CN104893090B - A kind of preparation method of food oxydating resistance packing film - Google Patents
A kind of preparation method of food oxydating resistance packing film Download PDFInfo
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- CN104893090B CN104893090B CN201510341594.7A CN201510341594A CN104893090B CN 104893090 B CN104893090 B CN 104893090B CN 201510341594 A CN201510341594 A CN 201510341594A CN 104893090 B CN104893090 B CN 104893090B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
A kind of EVOH food oxydating resistances packing film according to the present invention, comprising EVOH resins, PVA resins, alpha tocopherol and glycerol, the incorporation of each component by percentage to the quality, respectively：EVOH resins 70%～90%, PVA resins 5%～15%, alpha tocopherol 1%～10%, glycerol 1～5%.Wherein EVOH resins, ethylene contents 29mol%, are the SoarnoL of Japan's synthesis chemical productionTMD2908；PVA resins are 1799 models of Sinopec production.
Description
Technical field
The present invention relates to a kind of food oxydating resistance packaging material, refer in particular to one kind with ethylene/vinyl alcohol copolymer
(EVOH) it is food oxydating resistance packing film of main film forming base material and preparation method thereof.
Background technology
Lipid oxidation in food is the one of the main reasons that food spoilage becomes sour, and lipid oxidation causes food value
Reduce, so as to shorten Food Shelf-life.Presently mainly combined to control food with packing by adding antioxidant
Lipid oxidation, directly adds antioxidant in food in food processing, or configuration composite antioxidant to spray, film etc.
Mode processes food, and the lipid oxidation controlled in conjunction with technology such as vacuum, controlled atmospheric packings in food goes bad.In recent years, activity
Manufacturing for packaging material is increasingly received significant attention, and antioxidant is added or is coated on plastic sheeting, forms tool
There is the functional package thin film of anti-oxidation function, antioxidation is discharged using during food storing in food from thin film
Agent, plays a part of to suppress lipid oxidation, extends Shelf-life of Food-a Review.
EVOH is the alcoholysis product that ethylene-vinyl acetate copolymer carries out saponification or partly-hydrolysed reaction, is one
Highly crystalline body is planted, there is to gas fabulous barrier and fabulous processability, while with excellent mechanical property, generally making
For the intermediate barrier layer of composite plastic film, it is widely used in food packaging applications, excellent barrier properties that it has, excellent
Although good mechanical property and fabulous processing characteristics are with good prospect, material itself as the use of packaging material
The fresh keeping properties such as the due antioxidation of food fresh keeping institute, antibacterial are not had；Therefore its oxidation resistanct fresh-keeping function is further improved
It is extremely necessary.
Content of the invention
The purpose of the present invention is intended to：Food of the one kind so that ethylene/vinyl alcohol copolymer (EVOH) is main film forming base material is provided
A kind of preparation method of product antioxidation packing film, there is provided EVOH antioxidation packing films with antioxidant activity, is applied to
Packaging for foodstuff, can suppress food lipid oxidation, extend Food Shelf-life.
For achieving the above object, the present invention is adopted the following technical scheme that：
The preparation method of this EVOH food oxydating resistances packing film, comprising EVOH resins, polyvinyl alcohol (PVA) resin,
Alpha-tocopherol and glycerol；The incorporation of each component by percentage to the quality, respectively：EVOH resins 70%～90%, PVA trees
Fat 5%～15%, alpha-tocopherol 1%～10%, glycerol 1～5%.
Wherein EVOH resins, ethylene contents 29mol%, are the SoarnoL of Japan's synthesis chemical productionTMD2908；PVA trees
Fat is 1799 models of Sinopec production.
The preparation method of this EVOH food oxydating resistances packing film is as follows：
(1) antioxidant solution configuration：With 75% ethanol solution as solvent, the alpha-tocopherol for weighing certain mass is dissolved in
In ethanol solution, the antioxidant solution containing alpha-tocopherol is configured to.
