抗菌羊毛纤维制备及其结构与性能研究
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摘要
随着社会的发展和人民生活水平的提高,人们对功能性纺织品的需求越来越高,这在一定程度上推动了功能性纺织品的开发进程,今后的纺织品生产,功能性将成为其生存和发展的决定性因素。作为人类有史以来应用最久,最多的传统纤维天然纤维—羊毛纤维不仅是纺织工业的重要原料,而且它具有许多其它纤维不能与之媲美优良的特性。但是作为天然蛋白质纤维—羊毛本身并不具有抗菌功能,它的制品往往为细菌提供了生存的“温床”,对人体健康及环境造成一定的威胁。随着人们对时尚的追求,功能性羊毛制品越来越受到人们的喜爱和亲睐。于是赋予天然羊毛纤维抗菌功能就成了当前所面临的一项重要的攻坚任务。我国又是羊毛生产的重要大国,这就为研究更多更好的抗菌羊毛产品奠定了坚实的基础。
实验首先研究了不同紫外光(UV)辐照时间对羊毛纤维的结构与性能的影响,并对UV辐照羊毛纤维表面的改性机理进行了初步的探讨;然后制备了载银纳米SiO2抗菌剂(SLS)与壳聚糖-载银二氧化硅抗菌剂(CCTS-SLS),对其结构与性能进行了详细讨论;最后以SLS与CCTS-SLS为抗菌功能材料,采用化学接枝的方法制得抗菌羊毛纤维,并对抗菌羊毛纤维结构、性能以及抗菌层形成机理进行了系统的研究。
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)、FTIR1730红外光谱测试仪(IR)和RFS100/S型拉曼光谱仪(FTR)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)和ESCALABMKⅡ型多功能电子能谱仪(XPS)表征了样品中的银含量;通过DT-40型差热-热重分析仪表征了样品的热性能;采用活菌计数法、最小抑菌浓度法或振荡烧瓶法对各样品的抗菌性能进行了测试。同时还测试了羊毛纤维的热稳定性、力学性能和摩擦性能。
通过上述研究,主要取得了以下结论:
(1)随着辐照时间的增加,羊毛纤维结晶度在不断下降,分子结构中无序化程度提高。羊毛纤维的断裂强力、断裂伸长率、断裂强度在不断下降。UV辐照可在羊毛纤维表面形成活性自由基和悬键,并引入许多新的基团,可进行接枝改性。
(2)制备的SLS抗菌剂,抗菌剂呈球形,其平均粒径约60nm,且分布均匀。SLS抗菌剂具有良好的缓释性能,对大肠杆菌和金黄色葡萄球菌均具有良好的抗菌性能。
(3)采用最佳工艺制备的SLS抗菌羊毛纤维,表面形成了一层厚约200 nm的抗菌层,抗菌层与羊毛纤维以价键形式结合,使其摩擦性能和抗菌耐洗涤性能提高。在改性过程中,抗菌羊毛纤维分子的有序化程度提高,使其具有良好的力学性能和热稳定性。制备的抗菌羊毛纤维长度较长,细度变细,卷曲回复率和卷曲弹性率高,这些均有利于提高它的纺织加工性能。
(4)制备的CCTS-SLS抗菌剂,为层状无定形镶嵌结构,具有CTS与SLS两者的分子结构特征,SLS颗粒包裹在了壳聚糖分子层中,所形成的颗粒大小约110nm左右,颗粒的外围被厚约4nm的CTS分子层包覆,并且复合物中的银含量与SLS相似。CCTS-SLS复合物的缓释性能较好,并具有良好的抗菌性能。
(5) CCTS-SLS-Wool抗菌羊毛纤维,品质良好,手感柔软,颜色与原羊毛纤维颜色接近,并且CCTS-SLS抗菌剂是以价键形式接枝在了羊毛纤维表面,其分子结构的有序化程度与原羊毛接近。它的力学性能、摩擦性能、热稳定性和抗菌耐洗涤性能与原羊毛纤维相比均有提高。
利用外场诱导方法即UV辐照的方法对天然羊毛纤维进行表面改性,并将纳米抗菌功能基团通过接枝反应,形成化学键结合的纳米抗菌功能材料/纤维界面层,本质上区别于传统的物理吸附,实现了纤维的抗菌功能长效性、高力学性能和低成本,提高了羊毛纤维的应用与功能等级,改善了其可纺性、服用性和功能内涵,使其性价比和附加值得以提升,并克服了传统处理法水溶液排量多、污染大的问题,有利于节能减排和环境保护。提出的天然羊毛纤维表面纳米功能化改性机理,为建立天然纤维/纳米功能材料结合界面结构化学模型奠定了基础,对高性能功能纤维设计与生产起到重要的理论指导作用。
With the development of society and improvement of living standard, the demand for functional textiles is getting higher and higher, which, to some extent, promotes the development of functional textiles. In the future of textile production, functionality will become the decisive factor in development. Natural wool fiber has been widely used for long in human being history. Being lighter, warmer, softer and smoother than other fibers, wool has been known as superior textile material. But natural wool fiber is not antibacterial and wool textiles can provide living space for bacteria, which is harmful to health and environment. Along with their aspiration for new style, people choose functional wool textiles with more favor. Therefore, it becomes an important challenge to make wool fiber antibacterial. Moreover, China is among the main countries for wool production in the world , which provides good opportunities to develop antibacterial wool products.
