阻燃PVA/SiO_2复合纤维的制备与性能研究
摘要
利用湿法纺丝,将硅溶胶分散于PVA溶液中,制备阻燃PVA/SiO_2复合纤维,并研究无机颗粒与PVA的界面粘结状况,阻燃PVA/SiO_2复合纤维的纺丝过程、纤维的各种物理性能指标以及热稳定性、阻燃性。
分析了硅溶胶及PVA的结构特点对纺丝原液稳定性的影响,讨论了硅溶胶与PVA间的作用模式。通过对纺丝原液粘度及粘流活化能的分析,结果显示SiO_2的添加量、SiO_2和PVA间的相互作用力及温度共同决定着PVA/SiO_2混合液的粘度以及粘流活化能。并采用红外光谱方法及残留率、耐溶剂性能的测定,证明SiO_2与PVA能较好的反应复合。
利用红外光谱研究了缩醛化的反应模式,发现主要是分子间缩合。通过SEM、TEM观察无机粒子在纤维中的分散情况,结果表明SiO_2粒子在纤维中以小团聚体分散。并对阻燃PVA/SiO_2复合纤维的单纤维力学性质进行了分析,与PVA纤维相比,添加无机纳米粒子的阻燃PVA/SiO_2复合纤维的断裂强度提高,断裂伸长减小。
通过PVA纤维与阻燃PVA/SiO_2复合纤维的TG以及DTG分析比较,得出SiO_2的加入增强了PVA的热稳定性能。通过Kissinger、Ozawa、Friedman三种方法对纤维的热解活化能进行了研究,发现阻燃剂的加入在一定程度上改变了纤维素的热降解性能,减缓了热降解过程。利用对阻燃PVA/SiO_2复合纤维的燃烧过程以及燃烧时热量和质量损失进行了全面的研究,发现阻燃PVA/SiO_2复合纤维的热释放速率和质量损失均低于未阻燃纤维,说明SiO_2的加入能有效阻燃。利用红外光谱、SEM对纤维燃烧残余物进行分析,发现SiO_2粒子的加入促进了PVA的脱水炭化。
Colloidal silica was mixed with PVA solution in right proportion and made into flame retardant PVA/silica composite fibers by wet spinning. Linking state of the interface between inorganic particles and macromolecules was studied; the structure and the properties of flame retardant PVA/silica composite fibers were investigated, including spinning technics, mechanical properties of fibers, thermal stability and flame retardancy.
The influence on stability of spinning solution was analyzed by studying the structures of colloidal silica and PVA, and then the binding mode of silica and PVA was discussed. By analyzing viscosity and viscous flow activation energy of spinning solution, the results showed that: viscosity and viscous flow activation energy of spinning solution have relation with silica proportion, interaction of silica and PVA and temperature of solution. By FTIR, measuring residual rate and solvent resistance, a good reaction between PVA and colloidal silica could be concluded.
By FTIR, an intermolecular acetalization mode could be found. By observing the morphology of fibers by TEM and SEM, the results showed that silica can uniformly disperse into PVA at aggregate state, and have a better interface with PVA. At the same time, the results also showed that the breaking strength was increased and breaking elongation decreased compared with PVA fiber.
By analyzing burning residue of fibers, the results showed that: the adding of silica can promote dehydration and carbonization of PVA. Comparing with PVA fiber by TG and DTG, the results showed that the adding of silica reinforced thermal stability of flame retardant PVA/silica composite fibers. By analyzing pyrolysis activation evergy of fibers through Kissinger, Ozawa, Friedman method, the results showed that: in a certain extent, the adding of silica particles changed the thermal and reduced thermal degradation behaviors. An extensively research with burning process and its production of heat and mass loss of flame retardant PVA/silica composite fibers by CONE was done. The heat release rate and mass loss were greatly decreased compared with PVA fiber and the increased flame-retardance of PVA/silica composite fibers could be concluded.
分析了硅溶胶及PVA的结构特点对纺丝原液稳定性的影响,讨论了硅溶胶与PVA间的作用模式。通过对纺丝原液粘度及粘流活化能的分析,结果显示SiO_2的添加量、SiO_2和PVA间的相互作用力及温度共同决定着PVA/SiO_2混合液的粘度以及粘流活化能。并采用红外光谱方法及残留率、耐溶剂性能的测定,证明SiO_2与PVA能较好的反应复合。
利用红外光谱研究了缩醛化的反应模式,发现主要是分子间缩合。通过SEM、TEM观察无机粒子在纤维中的分散情况,结果表明SiO_2粒子在纤维中以小团聚体分散。并对阻燃PVA/SiO_2复合纤维的单纤维力学性质进行了分析,与PVA纤维相比,添加无机纳米粒子的阻燃PVA/SiO_2复合纤维的断裂强度提高,断裂伸长减小。
通过PVA纤维与阻燃PVA/SiO_2复合纤维的TG以及DTG分析比较,得出SiO_2的加入增强了PVA的热稳定性能。通过Kissinger、Ozawa、Friedman三种方法对纤维的热解活化能进行了研究,发现阻燃剂的加入在一定程度上改变了纤维素的热降解性能,减缓了热降解过程。利用对阻燃PVA/SiO_2复合纤维的燃烧过程以及燃烧时热量和质量损失进行了全面的研究,发现阻燃PVA/SiO_2复合纤维的热释放速率和质量损失均低于未阻燃纤维,说明SiO_2的加入能有效阻燃。利用红外光谱、SEM对纤维燃烧残余物进行分析,发现SiO_2粒子的加入促进了PVA的脱水炭化。
Colloidal silica was mixed with PVA solution in right proportion and made into flame retardant PVA/silica composite fibers by wet spinning. Linking state of the interface between inorganic particles and macromolecules was studied; the structure and the properties of flame retardant PVA/silica composite fibers were investigated, including spinning technics, mechanical properties of fibers, thermal stability and flame retardancy.
The influence on stability of spinning solution was analyzed by studying the structures of colloidal silica and PVA, and then the binding mode of silica and PVA was discussed. By analyzing viscosity and viscous flow activation energy of spinning solution, the results showed that: viscosity and viscous flow activation energy of spinning solution have relation with silica proportion, interaction of silica and PVA and temperature of solution. By FTIR, measuring residual rate and solvent resistance, a good reaction between PVA and colloidal silica could be concluded.
By FTIR, an intermolecular acetalization mode could be found. By observing the morphology of fibers by TEM and SEM, the results showed that silica can uniformly disperse into PVA at aggregate state, and have a better interface with PVA. At the same time, the results also showed that the breaking strength was increased and breaking elongation decreased compared with PVA fiber.
By analyzing burning residue of fibers, the results showed that: the adding of silica can promote dehydration and carbonization of PVA. Comparing with PVA fiber by TG and DTG, the results showed that the adding of silica reinforced thermal stability of flame retardant PVA/silica composite fibers. By analyzing pyrolysis activation evergy of fibers through Kissinger, Ozawa, Friedman method, the results showed that: in a certain extent, the adding of silica particles changed the thermal and reduced thermal degradation behaviors. An extensively research with burning process and its production of heat and mass loss of flame retardant PVA/silica composite fibers by CONE was done. The heat release rate and mass loss were greatly decreased compared with PVA fiber and the increased flame-retardance of PVA/silica composite fibers could be concluded.
引文
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