(2) film liquid configuration：First, the normal propyl alcohol for weighing certain mass is dissolved in distilled water, according to normal propyl alcohol and distillation
The volume ratio of water is configured to normal propyl alcohol aqueous solution for 1～2；Then, according to quality proportioning weigh certain mass EVOH resins,
PVA resins and glycerol, add it to form mixed solution in the normal propyl alcohol aqueous solution for preparing, and the mixed solution are put
Enter in thermostat water bath, be allowed to heat under the conditions of 50 DEG C～75 DEG C, stir to being completely dissolved；Then, will according to quality proportioning
Ask and weigh the antioxidant solution prepared in a certain amount of step (1), add it to continue to stir in solution mixed above
Mix, until obtaining the film making solution of uniform state.
(3) film forming：The film making solution prepared in step (2) is put in vacuum drying oven the gas that sloughs in solution
Bubble, then extracts film liquid tiling film forming in glass culture dish of certain volume, is then placed in blast dry oven with syringe
Heating, drying 5 hours under the conditions of inherent 50 DEG C, further take out put spontaneously dry 12 hours at ambient temperature after take off film, prepare
There is the EVOH antioxidation packing films of antioxidant activity.
The preparation method of this EVOH food oxydating resistances packing film proposed according to above technical scheme, with tradition use
Common EVOH food product packing films compare, with advantages below：
1) excellent barrier properties, excellent mechanical property and fabulous processability that traditional EVOH possesses not only are remained
Can, simultaneously because the effect of the antioxidant for adding, therefore also has good antioxygenic property, in packaging for foodstuff is applied to
Can play a part of to suppress food lipid oxidation, extend Food Shelf-life.
2) due to be cast performance be further improved, therefore filming technology, equipment requirement more simple.
Description of the drawings
Column comparison charts of the Fig. 1 for the DPPH free radical scavenging activities of the EVOH antioxidation packing films of different ratios of raw materials；
Fig. 2 is curve chart of the EVOH antioxidation packing film of different ratios of raw materials to the antioxidant effect of Oleum Arachidis hypogaeae semen.
Specific embodiment
The preparation method of this EVOH food oxydating resistances packing film, comprising EVOH resins, PVA resins, alpha-tocopherol and
Glycerol, the incorporation of each component by percentage to the quality, respectively：EVOH resins 70%～90%, PVA resins 5%～
15%th, antioxidant (alpha-tocopherol) 1%～10%, glycerol 1～5%.
Wherein EVOH resins, ethylene contents 29mol%, are the SoarnoL of Japan's synthesis chemical productionTMD2908；PVA trees
Fat is 1799 models of Sinopec production.
The preparation method of this EVOH food oxydating resistances packing film is as follows：
(1) antioxidant solution configuration：With 75% ethanol solution as solvent, the alpha-tocopherol for weighing certain mass is dissolved in
In ethanol solution, the antioxidant solution containing alpha-tocopherol is configured to.
(2) film liquid configuration：First, the normal propyl alcohol for weighing certain mass is dissolved in distilled water, according to normal propyl alcohol and distillation
The volume ratio of water is configured to normal propyl alcohol aqueous solution for 1～2；Then, according to quality proportioning weigh certain mass EVOH resins,
PVA resins and glycerol, add it to form mixed solution in the normal propyl alcohol aqueous solution for preparing, and the mixed solution are put
Enter in thermostat water bath, be allowed to heat under the conditions of 50 DEG C～75 DEG C, stir to being completely dissolved；Then, will according to quality proportioning
Ask and weigh the antioxidant solution prepared in a certain amount of step (1), add it to continue to stir in solution mixed above
Mix, until obtaining the film making solution of uniform state.
(3) film forming：The film making solution prepared in step (2) is put in vacuum drying oven the gas that sloughs in solution
Bubble, then extracts film liquid tiling film forming in glass culture dish of certain volume, is then placed in blast dry oven with syringe
Heating, drying 5 hours under the conditions of inherent 50 DEG C, further take out put spontaneously dry 12 hours at ambient temperature after take off film, prepare
There is the EVOH antioxidation packing films of antioxidant activity.
The present invention is further elaborated with reference to specific embodiment, but protection scope of the present invention and not only in
This：
Embodiment 1
(1) antioxidant solution configuration：With 75% ethanol solution as solvent, weigh 20g alpha-tocopherols and be dissolved in 20ml second
In alcoholic solution, the antioxidant solution that alpha-tocopherol concentration is 1g/ml is configured to.
