Co nanoparticles modified phase junction CdS for photoredox synthesis of hydrobenzoin and hydrogen evolution

doi:10.1016/S1872-2067(23)64393-1

Abstract

Abstract:

Coupling photocatalytic H₂ production with organic synthesis attracts immense attention in the field of energy research through collecting the sustainable green energy and high value-added products. Although tremendous progress has been made towards devoting to the oxidation of benzyl alcohol, only very limited study can meet high selectivity of the C-C coupled products during the process of H₂ evolution. Herein, the phase junction CdS (HC-CdS2) consisting of hexagonal CdS (H-CdS) with co-exposed facets of (001) and (101) and cubic CdS (C-CdS) was fabricated by fine tuning the proportion of cadmium and sulfur sources for photocatalytic H₂ production and selective benzyl alcohol oxidation. The HC-CdS2 is able to maintain a robust H₂ evolution rate of 11 mmol g^-1 by loading cobalt as cocatalyst, which is 4.7 and 34 times higher than those for C-CdS/Co and HC-CdS2, respectively. Especially, the selectivity of hydrobenzoin elevated from 12% to 97% after loading Co on HC-CdS2 after light irradiation for 9 h. EPR and in situ DRIFTS tests indicated that the hydrogen atom from the C-H bond of benzyl alcohol was abstracted to form ·C₇H₈O free radical. Subsequently, the ·C₇H₈O free radical coupling yield hydrobenzoin as the final C-C coupling product by ameliorating charge separation resulted from the internal electric fields of facet junction and phase junction CdS and Schottky junction between CdS and Co. The strategy can be further extended to various aromatic alcohols and provide a reference for highly selective synthesis of high-added value chemicals coupled with H₂ evolution.

Key words: Facet junction, Internal electric field, H₂ evolution, Hydrobenzoin, Schottky junction

Meiyu Zhang, Kongming Li, Chunlian Hu, Kangwei Ma, Wanjun Sun, Xianqiang Huang, Yong Ding. Co nanoparticles modified phase junction CdS for photoredox synthesis of hydrobenzoin and hydrogen evolution[J]. Chinese Journal of Catalysis, 2023, 47: 254-264.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(23)64393-1

https://www.cjcatal.com/EN/Y2023/V47/I4/254

Figures/Tables 8

Scheme 1. Schematic diagram for photocatalytic oxidation of benzyl alcohol and H2 evolution over HC-CdS2/Co.

Fig. 1. (a) Schematic illustration of the synthesis of HC-CdS2/Co. (b) XRD patterns of H-CdS(001), H-CdS(101), HC-CdS1, HC-CdS2 and C-CdS. (c) UV-vis DRS spectra of H-CdS(001), H-CdS(101), HC-CdS1, HC-CdS2 and C-CdS. High-resolution XPS spectra of S 2p (d) and Cd 3d (e) for HC-CdS2 and HC-CdS2/Co.

Fig. 2. (a-d) HRTEM images of HC-CdS2. (e) TEM image of HC-CdS2/Co. (f) HRTEM image of HC-CdS2/Co.

Fig. 3. (a) Photocatalytic H2 evolution amount over H-CdS(001), H-CdS(101), HC-CdS1, HC-CdS2 and C-CdS (all the catalysts with 1 wt% Co cocatalyst). (b) Photocatalytic H2 evolution rate over HC-CdS2 and HC-CdS2/Co after 9 h of visible light irradiation. (c) Photocatalytic benzyl alcohol oxidation. (d) Benzyl alcohol conversion rate, benzaldehyde and hydrobenzoin selectivity of HC-CdS2 and HC-CdS2/Co after 9 h of visible light irradiation.

Fig. 4. Secondary electron emission cutoff edge (Ecutoff) (a) and work functions (b) for HC-CdS2, HC-CdS2/Co and Co. (c) Schematics of Schottky junction formation in HC-CdS2/Co and charge transfer mechanism. (d) The steady state PL spectra of H-CdS(001), HC-CdS2 and C-CdS. (e) Time-resolved PL spectra of HC-CdS2 and HC-CdS2/Co.

Fig. 5. EPR spectra of 5,5-dimethyl-1-pyrroline N-oxide (DMPO)-·OH (a), DMPO-·O2? (b) and DMPO-·C7H8O (c) for HC-CdS2/Co (blank and simulation represent the signals of EPR spectrometer itself and simulation signals of the standard free radical curves, respectively). (d) In situ DRIFTS spectra of HC-CdS2/Co in photocatalytic H2 production coupled with benzyl alcohol oxidation.

Fig. 6. The optimized structures of H-CdS(101) (a) and H-CdS(001) (b). Band structures of H-CdS(101) (c) and H-CdS(001) (d). The work functions for H-CdS(101) (e) and H-CdS(001) (f).

Fig. 7. (a) Schematics of facet junction formation in H-CdS and charge transfer mechanism. (b) Schematic illustration of photocatalytic H2 production integrated with benzyl alcohol oxidation.

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