CALCINATION AND DEBORONATION OF [B]-MFI SINGLE-CRYSTALS

CALCINATION AND DEBORONATION OF [B]-MFI SINGLE-CRYSTALS
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DOI:
10.1016/0144-2449(93)90072-b
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发表时间:
1993-02-01
期刊:
ZEOLITES
影响因子:
--
通讯作者:
VANBEKKUM, H
VANBEKKUM, H
中科院分区:
其他
文献类型:
--
作者:
DERUITER, R;KENTGENS, APM;VANBEKKUM, H

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采用变温FTI. r研究了[B]-MFI的煅烧、脱硼及脱硼后MFI的硅醇巢再占据。光谱、X射线衍射和H-1、B-11和Si-29 MAS n.m.r.光谱技术。通过使用改进的煅烧程序使煅烧[B]-MFI时从骨架的硼损失最小化,在此过程中,硼保持在稳定的四面体/饱和配位中,并且避免了硼水解和萃取以及T原子重组。骨架硼可以通过在盐酸水溶液(pH小于或等于5)中浸泡从煅烧的硼MFI材料中提取,留下热稳定的(高达400 ℃,N2)均匀分布的硅烷醇巢,其是用于合成后再占据的有用的反应性位点。
Calcination and deboronation of [B]-MFI and silanol nest reoccupation of deboronated MFI were studied by variable temperature FTi.r. spectroscopy, X-ray diffraction, and H-1, B-11, and Si-29 MAS n.m.r. spectroscopy techniques. Boron loss from the framework upon calcining [B]-MFI was minimized by using an improved calcination procedure, during which boron is kept in a stable tetrahedral/saturated coordination and boron hydrolysis and extraction as well as T-atom reorganizations are avoided. Framework boron can be extracted from the calcined boron MFI material by refluxing in aqueous hydrochloric acid (pH less-than-or-equal-to 5), leaving thermally stable (up to 400-degrees-C, N2) homogeneously distributed silanol nests, which are useful reactive sites for postsynthesis reoccupation.