(2) film liquid configuration：First, normal propyl alcohol aqueous solution is configured, and normal propyl alcohol is 1 with the volume ratio of distilled water；Then, weigh
17.5gEVOH resins, 3.75gPVA resins and 1.25g glycerol, add it in 350ml normal propyl alcohol aqueous solutions, then should
Mixed solution is put in thermostat water bath under the conditions of 50 DEG C～75 DEG C and heats and stir to being completely dissolved；Then, molten toward mixing
The alpha-tocopherol solution 2.5ml prepared in step (1) is added in liquid, continues stirring until the masking for obtaining uniform state is molten
Liquid.
(3) film forming：The film making solution prepared in step (2) is put in vacuum drying oven the gas that sloughs in solution
Bubble, then extracts film liquid tiling film forming in glass culture dish of certain volume, is then placed in blast dry oven with syringe
Heating, drying 5 hours under the conditions of inherent 50 DEG C, further take out put spontaneously dry 12 hours at ambient temperature after take off film, prepare
There is the EVOH antioxidation packing films of antioxidant activity.
Embodiment 2
(1) antioxidant solution configuration：With 75% ethanol solution as solvent, weigh 20g alpha-tocopherols and be dissolved in 20ml second
In alcoholic solution, the antioxidant solution that alpha-tocopherol concentration is 1g/ml is configured to.
(2) film liquid configuration：First, normal propyl alcohol aqueous solution is configured, and normal propyl alcohol is 2 with the volume ratio of distilled water；Then, weigh
20gEVOH resins, 2.75gPVA resins and 0.25g glycerol, add it in 300ml normal propyl alcohol aqueous solutions, then this are mixed
Close solution and be put in thermostat water bath under the conditions of 50 DEG C～75 DEG C and heat and stir to being completely dissolved；Then, toward mixed solution
The middle film making solution for adding the alpha-tocopherol solution 2ml prepared in step (1), continuing to stir up to uniform state is obtained.
(3) film forming：The film making solution prepared in step (2) is put in vacuum drying oven the gas that sloughs in solution
Bubble, then extracts film liquid tiling film forming in glass culture dish of certain volume, is then placed in blast dry oven with syringe
Heating, drying 5 hours under the conditions of inherent 50 DEG C, further take out put spontaneously dry 12 hours at ambient temperature after take off film, prepare
There is the EVOH antioxidation packing films of antioxidant activity.
Embodiment 3
(1) antioxidant solution configuration：With 75% ethanol solution as solvent, weigh 20g alpha-tocopherols and be dissolved in 20ml second
In alcoholic solution, the antioxidant solution that alpha-tocopherol concentration is 1g/ml is configured to.
(2) film liquid configuration：First, normal propyl alcohol aqueous solution is configured, and normal propyl alcohol is 1.5 with the volume ratio of distilled water；Then, claim
22.5gEVOH resins, 1.25gPVA resins and 1g glycerol is taken, is added it in 375ml normal propyl alcohol aqueous solutions, then this is mixed
Close solution and be put in thermostat water bath under the conditions of 50 DEG C～75 DEG C and heat and stir to being completely dissolved；Then, toward mixed solution
The alpha-tocopherol solution 0.25ml prepared in middle addition step (1), continues stirring until the masking for obtaining uniform state is molten
Liquid.
(3) film forming：The film making solution prepared in step (2) is put in vacuum drying oven the gas that sloughs in solution
Bubble, then extracts film liquid tiling film forming in glass culture dish of certain volume, is then placed in blast dry oven with syringe
Heating, drying 5 hours under the conditions of inherent 50 DEG C, further take out put spontaneously dry 12 hours at ambient temperature after take off film, prepare
There is the EVOH antioxidation packing films of antioxidant activity.
Above-mentioned technical proposal of the applicant of the present invention according to proposition, to adopting this EVOH obtained in above-mentioned technical method
Food oxydating resistance packing film, has carried out including thickness, tensile strength, elongation at break, OTR oxygen transmission rate, carbon dioxide respectively
The physical performance indexs such as gas permeation rate, moisture-vapor transmission and light transmittance are determined；Meanwhile, using DPPH radical scavenging activities
Test determines the antioxygenic property of the EVOH antioxidation packing films for preparing；Packed using EVOH antioxidation is prepared
Film packaging Oleum Arachidis hypogaeae semen, evaluation of measuring its antioxidation packaging effect.Its experimental result is as follows：
First, physical performance index is measured
The physical performance index of the EVOH antioxidation packing films prepared using said method is measured, including
Thickness, tensile strength, elongation at break, OTR oxygen transmission rate, carbon dioxide transmitance, moisture-vapor transmission and light transmittance,
As a result as shown in table 1.