In this paper, the effect of ultraviolet (UV) irradiation on the structures and properties of wool fiber were studied. The mechanism of surface modification of wool fiber by UV irradiation was discussed. Silver-loading nano-SiO2 antibacterial agent (SLS) and chitosan crosslinked Ag-loading nano-SiO2 antibacterial agent (CCTS-SLS) were prepared and discussed in detail with respect to their molecular structures and properties. Antibacterial wool fibers were obtained by grafting SLS and CCTS-SLS antibacterial functional materials. The structures and properties of antibacterial wool fibers and the grafting mechanisms of SLS and CCTS-SLS on wool fiber surfaces 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), infrared spectroscopy (IR) and Fourier transformation Raman spectrometry (FTR). The contents of silver were measured with inductively coupled plasma spectrometry (ICPS) and X-ray photoelectron spectroscopy (XPS). The antibacterial properties of all specimens were tested using alive-bacteria-counting, minimum inhibitory concentration method (MIC), or flask-shaking method. The thermal stability, mechanical properties and friction behaviors were also measured.
The main conclusions are as follows:
(1) With the increase of UV irradiation time, the crystallinity of wool fiber was continuously declined, along with the increase in the degree of disorder in the molecular structure. Moreover, the force, tensile strength and elongation were decreased. The some active free radicals and dangling bonds were formed on the surface of wool fiber during UV irradiation along with the introduction of a lot of new groups, which can be used for grafting with antibacterial agents.
(2) The SLS antibacterial agent was narrowly distributed spherical particles with the mean particle size of 60 nm. They exhibited excellent release property of silver ions and good antibacterial performance against E. coil and S. aureus.
(3) The antibacterial wool fiber grafted with SLS under optimized conditions had an antibacterial layer of 200 nm in thickness, which was formed on the wool fiber surface by covalent bonding between SLS and wool fiber. The antibacterial wool fiber showed excellent friction performance and wash resistance property. The improved degree of disorder in the molecular structure during the modification resulted in the good mechanical property and thermal stability. The SLS-wool it was longer and thinner with higher crimp recovery and crimp elasticity, which may be more suitable for processing on conventional textile machinery.
(4) The morphologies of CCTS-SLS particles were amorphous, layered and embedded with mean particle sizes of 110 nm, which had the characteristic FTIR bands occurring in CTS and SLS. SLS particles were coated by CCTS layer with the thickness of 4 nm. In addition, the content of silver in CCTS-SLS was similar to that of SLS. CCTS-SLS had excellent release property and antibacterial performance, the same as SLS.
(5) The antibacterial wool fiber grafted with CCTS-SLS had good hand-feeling, thus fully exhibiting the excellent characters of wool fibers. The color was closed to that of original wool fiber. CCTS-SLS particles were grafted by covalent bonding on the surface of wool fiber. The degree of order in the molecular structure was similar to that of original wool fiber. Compared with original wool fiber, CCTS-SLS-wool was improved in mechanical, frictional, thermal and antibacterial wash-resistant properties.
