固体核磁共振技术在锡硅分子筛表征中的应用

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肖瑶^1,²,夏长久³,易先锋^1,*(

),刘凤庆^1,²,刘尚斌⁴,郑安民^1,*(

)

Progress in the Studies on Sn-Zeolites by Solid-State Nuclear Magnetic Resonance

Yao XIAO^1,²,Chang-jiu XIA³,Xian-feng YI^1,*(

),Feng-qing LIU^1,²,Shang-bin LIU⁴,An-min ZHENG^1,*(

)

图1. (A) 不同处理条件下，Sn-Beta分子筛的¹¹⁹Sn MAS NMR谱图：(a)煅烧；(b)煅烧后脱水；(c)煅烧脱水后再水合.(B)脱水Sn-Beta分子筛的(a) ¹¹⁹Sn MAS与(b~d)不同CP接触时间[(b) 0.2 ms，(c) 1.0 ms，(d) 2.0 ms]的¹H-¹¹⁹Sn CP MAS NMR谱图.(C)不同温度真空脱水的¹¹⁹Sn-Beta分子筛的¹H-¹¹⁹Sn CP-CPMG MAS NMR谱图.(D) (a)脱水与(b)未脱水Sn-Beta分子筛的¹¹⁹Sn DP-CPMG MAS NMR谱图，*表示旋转边带（根据文献[6]和[26]修改）

Fig.1. (A) ¹¹⁹Sn MAS NMR spectra of Sn-Beta after different treatments: (a) Calcined; (b) Dehydrated after calcination; (c) Rehydrated after step (b). (B) (a) ¹¹⁹Sn MAS and (b~d) ¹H-¹¹⁹Sn CP MAS NMR spectra of dehydrated Sn-Beta. The CP contact times from ¹H to ¹¹⁹Sn were varied: (b) 0.2 ms, (c) 1.0 ms, (d) 2.0 ms. (C) ¹H-¹¹⁹Sn CP-CPMG MAS NMR spectra of ¹¹⁹Sn-Beta sample dehydrated under vacuum conditions at different temperatures. (D) ¹¹⁹Sn DP-CPMG MAS NMR spectra of (a) dehydrated and (b) hydrated Sn-Beta. The spinning sidebands are marked as asterisks (Reproduced from Refs. [6] and [26])