醋酸纤维素的改性及可控电纺的研究
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摘要
随着纳米科技的发展，纳米纤维材料因其尺寸效应显著，在电、磁、光、热等方面展现出众多新奇的特性，因而受到研究者们的关注。静电纺丝技术是制备直径分布在纳米至微米级超细纤维简单且有效的方法之一。与传统纺丝方法不同，静电纺丝借助于高压电场作用获得超细纤维，所得纤维具有较大的比表面积以及孔隙率。醋酸纤维素首次制备于1865年，是纤维素的乙酸酯。由于其对光稳定、易溶于有机溶剂，具有温和、安全、良好的稳定性和相容性，常作为纤维素替代材料应用于静电纺丝领域。然而，醋酸纤维素性能单一，应用范围受限，大规模工业化生产具有难度，仍需要进一步系统的研究。
本文采用静电纺丝技术，以醋酸纤维素为基体材料，分别将聚乙烯亚胺、聚苯胺、以及聚乳酸添加到CA中，制备了三个体系的改性CA复合纳米纤维。研究了体系中溶液浓度、聚合物组成、改性聚合物性能对改性CA纳米纤维的形貌、结构和性能的影响，主要分为以下四部分研究工作：
（1）选取丙酮与水作为共溶剂，制备了CA/PEI电纺纳米复合材料。研究结果表明随着PEI含量的增加，复合纤维直径逐渐增大，且出现了两种不同直径的纤维分布；利用扫描电镜与透射电镜观察水洗后电纺纤维的形貌，水洗后的CA纤维表面仍然为光滑的圆柱形结构；而复合纤维表面出现大量的凹陷与孔洞，内部产生中空结构。结合DSC、FTIR、XPS等数据分析了复合纤维中两组分的分布，即PEI含量较低时，由于PEI和CA的侧基的极性基团相互作用增强，PEI均匀分散在CA体系中，水洗后形成中空结构；PEI含量逐渐增大，其侧基基团随电场力增大表现为斥力增强，在CA/PEI体系中向外扩散至纤维表面。
（2）制备了具有导电性能的CA/PANI电纺纤维，并通过对电纺纤维定向机理的分析和有限元模拟方法，选取置于绝缘基板上相互平行的铜丝作为接收装置制备得到了具有宏观结构可控的纳米纤维。通过改变电纺条件得出：材料导电性增大，纤维排布有序度提高；在一定范围内提高铜丝间距可以提高纤维排布的有序度；PANI浓度增加，材料导电性增强，铜丝上纤维排布的有序度提高；添加HCSA可以提高PANI在CA/PANI溶液中的溶解度，材料导电性增强，纤维排布的有序度提高。
（3）以氯仿和丙酮作为溶剂，制备了单组份左旋聚乳酸（PLLA）电纺纤维，通过提高溶液浓度能够有效的减少串珠结构，获得直径可控的超细纤维。引入CA组分后，复合纤维直径增大并伴有两相纤维产生，提高CA的含量，复合纤维直径呈递减趋势。DSC、XRD测试表明，两组分具有良好的相容性，CA组分是影响纤维焓变的主要因素。力学性能测试结果表明，复合纤维拉伸性能较纯CA纤维有所提高，两相纤维对于力学性能产生了有利的影响。此外，接触角测试表明，加入CA组分后，电纺纤维的亲水性能得到了显著提高。
（4）基于第三部分的研究工作，选取CA/PLLA及PLLA作为基体材料，绑定生物素后通过电纺丝制备生物传感器界面，并利用生物素/链霉亲和素之间快速特异的结合作用，将蛋白质固载于纤维膜表面以达到探测蛋白的目的。结合SEM、XRD、比色实验、以及酶联免疫吸附试验对比发现，CA组分的引入能够使复合纤维产生多孔的微观结构，进一步提高基体材料中的生物素与蛋白接触的面积，提高生物传感器的灵敏性及有效性。
With the development of nanotechnology, nano-fiber material exhibited many novelfeatures in the fields of electricity, magnetism, light, heat, for which received extensiveattention of the researchers. Electrospinning was a simple and effective method to preparefibers with nano-and micro-diameter distribution. Cellulose acetate was first prepared in1865, and it was stable in light, soluble in organic solvents, and had good compatibility. CAis commonly used as the substrate material in the electrospinning. However, CA had lowoxidation and chemical affinity which limited its further applications. Therefore,modification of CA have become a commercially viable approach to produce new materialswith improved properties.
