Crystal plane engineering of rutile TiO2 nanorods: Boosting Pt-WOx catalyzed glycerol hydrogenolysis to 1,3-propanediol via {110} plane-associated defects

doi:10.1016/S1872-2067(25)64877-7

Abstract

Abstract:

Crystal plane engineering is a powerful tool to optimize catalytic efficiency in heterogeneous catalysis. However, there is a surprising dearth in the exploration of the support plane effect on glycerol hydrogenolysis to 1,3-propanediol (1,3-PDO). In this work, we synthesized prism-shaped rutile TiO₂ nanorods (RTNR-T) with tunable {110}/{111} exposure ratios by varying the hydrothermal temperature. The proportion of the {110} planes is identified to exhibit a volcano-like relationship with the hydrothermal temperature. The concentrations of oxygen vacancies and Ti³⁺ sites on both the RTNR-T nanorods and Pt-WO_x/RTNR-T catalysts are positively correlated with the proportion of the {110} planes. Coherently, the Pt dispersion and surface acidity on the catalysts are parallel to the proportion of the {110} planes, attributable to the high defect density that facilitates the anchorage of Pt and promotes WO_x-support interaction. In glycerol hydrogenolysis, the Pt-WO_x/RTNR-453 catalyst with the highest proportion of the {110} planes displayed the best catalytic performance, with glycerol conversion and 1,3-PDO selectivity of 96.7% and 60.6%, respectively, affording an outstanding 1,3-PDO yield of 58.6% and excellent recyclability. Density functional theory calculations demonstrated that the presence of defects markedly reduced the dissociation and diffusion barriers, which greatly boosts hydrogen spillover to WO_x for in-situ Brönsted acid site generation and oxocarbenium intermediate hydrogenation. This work offers a robust design principle based on the crystal plane-defect-activity correlation for high-performance glycerol hydrogenolysis catalysts.

Key words: Rutile TiO₂, Crystal plane, Surface defect, Glycerol, 1,3-Propanediol

Lan Jiang, Yang Zeng, Jianhua Chen, Songhai Xie, Yan Pei, Weiming Hua, Shirun Yan, Xueying Chen, Minghua Qiao, Baoning Zong. Crystal plane engineering of rutile TiO₂ nanorods: Boosting Pt-WO_x catalyzed glycerol hydrogenolysis to 1,3-propanediol via {110} plane-associated defects[J]. Chinese Journal of Catalysis, 2026, 82: 312-326.

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Figures/Tables 13

Fig. 1. XRD patterns (A) and Raman spectra (B) of the RTNR-433 (a), RTNR-453 (b), RTNR-473 (c), and RTNR-493 (d) nanorods.

Fig. 2. TEM images of the RTNR-433 (a), RTNR-453 (c), RTNR-473 (e), and RTNR-493 (g) nanorods. The inset in (c) is a schematic model of an individual nanorod of RTNR-453. HRTEM images with FFT patterns of the RTNR-433 (b), RTNR-453 (d), RTNR-473 (f), and RTNR-493 (h) nanorods.

Fig. 3. (A) EPR spectra of the RTNR-433 (a), RTNR-453 (b), RTNR-473 (c), and RTNR-493 (d) nanorods. (B) EPR spectra of the Pt-WOx/RTNR-433 (a), Pt-WOx/RTNR-453 (b), Pt-WOx/RTNR-473 (c), and Pt-WOx/RTNR-493 (d) catalysts.

Table 1 Basic physicochemical properties of the Pt?WOx/RTNR-T catalysts.

Catalyst	Pt ^a (wt%)	W ^a (wt%)	A_BET^b (m² g⁻¹)	d_pore^b (nm)	V_pore^b (cm³ g⁻¹)	D_Pt^c (%)	S_Pt^c (m² g_Pt⁻¹)	d_Pt (nm)		n_L^e (μmol g_cat⁻¹)	n_B^e (μmol g_cat⁻¹)
Catalyst	Pt ^a (wt%)	W ^a (wt%)	A_BET^b (m² g⁻¹)	d_pore^b (nm)	V_pore^b (cm³ g⁻¹)	D_Pt^c (%)	S_Pt^c (m² g_Pt⁻¹)	CO ^c	TEM^d	n_L^e (μmol g_cat⁻¹)	n_B^e (μmol g_cat⁻¹)
Pt-WO_x/RTNR-433	3.0	7.0	12	15.7	0.04	23	56	5.0	1.6	10	1
Pt-WO_x/RTNR-453	2.9	7.2	14	16.5	0.05	35	87	3.2	1.4	38	4
Pt-WO_x/RTNR-473	2.9	7.1	17	14.6	0.06	26	64	4.4	1.6	22	3
Pt-WO_x/RTNR-493	2.8	7.0	20	15.2	0.08	22	54	5.2	2.0	9	1

Fig. 4. TEM images (a1?d1), TEM images with particle size distribution histograms of Pt NPs with Gaussian analysis fittings (a2?d2), and HRTEM images with FFT patterns (a3?d3). (a1?a3) Pt-WOx/RTNR-433; (b1?b3) Pt-WOx/RTNR-453; (c1?c3) Pt-WOx/RTNR-473; (d1?d3) Pt-WOx/RTNR-493.

