CN109749221A - A kind of antibacterial light degradation composite membrane and its preparation method and application - Google Patents
A kind of antibacterial light degradation composite membrane and its preparation method and application Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 86
- 230000015556 catabolic process Effects 0.000 title claims abstract description 28
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims abstract description 21
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims abstract description 20
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 claims abstract description 20
- 235000010331 calcium propionate Nutrition 0.000 claims abstract description 20
- 239000004330 calcium propionate Substances 0.000 claims abstract description 20
- 235000010241 potassium sorbate Nutrition 0.000 claims abstract description 20
- 239000004302 potassium sorbate Substances 0.000 claims abstract description 20
- 229940069338 potassium sorbate Drugs 0.000 claims abstract description 20
- 229920001903 high density polyethylene Polymers 0.000 claims abstract description 19
- 239000004700 high-density polyethylene Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 229920000092 linear low density polyethylene Polymers 0.000 claims abstract description 17
- 239000004707 linear low-density polyethylene Substances 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 15
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 12
- 238000000071 blow moulding Methods 0.000 claims description 12
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- 239000000203 mixture Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 235000013305 food Nutrition 0.000 claims description 3
- 229920006280 packaging film Polymers 0.000 claims description 3
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- 230000000845 anti-microbial effect Effects 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 7
- 239000001963 growth medium Substances 0.000 description 6
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 4
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- 239000002609 medium Substances 0.000 description 4
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 239000012895 dilution Substances 0.000 description 2
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- 231100000252 nontoxic Toxicity 0.000 description 2
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- 235000015097 nutrients Nutrition 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
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- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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Abstract
The embodiment of the invention discloses a kind of antibacterial light degradation composite membranes and its preparation method and application, and the composite membrane including the following raw material by being prepared: modified Nano TiO2, potassium sorbate, calcium propionate, Span80, LLDPE and HDPE.Composite membrane of the present invention passes through the specific selection of above-mentioned raw materials, and the composite membrane being prepared is enabled to have excellent mechanical performance, anti-microbial property and light degradation property.
Description
Technical field
The present embodiments relate to composite membrane technology fields, and in particular to a kind of antibacterial light degradation composite membrane and its preparation side
Method and application.
Background technique
Polymeric membrane is using organic high molecular polymer as film made of material.With the hair of petroleum industry and science and technology
Exhibition, the application field of polymeric membrane constantly expand, and have developed to intelligent macromolecular membrane, polymeric membrane by initial packaging film
Deng.
Currently, the preparation for antibacterial polymer film, is added to antibacterial agent in matrix using T-type die extrusion
Cast composite film, extrusion-blown modling process flow；Wherein the matrix resin overwhelming majority uses single LDPE or LLDPE；This
Outside, antibacterial agent uses single or complex antimicrobials, that is, includes answering for organic antibacterial agent, inorganic antiseptic or several antibacterial agents
It closes.However, there are certain toxicity for existing antibacterial agent, to the polymer film being prepared answering in food and Key works Drug packing film
With having some impact on, and existing antibacterial polymer film mechanical performance, anti-microbial property and light degradation property are poor.
Summary of the invention
For this purpose, the first mesh of the embodiment of the present invention provides a kind of antibacterial light degradation composite membrane, to solve to resist in the prior art
Bacterium polymer film has certain toxicity, and mechanical performance, anti-microbial property and the poor problem of light degradation property.
The second mesh of the embodiment of the present invention provides a kind of preparation method of antibacterial light degradation composite membrane, this method operation letter
It is single, each raw material can be mixed well, can be improved the comprehensive performance for the composite membrane being prepared.
Third of the embodiment of the present invention is designed to provide a kind of application of antibacterial light degradation composite membrane.
To achieve the goals above, the embodiment of the present invention provides the following technical solutions:
First aspect of the embodiment of the present invention provides a kind of antibacterial light degradation composite membrane, and the composite membrane is by including the following raw material system
It is standby to obtain:
Modified Nano TiO2, potassium sorbate, calcium propionate, Span80, LLDPE and HDPE.