In this dissertation, CA was modified by polyethyleneimine (PEI), polyaniline (PANI),and poly (lactic acid)(PLLA) respectively through electrospinning. CA composite fiberswere characterized by SEM, TEM, DSC, XPS, etc. In addition, the influences of the polymerconcentration, electrospinning condition and polymer properties on CA fibers were studiedsystematically. This thesis consisted of the following four parts:
(1) CA/PEI electrospun nanofibers were successfully fabricated by electrospinning.Acetone and water was chosen as the co-solvent. SEM and TEM images showed thatelectrospun CA fibers after water-treated remained smooth surface and cylindrical shape,while eletrospun CA/PEI fibers had a large number of recesses and holes on the surface, andhollow structure in the interior. DSC, FTIR and XPS data proved the distribution of the twocontents. When PEI content was low, the enhanced interaction from the polar groups of CAand PEI led to even distribution of PEI in the CA/PEI system. And then hollow structure wasobtained after water treated. When PEI content increased gradually, the repulsive forcebetween the side group enhanced with the increasing of electric force. PEI content diffusedoutward to the surface of the composite fibers.
(2) Based on the simulation of finite element and the analysis of the electrospun fibersorientation mechanism, the controllable CA/PANI nanofibers were fabricated successfully.The parallel copper wires on the insulated substrate were used as the collector. Theexperimental results were shown as followed. With the conductivity increased, the orderedarrangement of the electrospun fibers enhanced. Improving the distance between the two copper wires with a certain range, the order degree of the fibers increased. Whenconcentration of PANI increased, the conductivity of the fibers enhanced. And the fibersposited on the coppers had a better orientation. Besides, HCSA could increase the solubilityof the PANI in the CA/PANI solution effectively. Thus, fiber conductivity reinforced andordered orientation of the fibers raised.
(3) Poly(L-lactic) acid (PLLA) nanofiber was prepared successfully by electrospinningusing chloroform and acetone as the solvent. Increasing the concentration of the PLLA couldeffectively reduce the beaded structure to obtain controllable diameter of the fibers.CA/PLLA mixtures of different compositions were successfully electrospun to obtaincomposite nanofibrous membranes. The microstructures of the membranes changed fromhomogeneous to heterogeneous with the addition of CA, which was observed by FE-SEM.The CA/PLLA fabric membranes were characterized by mechanical testing, DSC andcontact angle measurements. The tensile stress of the composite fibrous membranesincreased obviously with the increase of CA content. DSC results indicated that the CAcomponent was the main factor for the changes of enthalpies in the composite fibers. Contactangle measurements showed the hydrophilicity of the electrospun nanofiber membranes wasimproved with.
(4) PLLA and CA/PLLA fiber membranes were prepared as biosensor substrate. Biotinwas added into PLLA and CA/PLLA fibers successfully. By using of the rapid and specificbinding between the biotin/streptavidin, the protein was immobilized on the surface of thefiber membrane and detected. SEM, XRD, colorimetric assay and enzyme linkedimmunosorbnent assay (ELISA) were used to characterize the capability of PLLA/biotin andCA/PLLA/biotin fibers binding streptavidin. The results showed that the introduction of CAcomponent enabled composite fibers to produce micro-porous structure, and furtherimproved the effect of the substrate material binding biotin, and finally improve thesensitivity and effectiveness of the biosensor.
本文采用静电纺丝技术，以醋酸纤维素为基体材料，分别将聚乙烯亚胺、聚苯胺、以及聚乳酸添加到CA中，制备了三个体系的改性CA复合纳米纤维。研究了体系中溶液浓度、聚合物组成、改性聚合物性能对改性CA纳米纤维的形貌、结构和性能的影响，主要分为以下四部分研究工作：
（1）选取丙酮与水作为共溶剂，制备了CA/PEI电纺纳米复合材料。研究结果表明随着PEI含量的增加，复合纤维直径逐渐增大，且出现了两种不同直径的纤维分布；利用扫描电镜与透射电镜观察水洗后电纺纤维的形貌，水洗后的CA纤维表面仍然为光滑的圆柱形结构；而复合纤维表面出现大量的凹陷与孔洞，内部产生中空结构。结合DSC、FTIR、XPS等数据分析了复合纤维中两组分的分布，即PEI含量较低时，由于PEI和CA的侧基的极性基团相互作用增强，PEI均匀分散在CA体系中，水洗后形成中空结构；PEI含量逐渐增大，其侧基基团随电场力增大表现为斥力增强，在CA/PEI体系中向外扩散至纤维表面。
（2）制备了具有导电性能的CA/PANI电纺纤维，并通过对电纺纤维定向机理的分析和有限元模拟方法，选取置于绝缘基板上相互平行的铜丝作为接收装置制备得到了具有宏观结构可控的纳米纤维。通过改变电纺条件得出：材料导电性增大，纤维排布有序度提高；在一定范围内提高铜丝间距可以提高纤维排布的有序度；PANI浓度增加，材料导电性增强，铜丝上纤维排布的有序度提高；添加HCSA可以提高PANI在CA/PANI溶液中的溶解度，材料导电性增强，纤维排布的有序度提高。
（3）以氯仿和丙酮作为溶剂，制备了单组份左旋聚乳酸（PLLA）电纺纤维，通过提高溶液浓度能够有效的减少串珠结构，获得直径可控的超细纤维。引入CA组分后，复合纤维直径增大并伴有两相纤维产生，提高CA的含量，复合纤维直径呈递减趋势。DSC、XRD测试表明，两组分具有良好的相容性，CA组分是影响纤维焓变的主要因素。力学性能测试结果表明，复合纤维拉伸性能较纯CA纤维有所提高，两相纤维对于力学性能产生了有利的影响。此外，接触角测试表明，加入CA组分后，电纺纤维的亲水性能得到了显著提高。
