高分子—氧化钛纳米杂化膜的制备与初步应用
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摘要
有机-无机杂化膜结合了传统有机膜与无机膜的优良性能,其制备和应用研究是当前膜领域的研究前沿和热点。TiO_2具有较高的化学稳定性、耐光腐蚀性和光催化活性、很强的散射和吸收紫外光能力和杀菌能力,填充在有机膜中,可提高膜的热稳定性、机械强度和渗透性能,并且TiO_2本身的特性也会在杂化膜中得到体现,因此,近年来高分子-TiO_2杂化膜的研究受到广泛关注。
目前,有机-无机杂化膜通常以物理或化学方法制备,随着近年来社会对环境保护的日益关注,寻求绿色合成方法逐渐成为一项具有挑战性的工作。
本文制备了多种生物高分子-氧化钛杂化膜,发明了一种合成有机-无机杂化膜的纯生物方法,并探讨了这些杂化膜的初步应用。
有鉴于此,本文首次利用纯生物方法制备了细菌纤维素-TiO_2纳米杂化膜,为有机-无机杂化膜的绿色合成提供了一个很好的思路;探讨了作为无机填充物的氧化钛的形貌和结构对高分子-TiO_2杂化膜分离性能的影响,并探索了这些杂化膜的初步应用。
首先,以木醋杆菌为多功能微生物反应器,一步合成了细菌纤维素-TiO_2纳米杂化膜,并且对其形成机理和应用进行了初步研究,对制备材料进行了X射线衍射、X射线光电子能谱、扫描电子显微镜和投射电子显微镜等表征。通过向培养基中加入钛前驱体二(2-羟基丙酸)二氢氧化二铵合钛,合成了细菌纤维素-TiO_2纳米杂化膜。研究表明:细菌纤维素膜是由直径为60-120nm的纳米纤维构成的三维网状结构,TiO_2的引入未改变细菌纤维素的微观结构,生成的30-50nm的TiO_2颗粒主要镶嵌在细菌纤维素的网络中,含量可达到4wt%。木醋杆菌在合成细菌纤维素的同时,矿化钛前驱体生成TiO_2纳米颗粒,细胞壁/膜在TiO_2合成过程中起到了重要作用。类似的,通过向培养基中加入硅酸钠和硅酸,生物合成了细菌纤维素-SiO_2纳米杂化膜,表明这种生物方法具有一定的通用性。
其次,为了解决生物合成法中TiO_2纳米颗粒在杂化膜中含量较低的问题,利用原位合成法制备细菌纤维素-TiO_2纳米杂化膜。通过向培养基中加入水热法合成的TiO_2凝胶纳米颗粒,原位合成了细菌纤维素-TiO_2纳米杂化膜,TiO_2凝胶颗粒的加入对木醋杆菌的生长未产生影响。TiO_2的引入未改变细菌纤维素的微观结构,TiO_2主要包埋在细菌纤维素网络结构中,含量可达到7.1%。据推测,在细菌纤维素膜的合成过程中,悬浮在培养基中的氧化钛胶体颗粒被包裹其中,从而最终形成了杂化膜。
第三,为研究具有特殊形貌和结构TiO_2对纳米杂化膜性能的影响,将水热法制备的钛酸盐纳米管与生物高分子壳聚糖(CS)共混,制备了CS-TNTs纳米杂化膜,并研究了其作为直接甲醇燃料电池质子交换膜的性能。由于TNTs的表面羟基与壳聚糖高分子链段上的羟基和氨基形成氢键相互作用,使TNTs很好分散在CS基质中,提高了杂化膜的机械性能和热稳定性;TNTs引入降低了杂化膜的自由体积分数,有效降低了杂化膜的甲醇渗透性能。其中,含15wt%的TNTs的CS-TNTs纳米杂化膜的机械强度为85.0Mpa,甲醇渗透率为为0.497×10~(-6) cm~2/s,质子传导率为0.0151S cm~(-1),具有较好的应用前景。
Recently, it has been focused on the fabrication and application of organic-inorganic composite membranes, owing to its combining the advantages of traditional organic and inorganic membrane. TiO_2 has a high chemical stability, light corrosion and photocatalytic activity, strong scattering ability, absorption of UV light, and sterilization. When incorporated into Polymer matrix, TiO_2 can increase the thermal stability, mechanical strength and permeability of composite membrane. The characteristic properties of TiO_2 can be reflected in the hybrid membrane. Therefore, polymer-TiO_2 hybrid membranes have been attracted wide spread concern.
Currently, organic-inorganic hybrid membranes are usually prepared by physical or chemical methods. Green synthesis method is becoming a challenging task with the growing concern on environmental protection.