Pass through modified Nano TiO in composite membrane of the present invention2Selection, nano-TiO can be sufficiently promoted2In composite membrane
Dispersion, and can be improved the light degradation rate of composite membrane；In addition modified Nano TiO2Work is cooperateed with potassium sorbate and calcium propionate
Under, enable to composite membrane that there is excellent anti-microbial property and heat resistance, and safe to the human body nontoxic；Pass through again
The addition of Span80 promotes dispersion of each raw material in composite membrane, improves the comprehensive performance of composite membrane, and Span80 can change
The wettability of kind composite membrane；In addition, the present invention selects LLDPE and HDPE as matrix, composite membrane is enabled to have excellent
Mechanical performance；To sum up, the present invention passes through the specific selection of above-mentioned raw materials, so that the composite membrane being prepared has excellent machine
Tool performance, anti-microbial property and light degradation property.
Further, the composite membrane is by including that the raw material of following parts by weight is prepared:
Modified Nano TiO22-20 parts, 2.5-10 parts of potassium sorbate, 2.5-10 parts of calcium propionate, 5-15 parts of Span80,
LLDPE95-105 parts and HDPE10-16 parts.
Further, the composite membrane is by including that the raw material of following parts by weight is prepared:
Modified Nano TiO25-10 parts, 4-5 parts of potassium sorbate, 5-10 parts of calcium propionate, 6-10 parts of Span80,
LLDPE100-105 parts and HDPE12-16 parts.
The present invention can preferably improve the synthesis for the composite membrane being prepared by the restriction to above-mentioned each raw material dosage
Performance.
In the present invention stringent limitation is not done to the type of HDPE, it is preferable that the HDPE is 5000s extrusion molding class.Pass through
HDPE type is further limited, the mechanical performance of composite membrane can be preferably improved.
In the present invention to modified Nano TiO2Type do not do stringent limitation, for example, can for this field routinely use
Modified Nano TiO2, it is preferable that the modified Nano TiO2By including the following steps to be prepared:
By nano-TiO2It is dispersed in ethanol solution and is ultrasonically treated with titanate coupling agent, then, at 70-80 DEG C
Under, 2.5-3.5h is stirred with 250-350r/min；The mixture after stirring is filtered by vacuum again, and true at 83-88 DEG C
Sky is drying to obtain modified Nano TiO2。
Preferably, the mass concentration of the ethanol solution is 3-6%.
Preferably, the titanate coupling agent and nano-TiO2Mass ratio be (2.5-3.5): 100；
Preferably, the sonication treatment time is 50-70min；Supersonic frequency is 35-45HZ.
The modified Nano TiO that the present invention is prepared by above-mentioned ad hoc approach2Rice, can advantageously promote nano-TiO2
Dispersion, raising prepares the comprehensive performance of composite membrane.
Second aspect of the embodiment of the present invention provides a kind of preparation method of antibacterial light degradation composite membrane, which includes
Following steps:
(a) by modified Nano TiO2, potassium sorbate, calcium propionate, Span80 and LLDPE mixed, stood, granulating and forming
Obtain nano modification composite master batch；
(b) by nano modification composite master batch and HDPE mix, blow molding obtains the composite membrane.
Further, the time of repose is 20-28h.
Further, the granulating and forming temperature is 150-170 DEG C.
Further, the blow molding temperature is 170-190 DEG C；Die head temperature is 175-185 DEG C.
The present invention is by the above method, first by modified Nano TiO2, potassium sorbate, calcium propionate, Span80 and LLDPE carry out
It mixes, can be improved the dispersing uniformity of each raw material, and mix with HDPE by the modification composite master batch after being granulated, be blow molded
To the composite membrane with Good All-around Property.
The composite membrane that the third aspect of the embodiment of the present invention provides a kind of above-mentioned composite membrane or above-mentioned preparation method is prepared
Application in food package film, vegetable and fruit packaging film, medical package film, agricultural film or refuse bag.
