银/聚合物纳米复合材料的制备、结构和抗菌性能研究
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摘要
银(Ag)纳米粒子是一种安全、持久的高效金属抗菌剂,将其与聚合物复合,不仅可改善Ag的分散性,还可赋予或增强高分子材料的抗菌性能。本文在离子液体1-丁基-3-甲基咪唑氟硼酸盐([BMIM]·BF4)中制备了稳定的Ag纳米胶体,并以[BMIM]·BF4/乙醇为混和溶剂,通过原位聚合方式制备出银/聚苯乙烯(Ag/PS)纳米核壳复合粒子。在苯乙烯聚合过程中,Ag与[BMIM]·BF4分子之间的强吸附作用,阻止了Ag粒子的团聚,而使之包覆在PS中。
采用液相化学还原法合成出Ag/壳聚糖(CS)复合胶乳,继而制备了Ag/CS-g-甲基丙烯酸甲酯(MMA)复合物。研究结果表明,Ag纳米粒子对CS与MMA的接枝聚合起阻碍作用,导致接枝率和接枝效率比无Ag粒子存在时有所下降。通过结构表征和机理分析证明,CS分子吸附Ag而形成了Ag-O键,并且通过静电效应和位阻效应阻止了Ag纳米粒子的聚集,使其均匀分散于复合物中;MMA在CS的羟基上发生了接枝共聚反应;与Ag纳米粒子复合后的CS及CS-g-MMA的热稳定性明显高于纯CS。
通过电纺方法制备了Ag/CS/聚氧化乙烯(PEO)复合超细纤维膜。利用扫描电镜和透射电镜观察了不同纺丝条件下电纺膜的微观形貌,结果表明,在Ag纳米粒子存在下可电纺得到形貌良好的超细纤维,Ag粒子均匀分布于纤维膜中。X-光电子能谱分析显示有约10%的Ag元素分布在了纤维膜的表面。吸水率测定结果表明,含有Ag纳米粒子的Ag/CS/PEO电纺纤维膜与CS/PEO电纺膜比较,其吸水率有所提高。拉伸试验表明Ag纳米粒子的引入提高了复合电纺膜的力学性能,其力学性能在湿态下较干态下有所下降。
抗菌评价研究结果表明,所制备的Ag纳米粒子具有明显的抗菌性能;Ag/PS核壳复合粒子的抑菌具有长效性;Ag/CS复合抗菌剂具有比单一抗菌剂更高效的抗菌性能;探讨了Ag纳米粒子和CS的抗菌机理,指出Ag/CS基复合抗菌剂的抗菌性能是Ag纳米粒子和CS协同作用的结果。
Silver (Ag) nanoparticle is a kind of high-performance metallic antimicrobial agents with security and durability. Compounding Ag nanoparticles with polymer could not only improve their dispersability but also provide with or enhance the antimicrobial properties of polymer materials.
In the present studys, Ag nanocolloids were synthesized in a room-temperature ionic liquid, 1-n-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]·BF4). And then Ag/polystyrene (PS) core/shell nanoparticles were prepared via in situ polymerization in the [BMIM]·BF4/ethanol mixed solvent. In the process of styrene polymerization, the strong sorption between Ag and [BMIM]·BF4 prevented Ag nanoparticles from aggregation, and made them disperse uniformly. Ag nanoparticles were finally embedded in PS.
Ag/chitosan (CS) composite colloids were synthesized by liquid-phase chemical reduction and then Ag/CS-g-methylmethacrylate (MMA) composite was prepared by graft polymerization. The results showed that Ag nanoparticles hindered the graft polymerization of CS with MMA, which resulted in the decrease of the graft percentage and graft efficiency in comparison with those without Ag nanoparticles.
Structural characterization and mechanism analysis verified that Ag-O bonds were formed by adsorption between CS molecules and Ag, and prevented Ag nanoparticles from aggregation through electrostatic effect and steric effect, which made Ag nanoparticles dispersed evenly in the composites. The graft copolymerization of CS with MMA was initiated on the hydroxide group of CS. After compounding with Ag nanoparticles, the thermal stability of CS and its graft product, CS-g-MMA was significantly increased in comparison with that of original CS.
Ag/CS/poly(ethylene oxide) (PEO) composite fibrous membrane was produced by electrospinning. The morphologies of electrospun fibers under different electrospining conditions were analyzed by scanning electron microscope and transmission electron microscope. The results indicated that the ultrafine fibers with fine morphology could be obtained by electrospinning at the present of Ag nanoparticles, and the nanoparticles were dispersed uniformly in the electrospun fibers. The result of X-ray photoelectron spectroscopy revealed that approximately 10% of Ag element distributed on the surface of the fibrous membranes. The Ag/CS/PEO membrane showed a higher water uptake than that of CS/PEO electrospun membrane. The composite Ag/CS/PEO fibrous membranes showed better tensile properties than CS/PEO membrane due to the introduction of Ag nanoparticles, but the tensile properties got worse in wet state.
