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单分散棒状MCM-41的制备及其对酚醛树脂改性的研究
其他题名Synthesis of monodispersed rod-like MCM-41 and its modification to PF
李明天
学位类型硕士
导师张劲松
2006-11-21
学位授予单位中国科学院金属研究所
学位授予地点金属研究所
学位专业材料加工工程
关键词介孔mcm-41 酚醛树脂 纳米复合材料 耐热性
摘要本论文在温和碱性条件下,以正硅酸乙酯为硅源,以十六烷基三甲基溴化胺为模板剂,以非离子表面活性剂平平加Os-25为助剂,于开放体系中成功地合成了分散性好并具有短棒状形貌的介孔氧化硅材料,同时在实验中考察了模板剂用量、助剂用量、碱量、溶剂水用量、温度、搅拌速度等多种因素对产品分散性和形貌的影响。结果表明,产物的形貌与分散性与上述各合成参数密切相关,加入适量的Os-25助剂,不但可以显著改善产物的分散性,而且可有效提高产物孔道排列的有序性。在优化工艺条件下合成的产物具有较高的比表面积和六方排列有序的介孔孔道,孔向基本平行于短棒状颗粒的长轴方向,而且孔径分布均匀。 本论文还采取共混、原位聚合以及两种工艺结合使用等不同方法制备了PF/MCM-41复合材料,结合IR、SEM、空气气氛和氮气气氛下的TG及XRD等手段,研究了纳米介孔氧化硅作为耐高温树脂基材料改性剂对材料性能的影响。结果表明,单独使用共混工艺时,MCM-41无法改善酚醛树脂基体的耐热性。如果预先使用偶联剂并借助超临界流体技术对MCM-41粉体改性,则共混制备的复合材料的耐热性可得到明显提高。采用原位聚合结合共混工艺制备的复合材料的耐热性有显著的提高。 导致纳米复合材料性能差异的原因在于树脂分子是否被引入到介孔氧化硅粉体的孔道中。MCM-41具有的纳米级孔道,有效限制了其内有机高分子链的自由运动,同时,其纳米级厚度的孔壁具有优良的耐热性及阻隔性,在快速升温的情况下延缓了孔道内树脂分子的热分解及分解产生的小分子的释放,这些都表现在酚醛树脂耐热性得到了明显提高。
其他摘要In this thesis, rod-like mesoporous silica MCM-41 was synthesized by using tetraethylorthosilicate (TEOS) as silicon source,the cationic surfactant cetyltrimeth- ylamonium bromide (CTAB) as template and nonionic surfactant Os-25 as co-template. The effects of the content of surfactant, co-template,and ammonia, the stir speed and the temperature on the dispersion ability and morphology of mesoporous silica were investigated. The results indicated that the dispersion ability and morphology of mesoporous silica depended tightly on the parameters mentioned above. The addition of Os-25 with a proper amount could not only improve the dispersion ability, but also the orientation of pores. High quality MCM-41 with a large specific surface area and highly ordered, uniform hexagonal pores parallel to the axis of the silica rods was obtained under the optimized synthesis conditions. Mesoporous silica filled Phenol formaldehyde resin(PF)composites (PF/MCM-41) were prepared by co-blending (CB), in-situ polymerization (ISP) and in-situ polymerization combined with co-blending (ISP-CB). The effects of MCM-41 on the heat-resistance of PF polymer were studied by use of IR, SEM, TG and XRD techniques. The results indicated that the heat resistance of the composites prepared by ISP and ISP-CB methods were improved remarkably. The mechnism of improvement in heat-resistance of PF/MCM-41 composites was attributed to the infiltration of PF polymer into the pores of silica rods. The nanochannels of MCM-41 confined the movement of polymer chains inside them effectively. Meanwhile, the nano-scaled hole walls with lower thermal conductivity delayed the pyrolysis process of PF and restrained the release of the pyrolysate. As a result, the thermal stability of PF was improved obviously, especially during rapid heating of the composites.
页数61
语种中文
文献类型学位论文
条目标识符http://ir.imr.ac.cn/handle/321006/16870
专题中国科学院金属研究所
推荐引用方式
GB/T 7714
李明天. 单分散棒状MCM-41的制备及其对酚醛树脂改性的研究[D]. 金属研究所. 中国科学院金属研究所,2006.
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