Synthesis of MFI titanosilicates from methylamine—TPABr media

Masashi Shibata, Zelimir Gabelica
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引用次数: 19

Abstract

A new synthesis route for MFI-type titanosilicates (TS-1) using methylamine along with tetrapropylammonium bromide (TPABr), silica or silicon tetrachloride and titanium tetrachloride, thus avoiding the use of costly TPAOH and Ti-alkoxide, has been investigated. The presence of titanium ions in the reaction gel slowed down the crystallization of MFI zeolites, while addition of hydrogen fluoride as a co-mineralizer into the gel dramatically improved the crystallization kinetics. Ti was readily incorporated into the zeolite framework, as confirmed by IR, XRD (unit cell expansion), and UV-vis spectroscopy. Reduced initial amounts of methylamine in the gel led to an increase of the apparent crystallization rate of the zeolite and to a remarkable decrease of the amount of framework Ti, suggesting that high concentration of methylamine is needed for the Ti incorporation into the growing MFI crystallites.

甲胺- tpabr介质合成MFI钛硅酸盐
研究了以甲胺和四丙基溴化铵(TPABr)、二氧化硅或四氯化硅和四氯化钛为原料合成mfi型钛酸盐(TS-1)的新路线,从而避免了昂贵的TPAOH和醇钛的使用。反应凝胶中钛离子的存在减慢了MFI沸石的结晶速度,而在凝胶中加入氟化氢作为助矿剂显著改善了结晶动力学。通过IR, XRD(单位细胞膨胀)和UV-vis光谱证实,Ti很容易被纳入沸石骨架中。凝胶中初始甲基胺含量的降低导致沸石表观结晶速率的增加,同时导致骨架Ti含量的显著降低,这表明在生长的MFI晶体中,Ti的掺入需要高浓度的甲基胺。
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