-polyphenol, Pericarpium Granati extract, rosemary extract or Semen Vitis viniferae extract; This Active Packaging Materials has certain antioxidant effect, and the preservation of food (especially containing the based food that grease is abundant) can be directly used in, can biological degradation, in particular to a kind of, there is certain tensile strength, elongation at break, there are the novel poly(lactic acid) anti-oxidant activity wrapping material of good anti-oxidant activity.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but scope is not limited to described content.
Embodiment 1: this poly(lactic acid) anti-oxidant activity wrapping material constituent and weight part are: matrix resin 100 weight part, tea-polyphenol 2 weight part, wherein matrix resin is that poly(lactic acid) (molecular weight 100,000) and polycaprolactone (molecular weight 100,000) are obtained by weight the ratio mixing of 6:4;
The preparation method of above-mentioned wrapping material is as follows:
(1) after poly(lactic acid) and polycaprolactone being mixed by weight the ratio of 6:4 in vacuum drying oven dry 12 hours obtained matrix resins;
(2) get the matrix resin 1000g obtained in step (1) to mix with 20g tea-polyphenol, add melting in twin screw extruder, extrude, granulation 2 times, poly(lactic acid), polycaprolactone and natural anti-reflecting oxide three are fully mixed;
(3) after granulation, add rolling press and obtain poly(lactic acid) anti-oxidant activity wrapping material, rolling press working temperature is 150 DEG C, and pressure is 1MPa, and the time is 20s, and obtained poly(lactic acid) anti-oxidant activity wrapping material thickness is 250 μm;
The poly(lactic acid) anti-oxidant activity wrapping material tensile strength that the present embodiment prepares is 15MPa, elongation at break is 180%, obtained polymeric lactic acid compound film is carried out antioxidant property experiment, result shows, this poly(lactic acid) oxidation-resistant film DPPH radical scavenging activity is 15%, shows certain antioxidant property.
Embodiment 2: this poly(lactic acid) anti-oxidant activity wrapping material constituent and weight part are: matrix resin 80 weight part, Pericarpium Granati extract 4 weight part, wherein matrix resin is that poly(lactic acid) (molecular weight 200,000) and polycaprolactone (molecular weight 150,000) are obtained by weight the ratio mixing of 7:3;
The preparation method of above-mentioned wrapping material is as follows:
(1) by weight after poly(lactic acid) and polycaprolactone being mixed for the ratio of 7:3 in vacuum drying oven dry 12 hours obtained matrix resins;
(2) get the Pericarpium Granati extract obtaining matrix resin 800g and 40g in step (1) to mix, add twin screw extruder melting, extrude, granulation 2 times, poly(lactic acid), polycaprolactone and Pericarpium Granati extract three are fully mixed;
(3) after granulation, add rolling press and obtain poly(lactic acid) anti-oxidant activity wrapping material, rolling press working temperature is 160 DEG C, and pressure is 2MPa, and the time is 40s, and obtained poly(lactic acid) anti-oxidant activity wrapping material thickness is 180 μm;
The poly(lactic acid) anti-oxidant activity wrapping material tensile strength that the present embodiment prepares is 19MPa, elongation at break is 150%, obtained polymeric lactic acid compound film is carried out antioxidant property experiment, result shows, this poly(lactic acid) oxidation-resistant film DPPH radical scavenging activity is 50%, shows certain antioxidant property.
Embodiment 3: this poly(lactic acid) anti-oxidant activity wrapping material constituent and weight part are: matrix resin 90 weight part, rosemary extract 6 weight part, wherein matrix resin is that poly(lactic acid) (molecular weight 200,000) and polycaprolactone (molecular weight 150,000) are obtained by weight the ratio mixing of 8:2;
The preparation method of above-mentioned wrapping material is as follows:
(1) by weight after poly(lactic acid) and polycaprolactone being mixed for the ratio of 8:2 in vacuum drying oven dry 12 hours obtained matrix resins;
(2) rosemary extract getting matrix resin 900g and the 6g obtained in step (1) mixes, and adds twin screw extruder melting, extrudes, granulation 3 times, and poly(lactic acid), polycaprolactone and rosemary extract three are fully mixed;
(3) after granulation, add rolling press and obtain poly(lactic acid) anti-oxidant activity wrapping material, rolling press working temperature is 170 DEG C, and pressure is 2MPa, and the time is 40s, and obtained poly(lactic acid) anti-oxidant activity wrapping material thickness is 150 μm;
The poly(lactic acid) anti-oxidant activity wrapping material tensile strength that the present embodiment prepares is 23MPa, elongation at break is 120%, obtained polymeric lactic acid compound film is carried out antioxidant property experiment, result shows, this poly(lactic acid) oxidation-resistant film DPPH radical scavenging activity is 80%, shows good antioxidant property.
