TS-1 沸石合成过程中模板剂用量对钛进入骨架的影响

Effect of different amount of TPABr on incorporation of titanium into framework during synthesis of TS 1

以ＴＰＡＢｒ为模板剂、ＮＨ３·Ｈ２Ｏ为碱源，水热条件下合成了ＴＳ－１沸石（ＭＦＩ结构），采用ＸＲＤ、ＩＲ、ＵＶ－Ｖｉｓ、２９ＳｉＣＰＭＡＳＮＭＲ、２７ＡｌＣＰＭＡＳＮＭＲ、１３ＣＣＰＭＡＳＮＭＲ等表征手段详细研究了模板剂不同用量对钛进入骨架的影响．结果表明：随模板剂用量的增加，沸石中非骨架钛量（缩聚的六配位钛物种）减少（ＵＶ－Ｖｉｓ），当ＴＰＡＢｒ／ＳｉＯ２增加到０．４时，仍有非骨架钛物种存在，而酸洗可以除去大部分非骨架钛物种．当ＴＰＡＢｒ／ＳｉＯ２＝０．０２５时，ＴＳ－１沸石的结晶度低且进入骨架的钛量减少（ＩＲ，ＸＲＤ），所有样品的ＮＭＲ谱图几乎没有变化．

TS 1 was synthesized in the hydrothermal condition using TPABr as templating agent and NH 3·H 2O as base resource. The effect of different amounts of TPABr on the incorporation of titanium into the framework was studied by adopting IR, XRD, UV Vis, 29 Si CP MAS NMR, 27 Al CP MAS NMR and 13 C CP MAS NMR techniques. The results of UV Vis spectra show that the increase in the amount of TPABr results in the decrease in the extraframework titanium, acid washing could remove most of the extraframework titanium. IR and XRD results show that, when TPA +/SiO 2 is more than or equal to 0.025, the crystallinity is very low and the amount of titanium into the framework decrease. The difference in the NMR spectra ( 29 Si, 27 Al and 13 C) of TS 1 synthesized with different TPABr content was not detected. Therefore the amount of TPABr is enough during the synthesis of TS 1 when TPA +/SiO 2 is equal to 0.050.