CN104059344A - Polylactic acid/modified graphene oxide antibacterial plastic and preparation method - Google Patents
Polylactic acid/modified graphene oxide antibacterial plastic and preparation method Download PDFInfo
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Abstract
The invention discloses polylactic acid/modified graphene oxide antibacterial plastic and a preparation method. The antibacterial plastic is composed of polylactic acid matrix resin and a composite antibacterial agent. The composite antibacterial agent is graphene oxide sheets with the surfaces loaded with zinc oxide nano-particles. The preparation method of the antibacterial plastic comprises the following steps that a trichloromethane solution of polylactic acid and a trichloromethane dispersing solution of the composite antibacterial agent are blended according to a certain ratio with a solution blending method, a clean glass plate is coated with the mixed solution through an automatic coating machine, and the solution is naturally volatilized at a room temperature. The polylactic acid/modified graphene oxide antibacterial plastic is obvious in antibacterial effect, wide in antibacterial range, biodegradable, safe, reliable, free from peculiar smell, and low in degree of harm and pollution to the human body and the environment.
Description
Technical field
The present invention relates to the antimicrobial technology field of poly-lactic acid material, be specifically related to a kind of poly(lactic acid)/modified graphene oxide antibiotic plastic and preparation method.
Background technology
In recent years, along with the enhancing of people's environmental consciousness, biodegradable plastic is subject to investigators' extensive concern day by day.Poly(lactic acid) (PLA) has good biocompatibility and biodegradable performance, and degraded product is in vivo carbonic acid gas and water, to biology and environment without any detrimentally affect.At present, poly(lactic acid) has a wide range of applications in fields such as packaging, automotive industry, drug conveying and organizational projects.But because poly(lactic acid) is decomposed the oligopolymer producing easily by various bacterial contamination, under suitable temperature humidity condition, bacterium very easily breeds, and affects human health.Therefore, people have higher requirement to the anti-microbial property of some poly-lactic acid products.
Preparing antimicrobial form poly(lactic acid) is generally in poly(lactic acid), to add antiseptic-germicide.Graphene oxide, as the important derivative of graphene-based material one class, has some unique physics and chemistry character, is therefore the focus of field of nanometer material technology research always.Except the good character such as chemical stability and mechanical property, Recent study person find that graphene oxide also has good biocompatibility and anti-microbial property.(the IsisE.Mej í asCarpio such as Carpio, CatherineM.Santos, XinWei, DeboraF.Rodrigues.Nanoscale, 2012,4:4746-4756) reported in polyvinyl carbazole matrix, add the graphene oxide of 3wt% can make matrix material have germ resistance and this material to mammalian cell without overt toxicity.But the addition of graphene oxide is relatively many.Nano zine oxide is a kind of conventional inorganic antiseptic, and it has good biocompatibility, environmental safety and long acting antibiotic.But, directly this nano antibacterial agent is added to the agglomeration that easily causes nano antibacterial agent in plastic substrate, will affect to a certain extent its original anti-microbial property.(the JongchulSeo such as Seo, GwonyoungJeon, EUiSungJang, SherBahadarKhan, HaksooHan.JournalofAppliedPolymerScience, 2011,112:1101-1108) report directly nano zine oxide and polypropylene carbonic ether have been made to composite membrane by solution blending, the anti-bacterial result shows that when nano zine oxide is added into 10wt%, composite membrane could reach respectively 100% and 87.5% to the antibiotic rate of intestinal bacteria and lactobacillus, and in material, zinc oxide exists obvious agglomeration.
Summary of the invention
The object of this invention is to provide a kind of poly(lactic acid)/modified graphene oxide antibiotic plastic and preparation method.Be intended to overcome the deficiencies in the prior art, not only can under the condition of adding less antiseptic-germicide, make material have significant anti-microbial property, and antibacterial range be wide, product be biodegradable, safe and reliable, free from extraneous odour, and harm and pollution level to human body and environment are low.
Realizing technical scheme of the present invention is:
In poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention, described poly(lactic acid)/modified graphene oxide antibiotic plastic is made up of polylactic acid based resin, complex antimicrobials, complex antimicrobials is the graphene oxide of area load Zinc oxide nanoparticle, described polylactic acid based resin, the mass ratio of complex antimicrobials are 100:(0.2～1.0), preferably 100:(0.2～0.7).
The graphene oxide of described area load Zinc oxide nanoparticle is the laminate structure that individual layer sheet or a small amount of lamella are piled up, and the Zinc oxide nanoparticle particle diameter of load is 15～30nm, and actual negative carrying capacity is about 80wt%.
The preparation of described complex antimicrobials is that the graphene oxide that Hummers method is made is dried and ultrasonic being dispersed in ethanol, under heating condition, add zinc acetate and constantly stir and make it abundant mixed dissolution, after solution boiling, slowly add sodium hydroxide solution, after completion of the reaction product centrifugal water is washed till to neutrality, vacuum-drying gained.
