导　　师： 党鸿辛;张治军

学科专业： 070305

授予学位： 博士

作　　者： ;

机构地区： 河南大学

摘　　要： γ-氨丙基三乙氧基硅烷/(APS/)表面修饰的纳米二氧化硅/(AMNS/)和γ-/(2,3-环氧丙氧基/)丙基三甲氧基硅烷/(GPS/)表面修饰的纳米二氧化硅/(GMNS/)作为催化剂和新材料在生命科学、分析化学、光学等领域具有广阔的应用前景。目前其相关的制备技术研究正步入全面的工艺完善阶段,应用研究也已经开始受到关注。然而,目前针对AMNS和GMNS的应用研究大多还处于经验探索阶段,其主要原因是对AMNS和GMNS表面的功能团/(即氨基和环氧基/)的存在浓度及形态缺乏了解,其中功能团的浓度影响是最主要的因素。另外,针对AMNS的应用开发研究亟需进行。据此,本论文主要从三个方面开展相关研究: 一、AMNS表面氨基浓度的测定 分别建立了盐酸-乙醇非水滴定法、高氯酸-冰乙酸非水滴定法、分光光度法、循环伏安法/(对氨基苯甲酸化学修饰电极法/)和凯氏定氮法等测定AMNS表面氨基浓度的方法;系统地研究了各种实验条件对测定结果的影响,探讨了影响测定结果准确度的主要因素;讨论了不同分析方法的优缺点以及导致其测量结果出现差异的主要原因;为该类纳米材料的合成和应用研究建立了分析测试平台。结果表明:所建立的各种分析方法均能用于对AMNS表面氨基进行比较准确的测定。在两种滴定分析法中,在滴定终点附近对样品进行超声振荡处理,有利于缩短滴定过程;在高氯酸-冰乙酸非水滴定法中加入异辛醇作为分散剂,可以改善体系的互溶性,降低体系的冰点,拓宽体系的应用范围;分光光度法灵敏度高,pH值是影响其测定结果的重要因素;化学修饰电极法较好地避免了纳米颗粒的吸附和光反射等对测定结果的影响,使测定结果更加准确;凯氏定氮法相应的测量结果较高,其原因在于采用凯氏定氮法测定的是AMNS中的总氮,而采用其他分析方法测定的是AMNS中氨基氮。 二、 As a kind of catalyst and novel functional materials, surface-modified nanosilica withγ-aminopropyltriethoxysilane /(APS/) andγ-glycidoxypropyltrimethoxysilane /(GPS/), coded as AMNS and GMNS, have been widely applied in the fields of life science, analytical chemistry and optics etc. At present, focus is being placed on modifying and integrating processes in terms of the preparation technology for AMNS and GMNS. And researches on the application of AMNS and GMNS are also begining to attract attention. However, current studies in relation to the applications of AMNS and GMNS are largely limited to exploration of experiences in labs, mainly due to insufficient understanding of the states and concentrations of the functional groups /(i.e., amino and epoxy groups/) on the surface of AMNS and GMNS, where the concentrations of the functional groups play a more critical role on the application. Besides, efforts are urgently needed to promote the application and development of AMNS in engineering. Therefore, the following three parts of research are to be highlighted in this dissertation: Part I: Determination of Amino Concentration on AMNS Methods such as hydrochloric acid-ethanol non-aqueous titration, perchloric acid-acetic acid non-aqueous titration, spectrophotometry and cyclic voltammetry /(using glassy carbon electrode modified with p-aminobenzoic acid/) were established for determining amino group on AMNS. The effects of various experimental conditions on the results of measurement were studied in detail. The main factors that affect the accuracy of measurement were investigated. The advantages and disadvantages of each method are discussed, and the main causes leading to differences from the measurement results by various methods are explored. Based on the above-mentioned studies, the analysis and test platforms have been established in relation to the synthesis and application of this type of nanomaterials. Results indicate that all the proposed methods could be well used to determine the amino con

关 键 词： 表面修饰纳米二氧化硅 氨基 环氧基 测定 尼龙 纳米复合材料

领　　域： [一般工业技术]