（4）基于第三部分的研究工作，选取CA/PLLA及PLLA作为基体材料，绑定生物素后通过电纺丝制备生物传感器界面，并利用生物素/链霉亲和素之间快速特异的结合作用，将蛋白质固载于纤维膜表面以达到探测蛋白的目的。结合SEM、XRD、比色实验、以及酶联免疫吸附试验对比发现，CA组分的引入能够使复合纤维产生多孔的微观结构，进一步提高基体材料中的生物素与蛋白接触的面积，提高生物传感器的灵敏性及有效性。
With the development of nanotechnology, nano-fiber material exhibited many novelfeatures in the fields of electricity, magnetism, light, heat, for which received extensiveattention of the researchers. Electrospinning was a simple and effective method to preparefibers with nano-and micro-diameter distribution. Cellulose acetate was first prepared in1865, and it was stable in light, soluble in organic solvents, and had good compatibility. CAis commonly used as the substrate material in the electrospinning. However, CA had lowoxidation and chemical affinity which limited its further applications. Therefore,modification of CA have become a commercially viable approach to produce new materialswith improved properties.
In this dissertation, CA was modified by polyethyleneimine (PEI), polyaniline (PANI),and poly (lactic acid)(PLLA) respectively through electrospinning. CA composite fiberswere characterized by SEM, TEM, DSC, XPS, etc. In addition, the influences of the polymerconcentration, electrospinning condition and polymer properties on CA fibers were studiedsystematically. This thesis consisted of the following four parts:
(1) CA/PEI electrospun nanofibers were successfully fabricated by electrospinning.Acetone and water was chosen as the co-solvent. SEM and TEM images showed thatelectrospun CA fibers after water-treated remained smooth surface and cylindrical shape,while eletrospun CA/PEI fibers had a large number of recesses and holes on the surface, andhollow structure in the interior. DSC, FTIR and XPS data proved the distribution of the twocontents. When PEI content was low, the enhanced interaction from the polar groups of CAand PEI led to even distribution of PEI in the CA/PEI system. And then hollow structure wasobtained after water treated. When PEI content increased gradually, the repulsive forcebetween the side group enhanced with the increasing of electric force. PEI content diffusedoutward to the surface of the composite fibers.
(2) Based on the simulation of finite element and the analysis of the electrospun fibersorientation mechanism, the controllable CA/PANI nanofibers were fabricated successfully.The parallel copper wires on the insulated substrate were used as the collector. Theexperimental results were shown as followed. With the conductivity increased, the orderedarrangement of the electrospun fibers enhanced. Improving the distance between the two copper wires with a certain range, the order degree of the fibers increased. Whenconcentration of PANI increased, the conductivity of the fibers enhanced. And the fibersposited on the coppers had a better orientation. Besides, HCSA could increase the solubilityof the PANI in the CA/PANI solution effectively. Thus, fiber conductivity reinforced andordered orientation of the fibers raised.
(3) Poly(L-lactic) acid (PLLA) nanofiber was prepared successfully by electrospinningusing chloroform and acetone as the solvent. Increasing the concentration of the PLLA couldeffectively reduce the beaded structure to obtain controllable diameter of the fibers.CA/PLLA mixtures of different compositions were successfully electrospun to obtaincomposite nanofibrous membranes. The microstructures of the membranes changed fromhomogeneous to heterogeneous with the addition of CA, which was observed by FE-SEM.The CA/PLLA fabric membranes were characterized by mechanical testing, DSC andcontact angle measurements. The tensile stress of the composite fibrous membranesincreased obviously with the increase of CA content. DSC results indicated that the CAcomponent was the main factor for the changes of enthalpies in the composite fibers. Contactangle measurements showed the hydrophilicity of the electrospun nanofiber membranes wasimproved with.
(4) PLLA and CA/PLLA fiber membranes were prepared as biosensor substrate. Biotinwas added into PLLA and CA/PLLA fibers successfully. By using of the rapid and specificbinding between the biotin/streptavidin, the protein was immobilized on the surface of thefiber membrane and detected. SEM, XRD, colorimetric assay and enzyme linkedimmunosorbnent assay (ELISA) were used to characterize the capability of PLLA/biotin andCA/PLLA/biotin fibers binding streptavidin. The results showed that the introduction of CAcomponent enabled composite fibers to produce micro-porous structure, and furtherimproved the effect of the substrate material binding biotin, and finally improve thesensitivity and effectiveness of the biosensor.
引文
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