In this article, a pure biological method was used to one pot synthesizing bacterial cellulose-TiO_2 composite membrane at the first time. It provides a good green synthesis strategy. The effect of morphology and structure of TiO_2 on the separation property and the preliminary application of hybrid membranes were explored.
First, Acetobacter was used as a multi-reactor to one pot synthesizing bacterial cllulose(BC)-TiO_2 nanocomoposite. The formation mechanism and preliminary application of BC-TiO_2 nanocomposite are explored, and characterized by X-ray diffraction, X-ray Photoelectron Spectroscopy, scanning electron microscope, and transmission electron microscopy. BC-TiO_2 nanocomposite was fabricated by adding the precursor titanium(IV) bis(ammonium lactato) dihydroxide into the culture medium. The results show that three dimensional bacterial cellulose membrane is composed of 60-120nm cellulose fibril. The introduction of TiO_2 does not change the microstructure of the membrane. TiO_2 nanoparticles with size of 30-50nm are main embedded in the bacterial cellulose network, the content of it can reach 4wt%. Acetobacter synthesize bacterial cellulose and mineralize TiO_2 simultaneously. Cell wall/membrane plays an important role in the mineralization of TiO_2. Similarly, when sodium silicate or silicic acid added into the culture medium, BC-SiO_2 nanocomposite membranes were synthesized. It shows that the biological method has some versatility.
Secondly, in order to enhance the TiO_2 nanoparticles content in the BC-TiO_2 membrane, BC-TiO_2 nanocomposite membrane are fabricated by in situ method. The growth of Acetobacter is not affect by adding TiO_2 gel particles into the culture medium, and the microstructure of the nanocomposite membrane does not change. TiO_2 nanoparticles are mainly embedded in the bacterial cellulose network, the content of it can reach up to 7.1wt%. It is supposed that the suspended TiO_2 in the culture medium are wrapped into the network when the bacterial cellulose are synthesized, and finally formed a nanocomposite membrane.
Third, in order to study the impact of the morphology and structure on the properties of composite membrane, Titanate nanotubes(TNTs) with layered structure synthesized by the hydrothermal method were incorporated into a chitosan matrix to fabricate organic-inorganic hybrid membranes. The strong hydrogen bond of surface -OH groups of TNTs with -OH or -NH_2 groups of chitosan chains facilitated the dispersion of TNTs, and rendered these hybrid membranes of lower methanol crossover and higher mechanical strength. Particularly, CS-TNTs-15 displayed the highest mechanical strength of 85.0 MPa, low methanol permeability of 0.497×10~(-6) cm2·s~(-1), and proton conductivity of 0.0151 S·cm~(-1), which had the potential for DMFC applications.
目前,有机-无机杂化膜通常以物理或化学方法制备,随着近年来社会对环境保护的日益关注,寻求绿色合成方法逐渐成为一项具有挑战性的工作。
本文制备了多种生物高分子-氧化钛杂化膜,发明了一种合成有机-无机杂化膜的纯生物方法,并探讨了这些杂化膜的初步应用。
有鉴于此,本文首次利用纯生物方法制备了细菌纤维素-TiO_2纳米杂化膜,为有机-无机杂化膜的绿色合成提供了一个很好的思路;探讨了作为无机填充物的氧化钛的形貌和结构对高分子-TiO_2杂化膜分离性能的影响,并探索了这些杂化膜的初步应用。
首先,以木醋杆菌为多功能微生物反应器,一步合成了细菌纤维素-TiO_2纳米杂化膜,并且对其形成机理和应用进行了初步研究,对制备材料进行了X射线衍射、X射线光电子能谱、扫描电子显微镜和投射电子显微镜等表征。通过向培养基中加入钛前驱体二(2-羟基丙酸)二氢氧化二铵合钛,合成了细菌纤维素-TiO_2纳米杂化膜。研究表明:细菌纤维素膜是由直径为60-120nm的纳米纤维构成的三维网状结构,TiO_2的引入未改变细菌纤维素的微观结构,生成的30-50nm的TiO_2颗粒主要镶嵌在细菌纤维素的网络中,含量可达到4wt%。木醋杆菌在合成细菌纤维素的同时,矿化钛前驱体生成TiO_2纳米颗粒,细胞壁/膜在TiO_2合成过程中起到了重要作用。类似的,通过向培养基中加入硅酸钠和硅酸,生物合成了细菌纤维素-SiO_2纳米杂化膜,表明这种生物方法具有一定的通用性。
其次,为了解决生物合成法中TiO_2纳米颗粒在杂化膜中含量较低的问题,利用原位合成法制备细菌纤维素-TiO_2纳米杂化膜。通过向培养基中加入水热法合成的TiO_2凝胶纳米颗粒,原位合成了细菌纤维素-TiO_2纳米杂化膜,TiO_2凝胶颗粒的加入对木醋杆菌的生长未产生影响。TiO_2的引入未改变细菌纤维素的微观结构,TiO_2主要包埋在细菌纤维素网络结构中,含量可达到7.1%。据推测,在细菌纤维素膜的合成过程中,悬浮在培养基中的氧化钛胶体颗粒被包裹其中,从而最终形成了杂化膜。
第三,为研究具有特殊形貌和结构TiO_2对纳米杂化膜性能的影响,将水热法制备的钛酸盐纳米管与生物高分子壳聚糖(CS)共混,制备了CS-TNTs纳米杂化膜,并研究了其作为直接甲醇燃料电池质子交换膜的性能。由于TNTs的表面羟基与壳聚糖高分子链段上的羟基和氨基形成氢键相互作用,使TNTs很好分散在CS基质中,提高了杂化膜的机械性能和热稳定性;TNTs引入降低了杂化膜的自由体积分数,有效降低了杂化膜的甲醇渗透性能。其中,含15wt%的TNTs的CS-TNTs纳米杂化膜的机械强度为85.0Mpa,甲醇渗透率为为0.497×10~(-6) cm~2/s,质子传导率为0.0151S cm~(-1),具有较好的应用前景。
