Usefulness of alkoxyltitanosiloxane for the preparation of mesoporous silica containing a large amount of isolated titanium.
Usefulness of alkoxyltitanosiloxane for the preparation of mesoporous silica containing a large amount of isolated titanium.
复制标题
烷氧基钛硅氧烷在制备含有大量分离钛的介孔二氧化硅中的用途。
DOI：
10.1016/j.jcis.2011.03.016
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发表时间：
2011
影响因子：
9.9
通讯作者：
K. Kuroda
中科院分区：
文献类型：
--
作者：
Kwang;Ryutaro Wakabayashi;T. Tatsumi;T. Yokoi;K. Kuroda
以烷氧钛硅氧烷为前驱体，采用硬模板法制备了含有大量分离Ti的介孔二氧化硅。合成了异丙氧基（三叔丁基硅氧基）钛((iPrO)Ti[OSi(OtBu)3]3, TS3)，并将TS3与硬模板介孔碳（CMK-3）混合。将混合物在180℃下热解，形成二氧化钛和硬模板组成的复合材料。在600℃下煅烧去除碳模板后，通过DR-UV-Vis、FTIR、XPS、XRD等测试证明钛种没有转化为锐钛矿型TiO2，而ESR结果表明钛分离存在。通过SEM、TEM和n2吸附对其介孔结构进行了表征。产物的Si/Ti比与前驱体的Si/Ti比基本一致。结果表明，该前驱体制备的材料为有序介孔二氧化硅，其骨架中含有大量分离Ti。使用定义明确的烷氧钛硅氧烷前驱体可以形成具有精确控制钛组成的介孔二氧化硅，既不会损失钛也不会转变为锐钛矿。
Mesoporous silica containing a large amount of isolated Ti was prepared from an alkoxytitanosiloxane precursor through a hard template method. Isopropoxytris(tris-tert-butoxysiloxy)titanium ((iPrO)Ti[OSi(OtBu)3]3, TS3) was synthesized and TS3 was mixed with mesoporous carbon (CMK-3), a hard template. The mixture was pyrolyzed at 180 °C to form a composite consisting of titanosilica and the hard template. After calcination at 600 °C for the removal of the carbon template, the titanium species were not transformed to anatase TiO2, proved by DR-UV–Vis, FTIR, XPS, and XRD, while the ESR results indicated the presence of isolated Ti. The mesoporous structure was verified by SEM, TEM, and N2adsorption. The Si/Ti ratio of the product was consistent with that of the precursor. All the results show that the material prepared from the precursor is ordered mesoporous silica containing a large amount of isolated Ti in the frameworks. The use of well-defined alkoxytitanosiloxane precursor leads to the formation of mesoporous silica with exactly controlled composition of titanium with neither loss of Ti nor transformation to anatase.