Embodiment 4: this poly(lactic acid) anti-oxidant activity wrapping material constituent and weight part are: matrix resin 100 weight part, Semen Vitis viniferae extract 8 weight part, wherein matrix resin is that poly(lactic acid) (molecular weight 300,000) and polycaprolactone (molecular weight 200,000) are obtained by weight the ratio mixing of 9:1;
The preparation method of above-mentioned wrapping material is as follows:
(1) by weight after poly(lactic acid) and polycaprolactone being mixed for the ratio of 9:1 in vacuum drying oven dry 12 hours obtained matrix resins;
(2) Semen Vitis viniferae extract getting matrix resin 1000g and the 8g obtained in step (1) mixes, and adds twin screw extruder melting, extrudes, granulation 3 times, and poly(lactic acid), polycaprolactone and Semen Vitis viniferae extract three are fully mixed;
(3) after granulation, add rolling press and obtain poly(lactic acid) anti-oxidant activity wrapping material, rolling press working temperature is 180 DEG C, and pressure is 3MPa, and the time is 60s, and obtained poly(lactic acid) anti-oxidant activity wrapping material thickness is 100 μm;
The poly(lactic acid) anti-oxidant activity wrapping material tensile strength that the present embodiment prepares is 30MPa, elongation at break is 100%, obtained polymeric lactic acid compound film is carried out antioxidant property experiment, result shows, this poly(lactic acid) oxidation-resistant film DPPH radical scavenging activity is 95%, shows good antioxidant property.
Claims (4)
1. poly(lactic acid) anti-oxidant activity wrapping material, is characterized in that constituent and weight part are: matrix resin 80 ~ 100 weight part, natural anti-reflecting oxide 2 ~ 8 weight part.
2. poly(lactic acid) anti-oxidant activity wrapping material according to claim 1, it is characterized in that: matrix resin is that poly(lactic acid) and polycaprolactone are obtained by weight the ratio mixing of 6:4 ~ 9:1, wherein, the weight average molecular weight of poly(lactic acid) is 10 ~ 300,000, and the weight average molecular weight of polycaprolactone is 10 ~ 200,000.
3. poly(lactic acid) anti-oxidant activity wrapping material according to claim 1 and 2, is characterized in that: natural anti-reflecting oxide is the one in tea-polyphenol, Pericarpium Granati extract, rosemary extract, Semen Vitis viniferae extract.
4. the preparation method of poly(lactic acid) anti-oxidant activity wrapping material according to claim 1, it is characterized in that: poly(lactic acid), polycaprolactone and natural anti-reflecting oxide are mixed, add twin screw extruder blended, melting, extrude, granulation 1 ~ 3 time, with rolling press at 150 ~ 180 DEG C, pressure obtained poly(lactic acid) anti-oxidant activity wrapping material under being 1 ~ 3 MPa condition.
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Cited By (9)
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CN107791535A (en) * | 2017-10-20 | 2018-03-13 | 福建恒安卫生材料有限公司 | Biodegradable film preparation method |
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CN113956633A (en) * | 2020-07-21 | 2022-01-21 | 中国农业大学 | Degradable active packaging material based on ginger essential oil and polylactic acid and preparation method thereof |
CN113956633B (en) * | 2020-07-21 | 2022-12-09 | 中国农业大学 | Degradable active packaging material based on ginger essential oil and polylactic acid and preparation method thereof |
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CN112544694B (en) * | 2020-10-16 | 2022-05-27 | 浙江杭化新材料科技有限公司 | Preservative paper for curing picked kiwi fruits and curing method of picked kiwi fruits |
CN113831755A (en) * | 2021-10-09 | 2021-12-24 | 厦门市鹭益印刷包装有限公司 | High-temperature-resistant sealing packaging film and preparation method thereof |
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