The preparation method of poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention, comprises the following steps:
(1) preparation of complex antimicrobials: the graphene oxide that Hummers method is made is dried and ultrasonic being dispersed in ethanol, under heating condition, add zinc acetate and constantly stir and make it abundant mixed dissolution, after solution boiling, slowly add sodium hydroxide solution, after completion of the reaction product centrifugal water is washed till to neutrality, vacuum-drying;
(2) utilize low boiling point solvent trichloromethane that poly(lactic acid) and complex antimicrobials are carried out to solution blending in proportion, with automatic film applicator by mixed solution film on clean sheet glass, the room temperature solvent of ordering volatilizees naturally, finally in warm water, demoulding is placed in baking oven dryly, obtains described poly(lactic acid)/modified graphene oxide antibiotic plastic.
In step (1), the concentration of graphene oxide in ethanolic soln is 0.5mg/mL, and the concentration of sodium hydroxide solution is 0.5mol/mL, and the mol ratio of sodium hydroxide and zinc acetate is 2:1.04, and the reaction times is 1h.
In step (2), the mass ratio of polylactic acid based resin, complex antimicrobials is 100:(0.2～1.0).
The concentration of step (2) poly(lactic acid) in blended liquid is 0.13～0.16g/mL, and the blend time is 3～6h.
When the middle film of step (2), controlling its thickness is 1.5mm.
In step (2), under trichloromethane solvent room temperature, the natural volatilization time is 12h, and oven drying temperature is 60 DEG C, and be 48h time of drying.
Poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention compared with prior art, has the following advantages:
(1) Zinc oxide nanoparticle is carried on to the surface of graphene oxide sheet, utilize the effect of chemical bond between zinc oxide and graphene oxide, effectively hinder the reunion of Zinc oxide nanoparticle in poly(lactic acid) matrix, improved the anti-microbial activity of zinc oxide in this system;
(2) graphene oxide has large specific surface area, and the oxygen-containing functional group on surface can form strong interface interaction power with polylactic acid based body, and Miscibility is good;
(3), due to the mutual synergy of graphene oxide in complex antimicrobials and nano zine oxide, only need to add a small amount of (< 1.0wt%) this complex antimicrobials can reach significant antibacterial effect;
(4) antibiotic plastic that the present invention obtains is recyclable, reusable, and antibacterial range is wide, and product is biodegradable, safe and reliable, and harm and pollution level to human body and environment are low.
Below in conjunction with accompanying drawing, the invention will be further described.
Brief description of the drawings
Fig. 1 is the graphene oxide transmission electron microscope picture of area load Zinc oxide nanoparticle in the present invention.
Fig. 2 is anti-bacteria test result figure in comparative example and embodiment 2.
Embodiment
A kind of poly(lactic acid)/modified graphene oxide antibiotic plastic, described poly(lactic acid)/modified graphene oxide antibiotic plastic is made up of polylactic acid based resin, complex antimicrobials, complex antimicrobials is the graphene oxide of area load Zinc oxide nanoparticle, described polylactic acid based resin, the mass ratio of complex antimicrobials are 100:(0.2～1.0), preferably 100:(0.2～0.7).
A preparation method for poly(lactic acid)/modified graphene oxide antibiotic plastic, comprises the following steps:
(1) preparation of complex antimicrobials: the graphene oxide that Hummers method is made is dried and ultrasonic being dispersed in ethanol, under heating condition, add zinc acetate and constantly stir and make it abundant mixed dissolution, after solution boiling, slowly add sodium hydroxide solution, after completion of the reaction product centrifugal water is washed till to neutrality, vacuum-drying;
(2) utilize low boiling point solvent trichloromethane that poly(lactic acid) and complex antimicrobials are carried out to solution blending in proportion, with automatic film applicator by mixed solution film on clean sheet glass, the room temperature solvent of ordering volatilizees naturally, finally in warm water, demoulding is placed in baking oven dryly, obtains described poly(lactic acid)/modified graphene oxide antibiotic plastic.
For Comprehension and Implementation better, below in conjunction with comparative example and embodiment, the present invention is further described.
Anti-microbial property test in following comparative example and embodiment: anti-microbial property detects with reference to the light industry standard QB/T2591-2003 of the People's Republic of China (PRC), adopts film applicator coating, investigates the antibiotic rate of sample 24h, and total number of bacterial colony is measured and counted according to GB/T4789.2-2003.The antibiotic plastic film of preparing is cut into the antibacterial sample of 50mm × 50mm.The calculation formula of antibiotic rate is as follows:
R(％)＝(B－C)/B×100
In formula, R is antibacterium rate (%), and B is blank sample average bacterial count recovered (cfu/ sheet), and C is antibiotic plastic sample average bacterial count recovered (cfu/ sheet).
