Chinese Journal of Catalysis ›› 2023, Vol. 49: 102-112.DOI: 10.1016/S1872-2067(23)64449-3
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Cheng Liua, Mengning Chena, Yingzhang Shia, Zhiwen Wanga, Wei Guoa, Sen Lina,*(), Jinhong Bia,b,*(
), Ling Wua,*(
)
Received:
2023-02-08
Accepted:
2023-04-30
Online:
2023-06-18
Published:
2023-06-05
Contact:
*E-mail: Supported by:
Cheng Liu, Mengning Chen, Yingzhang Shi, Zhiwen Wang, Wei Guo, Sen Lin, Jinhong Bi, Ling Wu. Ultrathin ZnTi-LDH nanosheet: A bifunctional Lewis and Brönsted acid photocatalyst for synthesis of N-benzylideneanilline via a tandem reaction[J]. Chinese Journal of Catalysis, 2023, 49: 102-112.
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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(23)64449-3
Fig. 3. (a) UV-vis DRS spectra and corresponding Tauc plots of the samples; The Zn 2p (b), Ti 2p (c) and O 1s (d) XPS spectra of the samples; FTIR (e) and ESR (f) spectra of the samples.
Type | Binding energy (eV) | ZT-1 (%) | ZT-2 (%) |
---|---|---|---|
O-lattice | 529.6 | 18.90 | 29.70 |
O-vacancy | 530.2 | 6.30 | 2.60 |
O-OH group | 531.4 | 39.40 | 25.50 |
O-H2O | 532.1 | 25.20 | 34.00 |
O-CO32- | 532.9 | 10.20 | 8.20 |
Table 1 The proportion of different types of O atoms in the samples.
Type | Binding energy (eV) | ZT-1 (%) | ZT-2 (%) |
---|---|---|---|
O-lattice | 529.6 | 18.90 | 29.70 |
O-vacancy | 530.2 | 6.30 | 2.60 |
O-OH group | 531.4 | 39.40 | 25.50 |
O-H2O | 532.1 | 25.20 | 34.00 |
O-CO32- | 532.9 | 10.20 | 8.20 |
Fig. 4. Nyquist impedance plots (a) and photocurrent measurements (b) of the samples. (c) In situ FT-IR spectra of pyridine absorption on ZT-1: (1) Degassing stage; (2) Physical and chemical adsorption stage; (3) Chemical adsorption stage. (d) The acid sites in ZT-1 structure. (e) On-off light experiments for the tandem reaction over ZT-1. (f) The experiments about the effect of the molar ratio of benzyl alchol and nitrobenzene to reaction activity.
Entry | Catalyst | Temperature (°C) | Atmosphere | hv (λ ≥ 320 nm) | Conversion (%) | Selectivity (%) |
---|---|---|---|---|---|---|
1 | ZT-1 | 25 | Ar | + | 100 | 96 |
2 | ZT-2 | 25 | Ar | + | 76 | 58 |
3 | ZT-1 | 25 | Ar | λ ≥ 400 nm | 18 | 37 |
4 | ZT-1 | 25 | Air | + | — | — |
5 | None | 25 | Ar | + | — | — |
6 | ZT-1 | 25 | Ar | — | — | — |
7 | ZT-1 | 80 | Ar | — | — | — |
Table 2 Photocatalytic activity tests for the tandem reaction.
Entry | Catalyst | Temperature (°C) | Atmosphere | hv (λ ≥ 320 nm) | Conversion (%) | Selectivity (%) |
---|---|---|---|---|---|---|
1 | ZT-1 | 25 | Ar | + | 100 | 96 |
2 | ZT-2 | 25 | Ar | + | 76 | 58 |
3 | ZT-1 | 25 | Ar | λ ≥ 400 nm | 18 | 37 |
4 | ZT-1 | 25 | Air | + | — | — |
5 | None | 25 | Ar | + | — | — |
6 | ZT-1 | 25 | Ar | — | — | — |
7 | ZT-1 | 80 | Ar | — | — | — |
Entry | Group (R) | t (h) | Conversion (%) | Selectivity (%) |
---|---|---|---|---|
1 | -H | 4.0 | 100 | 96 |
2 | -Cl | 3.0 | 98 | 97 |
3 | -Br | 3.5 | 100 | 95 |
4 | -CH3 | 5.0 | 93 | 96 |
5 | -OCH3 | 5.5 | 95 | 97 |
Table 3 Photocatalytic activity tests using various nitroarenes.
Entry | Group (R) | t (h) | Conversion (%) | Selectivity (%) |
---|---|---|---|---|
1 | -H | 4.0 | 100 | 96 |
2 | -Cl | 3.0 | 98 | 97 |
3 | -Br | 3.5 | 100 | 95 |
4 | -CH3 | 5.0 | 93 | 96 |
5 | -OCH3 | 5.5 | 95 | 97 |
Fig. 5. UV-vis DRS spectra of ZT-1 after the adsorption of benzyl alcohol (a) and nitrobenzene (b). (c) ESR spectra of the samples. In situ FTIR spectra of benzyl alcohol (d) and nitrobenzene (e) absorbed on ZT-1: (1) FTIR spectrum of free benzyl alcohol or nitrobenzene; (2) Degassing stage; (3) Physical and chemical adsorption stage; (4) Chemical adsorption stage. (f) Simulated in situ ESR spectra of the samples in the mixed solution (1.5 mL of BTF and 0.100 mmol of BA) in Ar atmosphere using DMPO as spin trapping agent.
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