The embodiment of the present invention has the advantages that
Pass through modified Nano TiO in composite membrane of the present invention2Selection, nano-TiO can be sufficiently promoted2In composite membrane
Dispersion, and can be improved the light degradation rate of composite membrane；In addition modified Nano TiO2Work is cooperateed with potassium sorbate and calcium propionate
Under, enable to composite membrane that there is excellent anti-microbial property and heat resistance, and safe to the human body nontoxic；Pass through again
The addition of Span80 promotes dispersion of each raw material in composite membrane, improves the comprehensive performance of composite membrane, and Span80 can change
The wettability of kind composite membrane；In addition, the present invention selects LLDPE and HDPE as matrix, composite membrane is enabled to have excellent
Mechanical performance.
Detailed description of the invention
It, below will be to embodiment party in order to illustrate more clearly of embodiments of the present invention or technical solution in the prior art
Formula or attached drawing needed to be used in the description of the prior art are briefly described.It should be evident that the accompanying drawings in the following description is only
It is merely exemplary, it for those of ordinary skill in the art, without creative efforts, can also basis
The attached drawing of offer, which is extended, obtains other implementation attached drawings.
Fig. 1 is modified Nano TiO of the present invention2Electron-microscope scanning figure；
Fig. 2 is nano-TiO of the present invention2Electron-microscope scanning figure.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily, it is clear that described embodiment is the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
The raw material that following embodiment uses is as follows:
LLDPE: model DFDA7042；From PetroChina Company Ltd.；
HDPE: model DFDA7750M；From PetroChina Company Ltd..
Modified Nano TiO2It is prepared by the following method:
By nano-TiO2It is dispersed in 5% ethanol solution and is ultrasonically treated with titanate coupling agent, then, 75
At DEG C, 3h is stirred with 300r/min；The mixture after stirring is filtered by vacuum again, and is dried in vacuo at 85 DEG C and changes to obtain the final product
Property nano-TiO2；Wherein, titanate coupling agent and nano-TiO2Mass ratio be 3: 100；Sonication treatment time is 60min；Ultrasound
Frequency is 40Hz；To above-mentioned nano-TiO before modified2With modified nano-TiO2Electron-microscope scanning is carried out respectively, and surface sweeping result is such as
Shown in Fig. 1, Fig. 2.
Embodiment 1
One, antibacterial light degradation composite membrane
Above-mentioned composite membrane including the following raw material by being prepared:
Modified Nano TiO220 parts, 2.5 parts of potassium sorbate, 10 parts of calcium propionate, 15 parts, LLDPE105 parts of Span80 and
HDPE16 parts.
Two, preparation method
Above-mentioned preparation method includes the following steps:
(a) by modified Nano TiO2, potassium sorbate, calcium propionate, Span80 and LLDPE be placed in high-speed mixer and mixing 30min,
20h is stood, then forms to obtain nano modification composite master batch by double-screw extruding pelletizing；Wherein granulating and forming temperature is 150 DEG C；
(b) nano modification composite master batch is mixed with HDPE, obtains antibacterial using the blow molding of blown film system is squeezed out
Light degradation composite membrane；Wherein, blow molding temperature is 190 DEG C；Die head temperature is 175 DEG C.
Embodiment 2
One, antibacterial light degradation composite membrane
Above-mentioned composite membrane including the following raw material by being prepared:
Modified Nano TiO22 parts, 10 parts of potassium sorbate, 2.5 parts of calcium propionate, 5 parts, LLDPE95 parts of Span80 and HDPE10
Part.
Two, preparation method
Above-mentioned preparation method includes the following steps:
(a) by modified Nano TiO2, potassium sorbate, calcium propionate, Span80 and LLDPE be placed in high-speed mixer and mixing 30min,
28h is stood, then forms to obtain nano modification composite master batch by double-screw extruding pelletizing；Wherein granulating and forming temperature is 170 DEG C；
(b) nano modification composite master batch is mixed with HDPE, obtains antibacterial using the blow molding of blown film system is squeezed out
Light degradation composite membrane；Wherein, blow molding temperature is 170 DEG C；Die head temperature is 185 DEG C.