The surface modification of natural wool fiber was realized using the method of UV radiation. Nano-antibacterial functional materials / fiber interfacial layer came into being in the form of chemical bond combination by grafting reaction, which was clearly different from traditional physical adsorption. This kind of antibacterial functionalization shows many advantages. Firstly, it realizes lasting antibacterial effect, excellent mechanical property and low cost; Secondly, it increases the grade of wool fiber in application and function; Thirdly, it improves the spinnability, serviceability and functionality of wool, thus greatly increasing added value. Finally, it prevents the emissions of contaminated aqueous solution in traditional treatment process and therefore conducive to energy saving, emission reduction and environmental protection. The surface functional modification mechanism of natural wool fiber lays the foundation of the interface structural model between natural fiber and nano-function materials, which, plays an important role of theoretical guidance for the design and manufacture of high-performance fibers.
实验首先研究了不同紫外光(UV)辐照时间对羊毛纤维的结构与性能的影响,并对UV辐照羊毛纤维表面的改性机理进行了初步的探讨;然后制备了载银纳米SiO2抗菌剂(SLS)与壳聚糖-载银二氧化硅抗菌剂(CCTS-SLS),对其结构与性能进行了详细讨论;最后以SLS与CCTS-SLS为抗菌功能材料,采用化学接枝的方法制得抗菌羊毛纤维,并对抗菌羊毛纤维结构、性能以及抗菌层形成机理进行了系统的研究。
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)、FTIR1730红外光谱测试仪(IR)和RFS100/S型拉曼光谱仪(FTR)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)和ESCALABMKⅡ型多功能电子能谱仪(XPS)表征了样品中的银含量;通过DT-40型差热-热重分析仪表征了样品的热性能;采用活菌计数法、最小抑菌浓度法或振荡烧瓶法对各样品的抗菌性能进行了测试。同时还测试了羊毛纤维的热稳定性、力学性能和摩擦性能。
通过上述研究,主要取得了以下结论:
(1)随着辐照时间的增加,羊毛纤维结晶度在不断下降,分子结构中无序化程度提高。羊毛纤维的断裂强力、断裂伸长率、断裂强度在不断下降。UV辐照可在羊毛纤维表面形成活性自由基和悬键,并引入许多新的基团,可进行接枝改性。
(2)制备的SLS抗菌剂,抗菌剂呈球形,其平均粒径约60nm,且分布均匀。SLS抗菌剂具有良好的缓释性能,对大肠杆菌和金黄色葡萄球菌均具有良好的抗菌性能。
(3)采用最佳工艺制备的SLS抗菌羊毛纤维,表面形成了一层厚约200 nm的抗菌层,抗菌层与羊毛纤维以价键形式结合,使其摩擦性能和抗菌耐洗涤性能提高。在改性过程中,抗菌羊毛纤维分子的有序化程度提高,使其具有良好的力学性能和热稳定性。制备的抗菌羊毛纤维长度较长,细度变细,卷曲回复率和卷曲弹性率高,这些均有利于提高它的纺织加工性能。
(4)制备的CCTS-SLS抗菌剂,为层状无定形镶嵌结构,具有CTS与SLS两者的分子结构特征,SLS颗粒包裹在了壳聚糖分子层中,所形成的颗粒大小约110nm左右,颗粒的外围被厚约4nm的CTS分子层包覆,并且复合物中的银含量与SLS相似。CCTS-SLS复合物的缓释性能较好,并具有良好的抗菌性能。
(5) CCTS-SLS-Wool抗菌羊毛纤维,品质良好,手感柔软,颜色与原羊毛纤维颜色接近,并且CCTS-SLS抗菌剂是以价键形式接枝在了羊毛纤维表面,其分子结构的有序化程度与原羊毛接近。它的力学性能、摩擦性能、热稳定性和抗菌耐洗涤性能与原羊毛纤维相比均有提高。
利用外场诱导方法即UV辐照的方法对天然羊毛纤维进行表面改性,并将纳米抗菌功能基团通过接枝反应,形成化学键结合的纳米抗菌功能材料/纤维界面层,本质上区别于传统的物理吸附,实现了纤维的抗菌功能长效性、高力学性能和低成本,提高了羊毛纤维的应用与功能等级,改善了其可纺性、服用性和功能内涵,使其性价比和附加值得以提升,并克服了传统处理法水溶液排量多、污染大的问题,有利于节能减排和环境保护。提出的天然羊毛纤维表面纳米功能化改性机理,为建立天然纤维/纳米功能材料结合界面结构化学模型奠定了基础,对高性能功能纤维设计与生产起到重要的理论指导作用。
With the development of society and improvement of living standard, the demand for functional textiles is getting higher and higher, which, to some extent, promotes the development of functional textiles. In the future of textile production, functionality will become the decisive factor in development. Natural wool fiber has been widely used for long in human being history. Being lighter, warmer, softer and smoother than other fibers, wool has been known as superior textile material. But natural wool fiber is not antibacterial and wool textiles can provide living space for bacteria, which is harmful to health and environment. Along with their aspiration for new style, people choose functional wool textiles with more favor. Therefore, it becomes an important challenge to make wool fiber antibacterial. Moreover, China is among the main countries for wool production in the world , which provides good opportunities to develop antibacterial wool products.
