Chem. J. Chinese Universities ›› 2021, Vol. 42 ›› Issue (1): 165.doi: 10.7503/cjcu20200416
Special Issue: 分子筛功能材料 2021年,42卷,第1期
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Received:
2020-07-01
Online:
2021-01-10
Published:
2021-01-12
Contact:
HUANG Jun
E-mail:jun.huang@sydney.edu.au
Supported by:
CLC Number:
TrendMD:
ZHAO Shufang, HUANG Jun. Study by Solid-state NMR Spectroscopy on the Acidity and Shape-selectivity of Zeolites[J]. Chem. J. Chinese Universities, 2021, 42(1): 165.
MAS NMR | Resonance, δ | Assignment | Correlations with acid sites |
---|---|---|---|
1H[ | 3.6—5.2 | SiOHAl, bridging hydroxyl group | BASs |
0.6—3.6 | Extraframework AlOH | LASs | |
1.2—2.2 | Nonacidic SiOH | ||
27Al[ | 50—65 | Four?coordinated framework Al | BASs |
30—40 | Five?coordinated extra?framework Al | LASs | |
-10—15 | Six?coordinated extra?framework Al | LASs | |
29Si[ | -100—-115 | Si(0Al) | The strength of acidity |
-95—-105 | Si(1Al) | ||
-90—-100 | Si(2Al) | ||
-85—-95 | Si(3Al) | ||
-80—-90 | Si(4Al) | ||
17O[ | -20—20 | Si—O—Si | No direct correlation |
10—40 | Si—O—Al | ||
11B[ | 12 | B(OSi)3 | Weak BASs |
15 | B(OSi)2(OH) | ||
71Ga[ | 150—160 | Tetrahedral framework Ga | BASs |
-7—12 | Octahedral extra?framework Ga | LASs | |
119Sn[ | -443 and -435 | 4?Coordinated closed Sn site | LASs |
-420 | 6?Coordinated open Sn site |
Table 1 Assignments of MAS NMR chemical shift of framework atoms in zeolites
MAS NMR | Resonance, δ | Assignment | Correlations with acid sites |
---|---|---|---|
1H[ | 3.6—5.2 | SiOHAl, bridging hydroxyl group | BASs |
0.6—3.6 | Extraframework AlOH | LASs | |
1.2—2.2 | Nonacidic SiOH | ||
27Al[ | 50—65 | Four?coordinated framework Al | BASs |
30—40 | Five?coordinated extra?framework Al | LASs | |
-10—15 | Six?coordinated extra?framework Al | LASs | |
29Si[ | -100—-115 | Si(0Al) | The strength of acidity |
-95—-105 | Si(1Al) | ||
-90—-100 | Si(2Al) | ||
-85—-95 | Si(3Al) | ||
-80—-90 | Si(4Al) | ||
17O[ | -20—20 | Si—O—Si | No direct correlation |
10—40 | Si—O—Al | ||
11B[ | 12 | B(OSi)3 | Weak BASs |
15 | B(OSi)2(OH) | ||
71Ga[ | 150—160 | Tetrahedral framework Ga | BASs |
-7—12 | Octahedral extra?framework Ga | LASs | |
119Sn[ | -443 and -435 | 4?Coordinated closed Sn site | LASs |
-420 | 6?Coordinated open Sn site |
Fig.1 1H MAS NMR spectra of dehydrated Hβ with different Si/Al ratios of Hβ1 to Hβ4[38](A) Hβ1; (B) Hβ2; (C) Hβ3; (D) Hβ4. Recorded before(top) and after(bottom) adsorption of CD3CN at room temperature and purged with under a N2 flow of 50 mL for 10 min. Copyright 2017, American Chemical Society.
Fig.2 1H MAS NMR spectra recorded at 7.05?T of H‐ZSM‐5, ZSM‐5(G2), ZSM‐5(I2), and ZSM‐5(I6)(A) and pyridine?d5 adsorbed on these samples(B)[20]Copyright 2016, Wiley?VCH.
Fig.3 Stack plot of the 1H MAS NMR spectra recorded at the temperature of 358 K during H/D exchange of deuterated ethylbenzene loaded on dehydrated zeolite H?Y[49]Copyright 2006, Elsevier.
Fig.4 Proton‐decoupled 31P MAS NMR spectra of MFI‐2(a, b) and Zn/MFI‐2(c, d) zeolite samples[55]The ratio TMP/BAS: a. 0.4, b. 1.3, c. 0.5, d. 2.6. Copyright 2019, Wiley?VCH.
Fig.5 Schematic representation of TMPO?loaded HZSM?5[n(Si)/n(Al)=15] and silicalite?1(A, C, E), 1H?31P HETCOR NMR spectra of TMPO?lloaded silicalite?1, HZSM?5, and steam?HZM?5(B, D, F)[10](B, D, F) The F2 axes??(top) projections display the 31P CPMAS NMR spectra. Copyright 2019, Royal Society of Chemistry.
Fig.6 13C CP/MAS NMR spectra of 2?13C?acetone adsorbed on parent H?Y(a), CAL?400(b), CAL?500(c), CAL?600(d), CAL?700(e), STY?350(f), STY?450(g), STY?550(h), OXA?0.8(i), and OXA?1.4(j) zeolites[57]Asterisks denote spinning sidebands. Copyright 2008, American Chemical Society.
Fig.7 27Al MAS and DQ‐MAS NMR spectra of parent HY(A), HY‐500(B), HY‐600(C), and ?HY‐700(D) zeolites[64]One‐dimensional 27Al MAS spectra are plotted on top of the two‐dimensional 27Al DQ MAS spectra. All spectra were recorded on hydrated samples at 18.8?T with a 3.2?mm probe at a sample rotation rate of 21.5?kHz. About 45?h were required to record one 27Al DQ‐MAS NMR spectrum. Copyright 2010, John Wiley & Sons.
Fig.8 13C MAS NMR spectra of deactivated H?SSZ?13(a) and HMOR(b) at 400 °C for 250 and 100 min, respectively[67]The black and red lines represent the spectrum observed with(S) and without(S0) 13C?{27Al} S?RESPDOR dipolar dephasing, respectively. The ΔS/S0 is indicated in parentheses. Copyright 2017, American Chemical Society.
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