Evaluation of antimicrobial activities showed that the resultant Ag nanoparticles demonstrated perfect antibacterial property, while Ag/PS core/shell nanocomposite particles displayed prolonged antibacterial effect and the Ag/CS composites existed higher antibacterial performance than Ag or CS alone. The antibacterial mechanisms of Ag nanoparticles and CS were studied. The antibacterial activities of Ag/CS based antimicrobial were displayed by the cooperation of Ag nanoparticles with CS.
采用液相化学还原法合成出Ag/壳聚糖(CS)复合胶乳,继而制备了Ag/CS-g-甲基丙烯酸甲酯(MMA)复合物。研究结果表明,Ag纳米粒子对CS与MMA的接枝聚合起阻碍作用,导致接枝率和接枝效率比无Ag粒子存在时有所下降。通过结构表征和机理分析证明,CS分子吸附Ag而形成了Ag-O键,并且通过静电效应和位阻效应阻止了Ag纳米粒子的聚集,使其均匀分散于复合物中;MMA在CS的羟基上发生了接枝共聚反应;与Ag纳米粒子复合后的CS及CS-g-MMA的热稳定性明显高于纯CS。
通过电纺方法制备了Ag/CS/聚氧化乙烯(PEO)复合超细纤维膜。利用扫描电镜和透射电镜观察了不同纺丝条件下电纺膜的微观形貌,结果表明,在Ag纳米粒子存在下可电纺得到形貌良好的超细纤维,Ag粒子均匀分布于纤维膜中。X-光电子能谱分析显示有约10%的Ag元素分布在了纤维膜的表面。吸水率测定结果表明,含有Ag纳米粒子的Ag/CS/PEO电纺纤维膜与CS/PEO电纺膜比较,其吸水率有所提高。拉伸试验表明Ag纳米粒子的引入提高了复合电纺膜的力学性能,其力学性能在湿态下较干态下有所下降。
抗菌评价研究结果表明,所制备的Ag纳米粒子具有明显的抗菌性能;Ag/PS核壳复合粒子的抑菌具有长效性;Ag/CS复合抗菌剂具有比单一抗菌剂更高效的抗菌性能;探讨了Ag纳米粒子和CS的抗菌机理,指出Ag/CS基复合抗菌剂的抗菌性能是Ag纳米粒子和CS协同作用的结果。
Silver (Ag) nanoparticle is a kind of high-performance metallic antimicrobial agents with security and durability. Compounding Ag nanoparticles with polymer could not only improve their dispersability but also provide with or enhance the antimicrobial properties of polymer materials.
In the present studys, Ag nanocolloids were synthesized in a room-temperature ionic liquid, 1-n-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]·BF4). And then Ag/polystyrene (PS) core/shell nanoparticles were prepared via in situ polymerization in the [BMIM]·BF4/ethanol mixed solvent. In the process of styrene polymerization, the strong sorption between Ag and [BMIM]·BF4 prevented Ag nanoparticles from aggregation, and made them disperse uniformly. Ag nanoparticles were finally embedded in PS.
Ag/chitosan (CS) composite colloids were synthesized by liquid-phase chemical reduction and then Ag/CS-g-methylmethacrylate (MMA) composite was prepared by graft polymerization. The results showed that Ag nanoparticles hindered the graft polymerization of CS with MMA, which resulted in the decrease of the graft percentage and graft efficiency in comparison with those without Ag nanoparticles.
Structural characterization and mechanism analysis verified that Ag-O bonds were formed by adsorption between CS molecules and Ag, and prevented Ag nanoparticles from aggregation through electrostatic effect and steric effect, which made Ag nanoparticles dispersed evenly in the composites. The graft copolymerization of CS with MMA was initiated on the hydroxide group of CS. After compounding with Ag nanoparticles, the thermal stability of CS and its graft product, CS-g-MMA was significantly increased in comparison with that of original CS.
Ag/CS/poly(ethylene oxide) (PEO) composite fibrous membrane was produced by electrospinning. The morphologies of electrospun fibers under different electrospining conditions were analyzed by scanning electron microscope and transmission electron microscope. The results indicated that the ultrafine fibers with fine morphology could be obtained by electrospinning at the present of Ag nanoparticles, and the nanoparticles were dispersed uniformly in the electrospun fibers. The result of X-ray photoelectron spectroscopy revealed that approximately 10% of Ag element distributed on the surface of the fibrous membranes. The Ag/CS/PEO membrane showed a higher water uptake than that of CS/PEO electrospun membrane. The composite Ag/CS/PEO fibrous membranes showed better tensile properties than CS/PEO membrane due to the introduction of Ag nanoparticles, but the tensile properties got worse in wet state.
Evaluation of antimicrobial activities showed that the resultant Ag nanoparticles demonstrated perfect antibacterial property, while Ag/PS core/shell nanocomposite particles displayed prolonged antibacterial effect and the Ag/CS composites existed higher antibacterial performance than Ag or CS alone. The antibacterial mechanisms of Ag nanoparticles and CS were studied. The antibacterial activities of Ag/CS based antimicrobial were displayed by the cooperation of Ag nanoparticles with CS.
引文
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