Embodiment 3
One, antibacterial light degradation composite membrane
Above-mentioned composite membrane including the following raw material by being prepared:
Modified Nano TiO210 parts, 5 parts of potassium sorbate, 5 parts of calcium propionate, 10 parts, LLDPE100 parts of Span80 and HDPE13
Part.
Two, preparation method
Above-mentioned preparation method includes the following steps:
(a) by modified Nano TiO2, potassium sorbate, calcium propionate, Span80 and LLDPE be placed in high-speed mixer and mixing 30min,
It stands for 24 hours, then forms to obtain nano modification composite master batch by double-screw extruding pelletizing；Wherein granulating and forming temperature is 160 DEG C；
(b) nano modification composite master batch is mixed with HDPE, obtains antibacterial using the blow molding of blown film system is squeezed out
Light degradation composite membrane；Wherein, blow molding temperature is 180 DEG C；Die head temperature is 180 DEG C.
Reference examples 1
This reference examples discloses a kind of antibacterial light degradation composite membrane, and the composite membrane and the composite membrane of embodiment 3 are essentially identical, area
It is not only that the LLDPE that HEPE is replaced with to same number；The preparation method of the composite membrane and the preparation method phase in embodiment 3
Together.
Reference examples 2
This reference examples discloses a kind of antibacterial light degradation composite membrane, and the composite membrane and the composite membrane of embodiment 3 are essentially identical, area
It is not only that the calcium propionate that potassium sorbate is replaced with to same number.The preparation method of the composite membrane and the preparation in embodiment 3
Method is identical.
Reference examples 3
This reference examples discloses a kind of antibacterial light degradation composite membrane, and the composite membrane and the composite membrane of embodiment 3 are essentially identical, area
It is not only that modified Nano TiO2Replace with the nano-TiO of same number2.In the preparation method and embodiment 3 of the composite membrane
Preparation method is identical.
Reference examples 4
This reference examples 1 disclose a kind of antibacterial light degradation composite membrane, and the composite membrane is identical as the composite membrane in embodiment 3, area
It is not only that, the composite membrane is the preparation method is as follows: by modified Nano TiO2, potassium sorbate, calcium propionate, Span80, LLDPE and
HDPE is placed in high-speed mixer and mixing 30min, stands for 24 hours, then form to obtain the compound mother of nano modification by double-screw extruding pelletizing
Material；Wherein granulating and forming temperature is 160 DEG C；
(b) nano modification composite master batch is obtained into antibacterial light degradation composite membrane using the blow molding of blown film system is squeezed out；Its
In, blow molding temperature is 180 DEG C；Die head temperature is 180 DEG C.
Experimental example 1
Carrying out film stretchability using electronic universal tester can test, and the long 15cm of batten, wide 2cm, stretching-machine stretches fast
Degree is 100mm/min, gauge length 5cm, every group batten average measurement 5 times, be averaged method and detect embodiment 1-3 and control respectively
The tensile strength of antibacterial light degradation composite membrane in example 1-4；Testing result is as shown in table 1:
Table 1
As shown in Table 1:
For the embodiment of the present invention compared with reference examples, composite membrane provided in an embodiment of the present invention has excellent tensile strength,
And changing the raw material components of composite membrane of the present invention and preparation method causes the composite membrane tensile strength being prepared to be remarkably decreased.
