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Preparation and Application of Ion Exchange Resin Loaded with p-t-Butylcalix[8]arene

对叔丁基杯[8]芳烃负载离子交换树脂的制备及应用

基本信息

批准号：
16550087
负责人：
YOSHIDA Isao
金额：
$ 1.02万
依托单位：
Sojo University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2004
资助国家：
日本
起止时间：
2004 至 2005
项目状态：
已结题

项目摘要

The silica gel particles and ion exchange resins loaded with p-t-butylcalix[n]arene, BC_n (n=4,6,8) were prepared and their adsorption properties were investigated for several small molecules including fullerene C_<60> in the present study. The silica gel particles with attached BC_n were prepared by allowing BC_n to react with 3-glycidoxypropyltrimethoxysilane in dry toluene to form phenyl ether in the presence of small amounts of perchloric acid. The resulting phenyl ether was linked by a methanolsis reaction to the silica gel particles then the particles were treated with water to give BC_n-Si by changing the silyl methoxy group to the hydroxyl group. The ion exchange resins loaded with p-t-butylcalix[n]arene-3-sulfopropylether, BC_n-PS_n, were prepared by allowing BC_n to react with 3-bromopropanesulfonic acid sodium salt in the presence of sodium hydride and potassium iodide, first, the resulting ether derivative of BC_n was then loaded on the ion exchange resins AGMP-1 by an anion exchange reaction. The adsorption properties of BC_n-Si and BC_n-PS_n were examined for three kinds of stilbene cationic dyes, four kinds of condensed aromatics and fullerene C_<60> and found that BC_n-Si has characteristic adsorption properties due to the molecular cavity of BC_n in the adsorption of the series of cationic dyes. Their adsorption ability for C_<60>, however, was small and can not be found any characteristic nature due to the presence of BC_n. This result was estimated to be from the "alternate" steric structures of BC_n in which some of the t-butyl groups are located on opposing site to make the catch up of C_<60> impossible. It is considered that the control of the steric structure of BC_n must be necessary in order to prepare the characteristic and strong adsorbents.

制备了负载对叔丁基杯[n]芳烃（BC_n，n= 4，6，8）的硅胶颗粒和离子交换树脂，研究了它们对富勒烯C_2等小分子的吸附性能<60>。在少量高氯酸存在下，BC_n与3-环氧丙氧丙基三甲氧基硅烷在无水甲苯中反应生成苯醚，制得了表面附着BC_n的硅胶颗粒。将所得的苯基醚通过甲醇化反应连接到硅胶颗粒上，然后将颗粒用水处理，通过将甲硅烷基甲氧基基团变为羟基基团而得到BC_n-Si。以对叔丁基杯[n]芳烃-3-磺丙基醚（BC_n）为载体，在氢化钠和碘化钾存在下与3-溴丙磺酸钠反应，得到BC_n的醚衍生物，再通过阴离子交换反应将其负载到AGMP-1上，制得BC_n-PS_n离子交换树脂。考察了BC_n-Si和BC_n-PS_n对3种二苯乙烯类阳离子染料、4种稠环芳烃和富勒烯C_2的吸附性能，<60>发现BC_n-Si对该系列阳离子染料具有特征吸附性能，这是由于BC_n的分子空穴结构所致。但它们对C_的吸附能力<60>很小，且由于BC_n的存在而没有表现出任何特征性。这可能是由于BC_n的“交替”空间结构，即某些叔丁基位于相对位置，使C_n不可能被赶上<60>。认为要制备性能优良的吸附剂，必须控制BC_n的空间结构。