Chinese Journal of Magnetic Resonance ›› 2021, Vol. 38 ›› Issue (4): 460-473.doi: 10.11938/cjmr20212913
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Received:
2021-04-28
Online:
2021-12-05
Published:
2021-06-16
Contact:
Jun HUANG
E-mail:jun.huang@sydney.edu.au
Supported by:
CLC Number:
Wen-jie YANG,Jun HUANG. Analysis of Local Structure, Acidic Property and Activity of Solid Acids by Solid-State Nuclear Magnetic Resonance Spectroscopy[J]. Chinese Journal of Magnetic Resonance, 2021, 38(4): 460-473.
Table 1
Typical 1H MAS NMR chemical shifts (δH) of various hydroxyl group in various solid acid catalysts
Solid acid | Hydroxyl group | δH | Assignment | Reference |
Zeolite | Si(OH) | 1.2~2.3 | 晶体表面或缺陷位的硅烷醇羟基 | [ |
Al(OH) | 2.1~2.8 | 金属修饰分子筛上骨架外的桥接羟基 | [ | |
Si(OH)Al | 3.3~4.4 | 超笼中桥接羟基 | [ | |
Si(OH)Al | 4.6~8.0 | 方纳石笼中具有氢键或通过静电相互作用被骨架干扰的通道中桥接羟基 | [ | |
Si(OH)Si | 10.0~16.0 | 探针分子吸附后的探测到的双硅烷醇基或以氢键相连的内部硅烷醇基 | [ | |
Amorphous | Si(OH) | 1.7~2.3 | 骨架上硅烷醇基 | [ |
Silica-alumina | Si(OH)Al/Al(OH) | 2.5~4.0 | 酸性羟基 | [ |
Heteropoly acid | Keggin units H+ | 6.7~9.3 | 杂多酸的凯金(Keggin)结构中的酸性羟基 | [ |
Metal-organic framework | Al(OH)Al | 1.7~2.7 | 骨架上桥接羟基 | [ |
Mixed oxides | M(OH) | 2.0~6.7 | 末端金属羟基和桥连金属羟基 | [ |
M(OH)..H2O..H2O | 9.5~10.3 | 通过氢键与水分子通过氢键相互作用两次的桥接金属羟基 | [ |
Table 2
Some commonly used probe molecules and the chemical shift changes-based characterization of acid site
Probe molecules | Strength of BAS | Strength of LAS | Reference |
Deuterated acetonitrile (CD3CN) | δH: 3.6 Weak | / | [ |
Pyridine-d5 (C5D5N) | δH: 12 Strong | / | [ |
Acetone-2-13C ((CH3)213CO) | δC: 216 Weak | δC: 233 Weak | [ |
15N-pyridine | δN: 212 Strong | δN: 260 Strong | [ |
Trimethylphosphine oxide (TMPO) | δP: 55 Weak | δP: 37 Weak | [ |
Trimethylphosphine (TMP) | δP: -2 Larger J-coupling constant between 31P and 1H | δP: -13 ~ -52 δP depends on Lewis centers, for identical Lewis centers, smaller δP | [ |
Table 3
Probe molecules for solid acid acidity characterizationa
Probe molecule | MAS NMR technique | Type | Strength | Density | Accessibility | |||||
B | L | B | L | B | L | |||||
Trimethylphosphine (TMP) | 31P | √ | √ | √ | √ | √ | √ | √ | ||
Acetone-2-13C ((CH3)213CO) | 13C | √ | √ | √ | ❌ | ❌ | ||||
Ammonia (NH3) | 1H | √ | √ | ❌ | ❌ | √ | √ | |||
Pyridine-d5 (C5D5N) | 1H | √ | ❌ | √ | ❌ | ❌ | √ | |||
15N-pyridine | 15N | √ | √ | √ | √ | √ | √ | √ | ||
Trialkylphosphine oxides (R3PO) | 31P | √ | √ | √ | √ | √ | √ | |||
Deuterated acetonitrile (CD3CN) | 1H | √ | ❌ | √ | ❌ | √ | ❌ | |||
Perfluorotributylamine | 1H | √ | ❌ | ❌ | ❌ | ❌ | √ |
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