Experimental example 2
This experimental example is anti-microbial property detection
Experimental material:
Escherichia coli: source Shenyang Inst. of Applied Ecology, Chinese Academy of Sciences；
Culture medium: as shown in table 2
2 culture medium prescription of table
Formulations of nutrient solution
The culture medium prescription in table 2 is weighed respectively in beaker, and 1000ml distilled water is added, and is placed in heated at constant temperature electric heating
Put on heating for dissolving, it is to be mixed uniformly after, its pH is adjusted in the NaOH solution for being 100g/L with concentration, is adjusted to 7.0-7.5；
Respectively obtain fluid nutrient medium, semisolid culturemedium and solid medium；
Actication of culture:
The Escherichia coli of freezen protective are inoculated on inclined-plane solid medium with the oese after high-temperature sterilization, 37 DEG C of rings
It cultivates under border and is once activated for 24 hours；Liquid training after being inoculated into high-temperature sterilization with the strain of oese scraping slant medium
It supports in base, is cultivated under the conditions of 37 DEG C for 24 hours, carry out re-activation, the bacterium solution of re-activation is stored in low temperature environment；
Bacterium colony counts:
Bacterial colony count is that 1ml water is added in nutrient agar culture solution, is cultivated in biochemical cultivation case for 24 hours in 37
Under the conditions of DEG C, the total number of bacterial colonies that is grown in culture medium；
Escherichia coli are subjected to concentration dilution 10 by multiple proportions6Times, Bacteria Culture is carried out after dilution；Take respectively 1ml bacterium solution in
In 5 culture dishes containing semisolid culturemedium, rocks uniformly, add embodiment 3 and reference examples respectively in four culture dishes
Composite membrane in 1-4, be placed in biochemical cultivation case 37 DEG C of cultures for 24 hours；It does three times in parallel；Obtain bacterium colony count results such as table
Shown in 3:
The bacterium colony of 3 Escherichia coli of table counts
As shown in Table 3:
The embodiment of the present invention and reference examples all have certain bacteriostasis, and the embodiment of the present invention 3 and reference examples 1,4
Fungistatic effect is best.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (10)
1. a kind of antibacterial light degradation composite membrane, which is characterized in that by being prepared including the following raw material:
Modified Nano TiO2, potassium sorbate, calcium propionate, Span80, LLDPE and HDPE.
2. composite membrane according to claim 1, which is characterized in that the composite membrane is by the raw material system including following parts by weight
It is standby to obtain:
Modified Nano TiO22-20 parts, 2.5-10 parts of potassium sorbate, 2.5-10 parts of calcium propionate, 5-15 parts of Span80, LLDPE 95-
105 parts and HDPE 10-16 parts.
3. composite membrane according to claim 1, which is characterized in that the composite membrane is by the raw material system including following parts by weight
It is standby to obtain:
Modified Nano TiO25-10 parts, 4-5 parts of potassium sorbate, 5-10 parts of calcium propionate, 6-10 parts of Span80, LLDPE 100-105
Part and HDPE 12-16 parts.
4. composite membrane according to claim 1 to 3, which is characterized in that the HDPE is 5000s extrusion molding class.
5. composite membrane according to claim 1 to 3, which is characterized in that the modified Nano TiO2By including following step
Suddenly it is prepared:
By nano-TiO2It is dispersed in ethanol solution and is ultrasonically treated with titanate coupling agent, then, at 70-80 DEG C, with
250-350r/min stirs 2.5-3.5h；The mixture after stirring is filtered by vacuum again, and is dried in vacuo at 83-88 DEG C
Up to modified Nano TiO2。
6. the preparation method of any composite membrane of claim 1-5, which comprises the steps of:
(a) by modified Nano TiO2, potassium sorbate, calcium propionate, Span80 and LLDPE is mixed, stood, granulating and forming obtains
Nano modification composite master batch；
(b) by nano modification composite master batch and HDPE mix, blow molding obtains the composite membrane.
7. preparation method according to claim 6, which is characterized in that the time of repose is 20-28h.
8. preparation method according to claim 6, which is characterized in that the granulating and forming temperature is 150-170 DEG C.
9. preparation method according to claim 6, which is characterized in that the blow molding temperature is 170-190 DEG C；Die head
Temperature is 175-185 DEG C.
10. what any any preparation method of the composite membrane or claim 6-9 of claim 1-5 was prepared answers
Close application of the film in food package film, vegetable and fruit packaging film, medical package film, agricultural film or refuse bag.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111057289A (en) * | 2019-12-16 | 2020-04-24 | 沈阳工业大学 | LDPE/corn starch/TiO2Antibacterial composite membrane and preparation method thereof |
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