Recently, it has been focused on the fabrication and application of organic-inorganic composite membranes, owing to its combining the advantages of traditional organic and inorganic membrane. TiO_2 has a high chemical stability, light corrosion and photocatalytic activity, strong scattering ability, absorption of UV light, and sterilization. When incorporated into Polymer matrix, TiO_2 can increase the thermal stability, mechanical strength and permeability of composite membrane. The characteristic properties of TiO_2 can be reflected in the hybrid membrane. Therefore, polymer-TiO_2 hybrid membranes have been attracted wide spread concern.
Currently, organic-inorganic hybrid membranes are usually prepared by physical or chemical methods. Green synthesis method is becoming a challenging task with the growing concern on environmental protection.
In this article, a pure biological method was used to one pot synthesizing bacterial cellulose-TiO_2 composite membrane at the first time. It provides a good green synthesis strategy. The effect of morphology and structure of TiO_2 on the separation property and the preliminary application of hybrid membranes were explored.
First, Acetobacter was used as a multi-reactor to one pot synthesizing bacterial cllulose(BC)-TiO_2 nanocomoposite. The formation mechanism and preliminary application of BC-TiO_2 nanocomposite are explored, and characterized by X-ray diffraction, X-ray Photoelectron Spectroscopy, scanning electron microscope, and transmission electron microscopy. BC-TiO_2 nanocomposite was fabricated by adding the precursor titanium(IV) bis(ammonium lactato) dihydroxide into the culture medium. The results show that three dimensional bacterial cellulose membrane is composed of 60-120nm cellulose fibril. The introduction of TiO_2 does not change the microstructure of the membrane. TiO_2 nanoparticles with size of 30-50nm are main embedded in the bacterial cellulose network, the content of it can reach 4wt%. Acetobacter synthesize bacterial cellulose and mineralize TiO_2 simultaneously. Cell wall/membrane plays an important role in the mineralization of TiO_2. Similarly, when sodium silicate or silicic acid added into the culture medium, BC-SiO_2 nanocomposite membranes were synthesized. It shows that the biological method has some versatility.
Secondly, in order to enhance the TiO_2 nanoparticles content in the BC-TiO_2 membrane, BC-TiO_2 nanocomposite membrane are fabricated by in situ method. The growth of Acetobacter is not affect by adding TiO_2 gel particles into the culture medium, and the microstructure of the nanocomposite membrane does not change. TiO_2 nanoparticles are mainly embedded in the bacterial cellulose network, the content of it can reach up to 7.1wt%. It is supposed that the suspended TiO_2 in the culture medium are wrapped into the network when the bacterial cellulose are synthesized, and finally formed a nanocomposite membrane.
Third, in order to study the impact of the morphology and structure on the properties of composite membrane, Titanate nanotubes(TNTs) with layered structure synthesized by the hydrothermal method were incorporated into a chitosan matrix to fabricate organic-inorganic hybrid membranes. The strong hydrogen bond of surface -OH groups of TNTs with -OH or -NH_2 groups of chitosan chains facilitated the dispersion of TNTs, and rendered these hybrid membranes of lower methanol crossover and higher mechanical strength. Particularly, CS-TNTs-15 displayed the highest mechanical strength of 85.0 MPa, low methanol permeability of 0.497×10~(-6) cm2·s~(-1), and proton conductivity of 0.0151 S·cm~(-1), which had the potential for DMFC applications.
引文
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