摘要
纺织材料在朝着功能化、舒适化和卫生保健的方向发展的过程中,抗菌纤维材料越来越引起了人们的关注。无机抗菌剂能够克服天然和有机抗菌剂在耐高温、耐洗涤、安全性、持久性等方面的不足,并可采用多种方法制备抗菌纤维,因而采用无机抗菌剂作为抗菌功能材料制备抗菌纤维的研究日益增多。自1991年Iijima发现碳纳米管(CNTs)以来,CNTs独特的结构、优异的物理和化学性能使其在许多领域具有潜在的应用前景,CNTs/高聚物复合材料已成为目前材料科学领域的研究热点之一。以CNTs为载体制备载银CNTs抗菌剂,并考察其在纤维中的应用具有重要的研究意义。
本文采用第一性原理计算了银在CNTs内壁和经羧基和羟基修饰的外壁上吸附后的结构和稳定性;选择经硝酸氧化处理的多壁碳纳米管(MWNTs)为载体,AgNO3溶液为反应液,通过吸附法制成了载银MWNTs抗菌剂(Ag/MWNTs);以Ag/MWNTs抗菌剂为功能材料,采用紫外光(UV)辐照的方法制备了Ag/MWNTs抗菌羊毛纤维;采用双螺杆挤出机制备了Ag/MWNTs抗菌PET母粒,并用熔融纺丝技术纺制抗菌PETFDY功能纤维,对纺丝工艺、抗菌PET母粒的添加量等对抗菌PETFDY功能纤维的可纺性的影响进行了系统的研究。
实验采用JSM-6700F型场发射扫描电镜(SEM)观察了样品的形貌;通过JEM-2010型高分辨透射电镜(HRTEM)、Y-2000型X射线衍射仪(XRD)和FTIR1730红外光谱测试仪(IR)表征了样品的结构;利用LABTAM-8410型等离子体原子发射光谱仪(ICPS)测定了样品中的银含量;采用DSC6200型差示扫描量热仪(DSC)测定了样品的结晶度;采用活菌计数法或振荡烧瓶法对样品的抗菌性能进行了测试。
上述研究围绕抗菌功能材料的设计并对其在天然羊毛纤维和合成纤维PET上应用进行了工艺参数优化,主要取得了以下结论:
(1) Ag离子在修饰后的CNTs中的负载主要以物理吸附为主;
(2)经硝酸氧化处理后的MWNTs可以作为载体,通过吸附法制备Ag/MWNTs抗菌剂,且具有良好的缓释和抗菌性能;
(3)采用“UV辐照处理后的羊毛纤维在抗菌功能溶液中浸渍,并进行二次UV辐照处理,可制得吸附率较高的Ag/MWNTs抗菌羊毛纤维,该纤维具有优良的热稳定性能,以及优良的抗菌和耐洗涤性能;
(4)采用双螺杆熔融共混挤出机可以制备具有良好的分散性和抗菌性能的抗菌PET功能纤维母粒,且可促进Ag/MWNTs抗菌剂沿样条轴向取向,有利于提高Ag/MWNTs抗菌PET功能纤维的可纺性;
(5)采用母粒熔融共混纺丝法可以纺制具有良好抗菌性能的抗菌PETFDY功能纤维。
In the development process of textile materials toward being functional, comfortable and healthy, more attention is being paid to the antibacterial fibers. Inorganic antimicrobial agents which are superior over natural and organic antibacterial agents in heat-resisting, launderability, safety and durability, can be used for manufacturing antibacterial fibers by different methods. Therefore, there are ever-increasing research in preparing antibacterial fibers in which inorganic antibacterial agents are used as antibacterial functional materials. Since its discovery by Iijima in 1991, carbon nanotubes (CNTs) with unique structures and excellent physical and chemical properties have exhibited promising applications in many areas. CNTs / polymer composite materials have become a hot topic in the field of material research. It is of significance to develop CNTs-supported silver antibacterial agents and explore their use fibers.
In present paper the first-principle simulation was carried out to investigate the structure and stability of silver adsorbed on the internal-walls and the outer-walls of CNTs, with the outer-walls modified by carboxyl and hydroxyl groups. Multi-walled carbon nanotubes (MWNTs) were oxidized in nitric acid and then used as carrier to perpare Ag/MWNTs antibacterial agent by adsorption in AgNO3 solution.With the Ag/MWNTs antibacterial agent as functional material, the Ag/MWNTs antibacterial wool fibers were prepared by ultraviolet (UV) irradiation method. Ag/MWNTs antibacterial PET masterbatch was prepared with a twin-screw extruder. Melt spinning technique was adopted to spin antibacterial PETFDY fiber. The influences of the spinning technology and the additive amount of anti-bacterial PET masterbatch on the spinnability of antibacterial PETFDY function fibers were systematically investigated.
The morphologies of the samples were observed by Scanning Electron Microscopy (SEM). The structures of specimens were characterized by High-Resolution Transmission Electron Microscopy (HRTEM), X-ray diffraction (XRD), and Infrared Spectrometry (IR). The contents of silver were measured with Inductively Coupled Plasma Spectrometry (ICPS). The degree of crystallinity was measured with differential scanning calorimetry (DSC). The antibacterial properties of all specimens were tested using alive-bacteria-counting and flask-shaking methods.
With emphasis on the design of antibacterial functional materials and the process optimization for their applications in natural wool fibers and PET fibers, this study reached the main conclusions as follows.
(1)The loading of Ag ions in the modified CNTs was mainly by physical adsorption.
(2)HNO3-treated MWNTs used as carrier to prepare Ag/MWNTs antibacterial agent by adsorption. It had excellent release and antibacterial properties.
(3) The antibacterial wool fibers were prepared by“UV-treatment + dipping + secondary UV-irradiation +washing and drying”. The fibers exhibited excellent thermal, antibacterial and wash-resistant properties.
(4) Ag/MWNTs antibacterial PET masterbatch with good dispersity and antibacterial property was prepared using a twin-screw extruder. The orientation of Ag/MWNTs antibacterial agents was promoted along the axial direction, which was beneficial to improve the spinnability of antibacterial PET fibers.
(5)Ag/MWNTs antibacterial PETFDY fibers with excellent antibacterial property were prepared by melt spinning technique.
引文
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