The physical property of the EVOH antioxidation packing films of 1 different ratios of raw materials of table
| Test index | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Thickness (mm) | 0.050 | 0.049 | 0.046 |
| Tensile strength (Mpa) | 78.54 | 83.14 | 86.32 |
| Elongation at break (%) | 34.11 | 28.56 | 26.13 |
| OTR oxygen transmission rate (m3·m/(m2·s·Pa)) | 8.48×10-19 | 6.93×10-19 | 5.19×10-19 |
| Carbon dioxide transmitance (m3·m/(m2·s·Pa)) | 6.51×10-19 | 4.33×10-19 | 3.68×10-19 |
| Moisture-vapor transmission (g m/ (m2·s·Pa)) | 7.88×10-15 | 8.72×10-15 | 2.15×10-14 |
| Light transmittance (%) | 56.3% | 60.6% | 83.4% |
The data determined from upper table can be seen that：The each physical property of thin film generally difference is little, mainly EVOH and PVA
Incorporation ratio different caused by, as the increase of PVA additions, tensile strength reduce, elongation at break increases, and oxygen is saturating
Cross rate, carbon dioxide transmission rate to be increased slightly, moisture-vapor transmission reduces, and causes mainly due to PVA water absorption；Due to α-
Tocopherol is yellow viscous liquid, as the increase of alpha-tocopherol content in thin film, the yellow colors of thin film are deepened, causes printing opacity
Rate is also decreased.
2nd, antioxygenic property is determined
The antioxygenic property test carried out by the EVOH antioxidation packing film prepared using said method is determined：
The antioxygen of the EVOH antioxidation packing films for preparing is determined using the test of DPPH radical scavenging activities
Change performance, its corresponding EVOH antioxidation packing film DPPH free radical scavenging activity is as shown in Figure 1.Due to prepared
Putting in order for alpha-tocopherol content ratio (from high to low) in EVOH antioxidation packing films is followed successively by：1 (α-life of embodiment
Educate phenol 10%)>Embodiment 2 (alpha-tocopherol 8%)>Embodiment 3 (alpha-tocopherol 1%).As can be seen from Figure 1：With thin film
The increase of middle alpha-tocopherol content, DPPH free radical scavenging activities are significantly improved, wherein the EVOH antioxidation containing 10% alpha-tocopherol
The oxidation resistance of packing film is most strong, and the oxidation resistance of the EVOH antioxidation packing films containing 1% alpha-tocopherol is most weak.From
DPPH radical scavenging activity evaluation tests can be seen that alpha-tocopherol and gradually discharge from thin film, so as to play removing
The effect of DPPH free radicals, shows that the EVOH packing films for adding alpha-tocopherol have anti-oxidation function.
3rd, actually used middle antioxidation packaging test Piglet s colibacillosis
Thin film antioxidation packaging effect assessment is carried out to the EVOH antioxidation packing film prepared using said method
Test：Using the EVOH antioxidation packing film packaging Oleum Arachidis hypogaeae semen for preparing, the peroxidating in Oleum Arachidis hypogaeae semen storage is determined
Value changes, Fig. 2 are peroxide value during the EVOH antioxidation packing film packaging Oleum Arachidis hypogaeae semen obtained using the inventive method
Curve chart.