Detect with bacterium: streptococcus aureus (Staphylococcusaureus) ATCC6538; Colon bacillus (Escherichiacoli) ATCC25922
The preparation of different ingredients poly(lactic acid)/modified graphene oxide antibiotic plastic:
Comparative example: take 10g poly(lactic acid) and be dissolved in 60mL trichloromethane, magnetic agitation 6h fully dissolves it.With automatic film applicator, solution is painted on sheet glass to the film of 1.5mm, is at room temperature made subsequently the trichloromethane 24h that naturally volatilizees, with after the warm water demoulding at 60 DEG C vacuum-drying 48h, make poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention.Antibiotic rate test result: streptococcus aureus 0; Colon bacillus 0.
Embodiment 1: take 10g poly(lactic acid) and be dissolved in 40mL trichloromethane, magnetic agitation 2h fully dissolves it.Take 0.02g complex antimicrobials and be scattered in 20mL trichloromethane, ultrasonic 1.5h makes it to be uniformly dispersed.Subsequently by two dispersion liquid mix and blends, blend 4h.With automatic film applicator, mixing solutions is painted on sheet glass to the film of 1.5mm, is at room temperature made subsequently the trichloromethane 24h that naturally volatilizees, with after the warm water demoulding at 60 DEG C vacuum-drying 48h, make poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention.Antibiotic rate test result: streptococcus aureus 99.2%; Colon bacillus 97.6%.
Embodiment 2: take 10g poly(lactic acid) and be dissolved in 40mL trichloromethane, magnetic agitation 2h fully dissolves it.Take 0.05g complex antimicrobials and be scattered in 20mL trichloromethane, ultrasonic 1.5h makes it to be uniformly dispersed.Subsequently by two dispersion liquid mix and blends, blend 4h.With automatic film applicator, mixing solutions is painted on sheet glass to the film of 1.5mm, is at room temperature made subsequently the trichloromethane 24h that naturally volatilizees, with after the warm water demoulding at 60 DEG C vacuum-drying 48h, make poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention.Antibiotic rate test result: streptococcus aureus 99.9%; Colon bacillus 98.5%.
Embodiment 3: take 10g poly(lactic acid) and be dissolved in 40mL trichloromethane, magnetic agitation 2h fully dissolves it.Take 0.07g complex antimicrobials and be scattered in 20mL trichloromethane, ultrasonic 1.5h makes it to be uniformly dispersed.Subsequently by two dispersion liquid mix and blends, blend 4h.With automatic film applicator, mixing solutions is painted on sheet glass to the film of 1.5mm, is at room temperature made subsequently the trichloromethane 24h that naturally volatilizees, with after the warm water demoulding at 60 DEG C vacuum-drying 48h, make poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention.Antibiotic rate test result: streptococcus aureus 99.6%; Colon bacillus 98.7%.
Embodiment 4: take 10g poly(lactic acid) and be dissolved in 40mL trichloromethane, magnetic agitation 2h fully dissolves it.Take 0.10g complex antimicrobials and be scattered in 20mL trichloromethane, ultrasonic 1.5h makes it to be uniformly dispersed.Subsequently by two dispersion liquid mix and blends, blend 4h.With automatic film applicator, mixing solutions is painted on sheet glass to the film of 1.5mm, is at room temperature made subsequently the trichloromethane 24h that naturally volatilizees, with after the warm water demoulding at 60 DEG C vacuum-drying 48h, make poly(lactic acid)/modified graphene oxide antibiotic plastic of the present invention.Antibiotic rate test result: streptococcus aureus 98.9%; Colon bacillus 97.8%.
As shown in Figure 1, in the present invention, the pattern of the graphene oxide of area load Zinc oxide nanoparticle is the laminate structure that individual layer sheet or a small amount of lamella are piled up, and the Zinc oxide nanoparticle particle diameter of load is 15～30nm.
As shown in Figure 2, (a) (b) is for the polylactic acid plastic film that adds complex antimicrobials in pure polylactic acid film in comparative example and embodiment 2 is respectively to effects on surface enumeration result after the antibacterial test of gram-positive microorganism streptococcus aureus and Gram-negative bacteria colon bacillus 24h.In embodiment 2, add the polylactic acid plastic film of complex antimicrobials described in the present invention than pure polylactic acid film, fungistatic effect is remarkable, can reach respectively 99.9% and 98.5% to the antibiotic rate of streptococcus aureus and colon bacillus.
Claims (10)
1. poly(lactic acid)/modified graphene oxide antibiotic plastic, it is characterized in that, described poly(lactic acid)/modified graphene oxide antibiotic plastic is made up of polylactic acid based resin, complex antimicrobials, complex antimicrobials is the graphene oxide of area load Zinc oxide nanoparticle, and described polylactic acid based resin, the mass ratio of complex antimicrobials are 100:(0.2～1.0).
2. poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 1, is characterized in that, described polylactic acid based resin, the mass ratio of complex antimicrobials are 100:(0.2～0.7).
3. poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 1, it is characterized in that, the graphene oxide of described area load Zinc oxide nanoparticle is the laminate structure that individual layer sheet or a small amount of lamella are piled up, the Zinc oxide nanoparticle particle diameter of load is 15～30nm, and actual negative carrying capacity is about 80wt%.
4. poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 1, it is characterized in that, the preparation of described complex antimicrobials is that the graphene oxide that Hummers method is made is dried and ultrasonic being dispersed in ethanol, under heating condition, add zinc acetate and constantly stir and make it abundant mixed dissolution, after solution boiling, slowly add sodium hydroxide solution, after completion of the reaction product centrifugal water is washed till to neutrality, vacuum-drying gained.
5. a preparation method for poly(lactic acid)/modified graphene oxide antibiotic plastic, is characterized in that, comprises the following steps:
(1) preparation of complex antimicrobials: the graphene oxide that Hummers method is made is dried and ultrasonic being dispersed in ethanol, under heating condition, add zinc acetate and constantly stir and make it abundant mixed dissolution, after solution boiling, slowly add sodium hydroxide solution, after completion of the reaction product centrifugal water is washed till to neutrality, vacuum-drying;
(2) utilize low boiling point solvent trichloromethane that poly(lactic acid) and complex antimicrobials are carried out to solution blending in proportion, with automatic film applicator by mixed solution film on clean sheet glass, the room temperature solvent of ordering volatilizees naturally, finally in warm water, demoulding is placed in baking oven dryly, obtains described poly(lactic acid)/modified graphene oxide antibiotic plastic.
6. the preparation method of poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 5, it is characterized in that, in step (1), the concentration of graphene oxide in ethanolic soln is 0.5mg/mL, the concentration of sodium hydroxide solution is 0.5mol/mL, the mol ratio of sodium hydroxide and zinc acetate is 2:1.04, and the reaction times is 1h.
7. the preparation method of poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 5, is characterized in that, in step (2), the mass ratio of polylactic acid based resin, complex antimicrobials is 100:(0.2～1.0).
8. the preparation method of poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 5, is characterized in that, the concentration of step (2) poly(lactic acid) in blended liquid is 0.13～0.16g/mL, and the blend time is 3～6h.
9. the preparation method of poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 5, is characterized in that, when the middle film of step (2), controlling its thickness is 1.5mm.
10. the preparation method of poly(lactic acid)/modified graphene oxide antibiotic plastic according to claim 5, it is characterized in that, in step (2), under trichloromethane solvent room temperature, the natural volatilization time is 12h, and oven drying temperature is 60 DEG C, and be 48h time of drying.
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| CN104710733A (en) * | 2015-04-07 | 2015-06-17 | 嘉兴学院 | Heat-resistant antimicrobial polylactic acid material and preparation method thereof |
| CN105380067A (en) * | 2015-10-19 | 2016-03-09 | 南京财经大学 | Coating inhibiting listeria monocytogenes and preparation method and application |
| CN105778140A (en) * | 2016-04-28 | 2016-07-20 | 南京凤源新材料科技有限公司 | Preparation method of high-barrier-property polylactic acid multilayer composite film |
| CN106893301A (en) * | 2017-03-27 | 2017-06-27 | 佛山汇沐化学科技有限公司 | A kind of antibiotic plastic and preparation method thereof |
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| CN104710733A (en) * | 2015-04-07 | 2015-06-17 | 嘉兴学院 | Heat-resistant antimicrobial polylactic acid material and preparation method thereof |
| CN105380067A (en) * | 2015-10-19 | 2016-03-09 | 南京财经大学 | Coating inhibiting listeria monocytogenes and preparation method and application |
| CN105778140A (en) * | 2016-04-28 | 2016-07-20 | 南京凤源新材料科技有限公司 | Preparation method of high-barrier-property polylactic acid multilayer composite film |
| CN106893301A (en) * | 2017-03-27 | 2017-06-27 | 佛山汇沐化学科技有限公司 | A kind of antibiotic plastic and preparation method thereof |
| CN106893301B (en) * | 2017-03-27 | 2019-06-04 | 广东乔艺塑胶有限公司 | A kind of antibiotic plastic and preparation method thereof |
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| WO2019062675A1 (en) * | 2017-09-27 | 2019-04-04 | 江南大学 | Non-migrating high-efficiency antibacterial composite material and manufacturing method therefor |
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| CN113829689A (en) * | 2021-10-19 | 2021-12-24 | 深圳市石能纸业有限公司 | Antibacterial modified stone paper and production and preparation method thereof |
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