Macedo Thaís R, Airoldi Claudio
Institute of Chemistry, University of Campinas, P.O. Box 6154, 13084-971, Campinas, Sao Paulo, Brasil.
Dalton Trans. 2009 Sep 28(36):7402-9. doi: 10.1039/b908857a. Epub 2009 Jul 17.
Two distinct methods to graft the silylating agent 3-cyanopropyltriclorosilane (CN) in the interlayer space of the layered silicate Na-RUB-18, with composition Na2Si8O17.nH2O, are described. The organosilylation was carried out by reflux and solvent evaporation methodologies, using the intercalated surfactant cetyltrimethylammonium after sodium exchange as one intermediate (CTA-RUB-18) and the acidic form (H-RUB-18) as the other intermediate. The resulting silylated derivatives obtained by both methods possessed basal spacings of 1.19 and 1.54 nm, and 1.26 and 1.16 nm, starting from CTA-RUB-18 and H-RUB-18, with the reflux and solvent evaporation methods, respectively. A favourable condition for this immobilization methodology is the use of small amounts of the silylating agent, with six times less than the previous procedure. The maximum amount of the silane attached to the RUB-18 surface, based on analytical results considering the nitrogen content, gave the values 5.64, 4.16, 4.37 and 4.05 mmol g(-1), respectively. All preparation processes were followed by elemental analyses and X-ray diffraction and the organofunctionalizations were confirmed through chemical and thermogravimetric data. The presence of pendant chains covalently bonded to the inorganic RUB-18 layers was confirmed by 13C and 29Si NMR spectroscopy. The inorganic-organic hybrids have the ability for divalent cation removal from aqueous solutions at the solid/liquid interface. The series of adsorption isotherms were favourably adjusted to the Freundlich equation, demonstrating the applicability of these synthesized chemically modified layered materials.
本文描述了两种将硅烷化试剂3-氰基丙基三氯硅烷(CN)接枝到层状硅酸盐Na-RUB-18(组成为Na2Si8O17·nH2O)层间空间的不同方法。有机硅烷化反应通过回流和溶剂蒸发方法进行,使用钠交换后的插层表面活性剂十六烷基三甲基铵(CTA-RUB-18)作为一种中间体,酸性形式(H-RUB-18)作为另一种中间体。通过这两种方法得到的硅烷化衍生物,从CTA-RUB-18和H-RUB-18出发,分别采用回流法和溶剂蒸发法,其层间距分别为1.19和1.54 nm,以及1.26和1.16 nm。这种固定化方法的一个有利条件是使用少量的硅烷化试剂,其用量比以前的方法少六倍。基于考虑氮含量的分析结果,附着在RUB-18表面的硅烷的最大量分别为5.64、4.16、4.37和4.05 mmol g(-1)。所有制备过程均通过元素分析和X射线衍射进行跟踪,并通过化学和热重数据确认有机官能化。通过13C和29Si NMR光谱证实了与无机RUB-18层共价键合的侧链的存在。无机-有机杂化物具有在固/液界面从水溶液中去除二价阳离子的能力。一系列吸附等温线能很好地拟合Freundlich方程,证明了这些合成的化学改性层状材料的适用性。