Precursor and dual-template assisted synthesis of highly acidic SAPO-17 molecular sieve: Excellent NH3-SCR activity of Cu-exchanged forms

doi:10.1016/S1872-2067(25)64801-7

Abstract

Abstract:

Silicoaluminophosphate (SAPO) molecular sieves possess diverse architectures and exceptional high-temperature hydrothermal stability, rendering them important acid catalysts. However, enhancing acid concentration of certain SAPO materials remains challenging, which limits their catalytic applications. Here, we report the synthesis of a series of SAPO materials using a developed SAPO precursor plus dual template (SPDT) strategy. A variety of SAPO materials characterized by high silica content and enhanced acidity, such as SAPO-34/56 intergrowths, SAPO-56, and SAPO-17, have been synthesized and thoroughly characterized using various techniques including integrated differential phase-contrast scanning transmission electron microscopy, two-dimensional solid-state nuclear magnetic resonance spectroscopy, and continuous rotation electron diffraction. The use of silica-enriched SAPO precursor combined with the flexible selection of the second template enables the crystalline phase regulation and improves the Si atoms incorporation into the framework. Notably, the synthesized SAPO-17 with abundant Si(4Al) species and unprecedentedly high acid density exhibits exceptional DeNO_x activity after Cu loading, with NO_x conversion exceeding 90% at 175-700 °C. This outstanding performance can be attributed to the unique ERI structure and the increased acidity of SAPO-17. This work not only presents an effective method for synthesizing SAPO molecular sieves with enhanced acidity but also offers a new perspective for expanding the active temperature range of the ammonia selective catalytic reduction reaction.

Key words: SAPO molecular sieve, Ammonia selective catalytic reduction, Ultra-wide temperature window, Si distribution, Acidity

Ye Wang, Pan Gao, Dan Zhao, Tongrui Liu, Sitong Zhou, Miao Yang, Shiping Liu, Bing Li, Yida Zhou, Wenhao Cui, Guangjin Hou, Peng Tian, Zhongmin Liu. Precursor and dual-template assisted synthesis of highly acidic SAPO-17 molecular sieve: Excellent NH₃-SCR activity of Cu-exchanged forms[J]. Chinese Journal of Catalysis, 2025, 78: 279-291.

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Figures/Tables 9

Scheme 1. The SPDT strategy and the synthesized SAPO materials including SAPO-17, SAPO-34/56 intergrowth and SAPO-56.

Table 1 Synthesis conditions and results of SAPO materials a.

Sample	Mass ratio of L/S^c	2^nd template^d	Chemical compositions^e	SSA ^f (m² g^-1)			Pore volume ^g (cm³ g^-1)		OSDA ^h (wt%)	C/N^j	Strong acid ^m (mmol g^-1)	Cu/Si^e
Sample	Mass ratio of L/S^c	2^nd template^d	Chemical compositions^e	S_BET	S_micro	S_ext	V_total	V_micro	OSDA ^h (wt%)	C/N^j	Strong acid ^m (mmol g^-1)	Cu/Si^e
S34/56-10	10:1	—	Al_0.470Si_0.201P_0.328O₂	558	507	51	0.34	0.25			1.25
S34/56-3	3:1	—	Al_0.455Si_0.217P_0.327O₂	568	506	62	0.34	0.25		4.60	1.14
S56-DMA	10:1	DMA	Al_0.496Si_0.193P_0.311O₂	571	520	51	0.33	0.25	18	4.89	1.17	0.14
S56-TMA	10:1	TMA	Al_0.492Si_0.197P_0.311O₂	547	478	69	0.39	0.23
S17-N ^b	10:1	NH₄⁺	Al_0.491Si_0.197P_0.312O₂	479	434	45	0.29	0.21	16	3.84	1.06	0.08/0.14/0.22
S17-K ^b	10:1	K⁺	Al_0.487Si_0.196P_0.317O₂	330	306	24	0.20	0.15	13	5.00	0.59	0.14
S17-C	N/A	N/A	Al_0.437Si_0.185P_0.378O₂	448	403	45	0.32	0.20	11.5		0.36	0.12
S56-C	N/A	N/A	Al_0.452Si_0.204P_0.344O₂	616	547	70	0.37	0.27

Fig. 1. Simulated and experimental XRD patterns (a), SEM images (b,c), TG analysis (d) of as-synthesized S17-N and S17-K. N2 adsorption (e) and NH3-TPD profiles (f) of calcined S17-N and S17-K samples.

Fig. 2. The crystal structures of S17-N (a) and S17-K (b) viewed along the [110] direction. The positions of TMHDA (R) and inorganic cations are shown in it. Due to the high structural symmetry, the positioning of some methyl groups and H atoms failed.

Fig. 3. Solid-state 31P (a), 29Si (b), 27Al (c) MAS NMR, 2D 27Al 3Q MAS NMR (d), 2D 31P-27Al MQ-J-RINEPT correlation MAS NMR (e) spectra of as-made S17-N. (f) 1H MAS NMR spectra of calcined S17-N and S17-K.

Fig. 4. NOx conversions as a function of temperature during standard NH3-SCR for fresh (a) and hydrothermal aged (b) Cux-S17-N, fresh (c) and hydrothermally aged (d) Cu2.5-S17-K, Cu2.8-S17-C and Cu2.5-ERI-6.4 catalysts. Catalytic conditions: 500 ppm NO, 500 ppm NH3, 14% O2, 4.5% H2O, balanced with N2, GHSV = 180000 h-1.

Table 2 Comparison of the structural characteristics and physical properties of molecular sieves.

Essential rings of three zeolite topologies ^a
Structure type		ERI		CHA	AFX
Essential rings		[8₁·6₃·4₂]		[8₁·6₁·4₂]	[8₂·6₂·4₄]
The percentage of 6-ring units (%)		52.9		27.3	27.3
Deconvolution results of the distributions of paired acidic sites ^b
Sample	Paired acidic sites (%)	τ (%)	ω (%)		σ (%)
Co-S17-N	77.8	32.8	38.8		6.1
Co-ERI-6.4	26.0	9.1	15.3		1.6

Fig. 5. (a) H2-TPR curves of fresh Cu1.6-S17-N, Cu2.9-S17-N and Cu4.4-S17-N. (b) EPR spectra of fresh and hydrothermally aged Cu2.9-S17-N. (c) XANES spectra of Cu2.9-S17-N, Cu2.9-S17-N-HT and reference materials. (d) EXAFS of Cu K-edge of Cu2.9-S17-N, Cu2.9-S17-N-HT and reference materials (not corrected for phase shift).

Fig. 6. The possible paired acidic sites and copper locations in the S17-N with ERI topology.

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Precursor and dual-template assisted synthesis of highly acidic SAPO-17 molecular sieve: Excellent NH₃-SCR activity of Cu-exchanged forms

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