Can be seen that from the curve chart：The Oleum Arachidis hypogaeae semen that is packed using the EVOH packing films (embodiment) containing alpha-tocopherol
During peroxide value is low compared with blank group in same minute, and the peroxide value of Oleum Arachidis hypogaeae semen is with EVOH antioxidation packing films
The increase of alpha-tocopherol content and reduce, such as：It is 10.3mmol/kg that the Oleum Arachidis hypogaeae semen of blank group is stored to the 5th day peroxide value, and
Embodiment 3, embodiment 2 and embodiment 1 pack the corresponding Oleum Arachidis hypogaeae semen peroxide value ability when storage was to the 10th, 20,25 days respectively
More than 10.3mmol/kg.As a result show that the EVOH packing films containing alpha-tocopherol have certain antioxidation to Oleum Arachidis hypogaeae semen,
Its oxidative rancidity is inhibited, and antioxidant effect increases with the increase of alpha-tocopherol content in EVOH antioxidation packing films
Plus.
Shown by actual fabrication and application experiment：This with the addition of the additives such as alpha-tocopherol antioxidant, glycerol
EVOH antioxidation packing films, not only remain excellent barrier properties, excellent mechanical property that traditional EVOH possesses and
Fabulous processing characteristics, also has good antioxygenic property, can play suppression food lipid in packaging for foodstuff is applied to
Oxidation, the effect for extending Food Shelf-life.Further, since curtain coating performance be further improved, therefore to filming technology, set
Standby requirement is more simple, it is easy to which popularity is used.
The above only basic embodiment that the applicant is given according to intention of the invention and basic effect, but not only
It is limited only to this.Any some improvement the technical program proposed with reference to this intention, are regarded as, category similar with this intention
Protection category in the present invention.
Claims (1)
1. a kind of preparation method of food oxydating resistance packing film, it is characterised in that：Comprising EVOH resins, PVA resins, α-fertility
Phenol and glycerol, the incorporation of each component by percentage to the quality, respectively：EVOH resins 70%～90%, PVA resins 5%
～15%, alpha-tocopherol 1%～10%, glycerol 1～5%；Wherein EVOH resins, ethylene contents 29mol%, are Japanese synthesis
The SoarnoL of chemical productionTMD2908；PVA resins are 1799 models of Sinopec production；
Its concrete preparation method is as follows：
(1) antioxidant solution configuration：With 75% ethanol solution as solvent, the alpha-tocopherol for weighing certain mass is dissolved in ethanol
In solution, the antioxidant solution containing tocopherol is configured to；
(2) film liquid configuration：First, the normal propyl alcohol for weighing certain mass is dissolved in distilled water, according to normal propyl alcohol and distilled water
Volume ratio is configured to normal propyl alcohol aqueous solution for 1～2；Then, EVOH resins, the PVA trees of certain mass are weighed according to quality proportioning
Fat and glycerol, add it to form mixed solution in the normal propyl alcohol aqueous solution for preparing, and the mixed solution are put into perseverance
In warm water bath, it is allowed to heat under the conditions of 50 DEG C～75 DEG C, stirs to being completely dissolved；Then, require to claim according to quality proportioning
The antioxidant solution prepared in a certain amount of step (1) is taken, adds it in solution mixed above, continue stirring, directly
To the film making solution for obtaining uniform state；
(3) film forming：The film making solution prepared in step (2) is put in vacuum drying oven the bubble that sloughs in solution, is connect
Film liquid tiling film forming in glass culture dish that certain volume is extracted with syringe, be then placed in blast dry oven 50
Heating, drying 5 hours under the conditions of DEG C, further take out put spontaneously dry 12 hours at ambient temperature after take off film, prepare have anti-
The EVOH antioxidation packing films of oxidation activity.
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| CN106578002A (en) * | 2016-12-05 | 2017-04-26 | 上海海洋大学 | Green vegetable freshness preservation method |
| CN107232295A (en) * | 2017-07-21 | 2017-10-10 | 上海海洋大学 | A kind of fresh-cut Hangzhoupro Chinese cabbage preservation method |
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2015
- 2015-06-18 CN CN201510341594.7A patent/CN104893090B/en not_active Expired - Fee Related
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| EP0454850A1 (en) * | 1989-11-20 | 1991-11-06 | Showa Denko Kabushiki Kaisha | Polyvinyl alcohol copolymer resin composition |
| CN101319067A (en) * | 2008-07-22 | 2008-12-10 | 金荣范 | Gas-phase anti-rust composite packaging film for industry and preparation method thereof |
| CN101905776A (en) * | 2010-07-26 | 2010-12-08 | 刘燕 | Multilayer coextrusion paper-like liquid packaging film |
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