Fig. 5. Ti 2p (A), O 1s (B), Pt 4f/W 5s (C), and W 4f/Ti 3p (D) spectra of the Pt-WOx/RTNR-433 (a), Pt-WOx/RTNR-453 (b), Pt-WOx/RTNR-473 (c), and Pt-WOx/RTNR-493 (d) catalysts.

Table 2 The XPS fitting results and EPR results of the Pt?WOx/RTNR-T catalysts.

Catalyst	Pt²⁺/(Pt⁰ + Pt²⁺) intensity ratio	W⁵⁺/(W⁵⁺ + W⁶⁺) intensity ratio	Ti³⁺/Ti⁴⁺ intensity ratio	O_v/O_L intensity ratio	Pt/Ti (at%)	W/Ti (at%)	O_v^b (spins g⁻¹)	Ti^{3+ b} (spins g⁻¹)
Pt-WO_x/RTNR-433	0.26	0.14	0.20(16.7%) ^a	0.09	0.13	0.22	11.5 × 10²⁰	17.1 × 10¹⁸
Pt-WO_x/RTNR-453	0.39	0.15	0.43(30.1%)	0.17	0.13	0.21	17.6 × 10²⁰	58.7 × 10¹⁸
Pt-WO_x/RTNR-473	0.36	0.15	0.24(19.4%)	0.11	0.11	0.23	13.1 × 10²⁰	32.6 × 10¹⁸
Pt-WO_x/RTNR-493	0.14	0.15	0.14(12.3%)	0.05	0.13	0.21	7.54 × 10²⁰	8.55 × 10¹⁸

Fig. 6. Raman spectra (A), UV-vis spectra (B), and Py-IR spectra (C) of the Pt-WOx/RTNR-433 (a), Pt-WOx/RTNR-453 (b), Pt-WOx/RTNR-473 (c), and Pt-WOx/RTNR-493 (d) catalysts. The Py-IR spectra are collected at 423 K. (D) The quantities of Br?nsted and Lewis acid sites and their total quantities on the Pt-WOx/RTNR-T catalysts.

Table 3 The catalytic results of the Pt-WOx/RTNR-T catalysts in the hydrogenolysis of glycerol.a

Catalyst	Conv. (%)	Sel. (%)					Yield_1,3-PDO (%)	TOF ^c (h⁻¹)
Catalyst	Conv. (%)	1,3-PDO	1,2-PDO	1-PrOH	2-PrOH	Others ^b	Yield_1,3-PDO (%)	TOF ^c (h⁻¹)
Pt-WO_x/RTNR-433	59.5	41.3	0.7	52.3	5.5	trace	24.3	71
Pt-WO_x/RTNR-453	96.7	60.6	0.6	34.8	4.0	trace	58.6	109
Pt-WO_x/RTNR-473	75.6	46.0	0.7	44.3	8.9	trace	35.2	84
Pt-WO_x/RTNR-493	64.2	35.5	0.7	57.5	6.1	trace	22.8	52
WO_x/RTNR-453	—	—	—	—	—	—	—	—
Pt/RTNR-453	0.4	51.0	3.5	20.2	20.1	5.3	0.2	—

Fig. 7. Comparisons of the 1,3-PDO yield over the Pt?WOx/RTNR-453 catalyst with those over the literature TiO2-supported catalysts for glycerol hydrogenolysis (a) and the stability of the Pt?WOx/RTNR-453 catalyst with those of the literature TiO2-supported catalysts for glycerol hydrogenolysis with their stability being reported (b).

Fig. 8. Correlations of the {110}/{111} exposure ratio with the surface defect ratio determined by XPS and the amounts of Ti3+ and Ov quantified by EPR (a), Pt particle size and the amount of acid sites (b), and TOF and selectivity to 1,3-PDO (c).

Fig. 9. (a) Calculated energy profiles for H2 dissociation on Pt-WOx/rutile (110)-Ov and Pt-WOx/rutile (110) surfaces. (b,c) IS, TS, and FS for H2 dissociation on Pt-WOx/rutile (110)-Ov surfaces. (d,e) IS, TS, and FS for H2 dissociation on Pt-WOx/rutile (110) surfaces. IS, TS, and FS represent the initial state, transition state, and final state. Light blue, red, gray, brown, and off-white spheres represent Ti, O, Pt, W, and H, respectively.

Fig. 10. (a) Calculated energy profiles for hydrogen diffusion on Pt-WOx/rutile (110)-Ov and Pt-WOx/rutile (110) surfaces. (b,c) IS, TS, and FS for hydrogen diffusion on Pt-WOx/rutile (110)-Ov surfaces. (d,e) IS, TS, and FS for hydrogen diffusion on Pt-WOx/rutile (110) surfaces. IS, TS, and FS represent the initial state, transition state, and final state. Light blue, red, gray, brown, and off-white spheres represent Ti, O, Pt, W, and H, respectively.

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Crystal plane engineering of rutile TiO₂ nanorods: Boosting Pt-WO_x catalyzed glycerol hydrogenolysis to 1,3-propanediol via {110} plane-associated defects

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