In this paper, the effect of ultraviolet (UV) irradiation on the structures and properties of wool fiber were studied. The mechanism of surface modification of wool fiber by UV irradiation was discussed. Silver-loading nano-SiO2 antibacterial agent (SLS) and chitosan crosslinked Ag-loading nano-SiO2 antibacterial agent (CCTS-SLS) were prepared and discussed in detail with respect to their molecular structures and properties. Antibacterial wool fibers were obtained by grafting SLS and CCTS-SLS antibacterial functional materials. The structures and properties of antibacterial wool fibers and the grafting mechanisms of SLS and CCTS-SLS on wool fiber surfaces 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), infrared spectroscopy (IR) and Fourier transformation Raman spectrometry (FTR). The contents of silver were measured with inductively coupled plasma spectrometry (ICPS) and X-ray photoelectron spectroscopy (XPS). The antibacterial properties of all specimens were tested using alive-bacteria-counting, minimum inhibitory concentration method (MIC), or flask-shaking method. The thermal stability, mechanical properties and friction behaviors were also measured.
The main conclusions are as follows:
(1) With the increase of UV irradiation time, the crystallinity of wool fiber was continuously declined, along with the increase in the degree of disorder in the molecular structure. Moreover, the force, tensile strength and elongation were decreased. The some active free radicals and dangling bonds were formed on the surface of wool fiber during UV irradiation along with the introduction of a lot of new groups, which can be used for grafting with antibacterial agents.
(2) The SLS antibacterial agent was narrowly distributed spherical particles with the mean particle size of 60 nm. They exhibited excellent release property of silver ions and good antibacterial performance against E. coil and S. aureus.
(3) The antibacterial wool fiber grafted with SLS under optimized conditions had an antibacterial layer of 200 nm in thickness, which was formed on the wool fiber surface by covalent bonding between SLS and wool fiber. The antibacterial wool fiber showed excellent friction performance and wash resistance property. The improved degree of disorder in the molecular structure during the modification resulted in the good mechanical property and thermal stability. The SLS-wool it was longer and thinner with higher crimp recovery and crimp elasticity, which may be more suitable for processing on conventional textile machinery.
(4) The morphologies of CCTS-SLS particles were amorphous, layered and embedded with mean particle sizes of 110 nm, which had the characteristic FTIR bands occurring in CTS and SLS. SLS particles were coated by CCTS layer with the thickness of 4 nm. In addition, the content of silver in CCTS-SLS was similar to that of SLS. CCTS-SLS had excellent release property and antibacterial performance, the same as SLS.
(5) The antibacterial wool fiber grafted with CCTS-SLS had good hand-feeling, thus fully exhibiting the excellent characters of wool fibers. The color was closed to that of original wool fiber. CCTS-SLS particles were grafted by covalent bonding on the surface of wool fiber. The degree of order in the molecular structure was similar to that of original wool fiber. Compared with original wool fiber, CCTS-SLS-wool was improved in mechanical, frictional, thermal and antibacterial wash-resistant properties.
The surface modification of natural wool fiber was realized using the method of UV radiation. Nano-antibacterial functional materials / fiber interfacial layer came into being in the form of chemical bond combination by grafting reaction, which was clearly different from traditional physical adsorption. This kind of antibacterial functionalization shows many advantages. Firstly, it realizes lasting antibacterial effect, excellent mechanical property and low cost; Secondly, it increases the grade of wool fiber in application and function; Thirdly, it improves the spinnability, serviceability and functionality of wool, thus greatly increasing added value. Finally, it prevents the emissions of contaminated aqueous solution in traditional treatment process and therefore conducive to energy saving, emission reduction and environmental protection. The surface functional modification mechanism of natural wool fiber lays the foundation of the interface structural model between natural fiber and nano-function materials, which, plays an important role of theoretical guidance for the design and manufacture of high-performance fibers.
引文
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