前驱体协同双模板剂辅助合成强酸性SAPO-17分子筛及其铜交换后优异的NH3-SCR催化性能

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

催化学报 ›› 2025, Vol. 78: 279-291.DOI: 10.1016/S1872-2067(25)64801-7

前驱体协同双模板剂辅助合成强酸性SAPO-17分子筛及其铜交换后优异的NH₃-SCR催化性能

王冶^a^,^b, 高攀^c, 赵丹^b, 刘桐睿^b, 周思彤^b, 杨淼^b^,^*(), 刘世平^b, 李冰^b, 周易达^b, 崔文浩^d, 侯广进^c, 田鹏^b, 刘中民^b^,^*()

^a郑州大学化学学院, 河南郑州 450001
^b中国科学院大连化学物理研究所, 洁净能源国家实验室, 低碳催化技术国家工程研究中心, 辽宁大连 116023
^c中国科学院大连化学物理研究所, 洁净能源国家实验室, 催化基础国家重点实验室, 辽宁大连 116023
^d中国科学院大连化学物理研究所, 能源研究技术平台, 辽宁大连 116023

收稿日期:2025-06-03 接受日期:2025-08-05 出版日期:2025-11-18 发布日期:2025-10-14
通讯作者: *电子信箱: yangmiao@dicp.ac.cn (杨淼), liuzm@dicp.ac.cn (刘中民).
基金资助:
国家重点研发计划(2024YFE0207000);国家自然科学基金(22171259);国家自然科学基金(22288101);中法国际研究框架(IRN);榆林中科洁净能源创新研究院人工智能科技专项资助(DNL-YL A202206)

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

Ye Wang^a^,^b, Pan Gao^c, Dan Zhao^b, Tongrui Liu^b, Sitong Zhou^b, Miao Yang^b^,^*(), Shiping Liu^b, Bing Li^b, Yida Zhou^b, Wenhao Cui^d, Guangjin Hou^c, Peng Tian^b, Zhongmin Liu^b^,^*()

^aCollege of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, China
^bNational Engineering Research Center of Lower-Carbon Catalysis Technology, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^cState Key Laboratory of Catalysis, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^dDivision of Energy Research Resources, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China

Received:2025-06-03 Accepted:2025-08-05 Online:2025-11-18 Published:2025-10-14
Contact: *E-mail: yangmiao@dicp.ac.cn (M. Yang), liuzm@dicp.ac.cn (Z. Liu).
Supported by:
National Key Research and Development Program of China(2024YFE0207000);National Natural Science Foundation of China(22171259);National Natural Science Foundation of China(22288101);Sino-French IRN(International Research Network);AI S&T Program of Yulin Branch, Dalian National Laboratory for Clean Energy, CAS(DNL-YL A202206)

摘要/Abstract

摘要：

磷酸硅铝(SAPO)分子筛因其丰富的拓扑结构和优异的水热稳定性, 在酸催化领域备受关注. 然而, 提升特定SAPO分子筛的酸性质仍面临巨大挑战, 使其难以应用于高酸性要求的催化反应. 与硅铝分子筛不同, SAPO分子筛的酸性质主要取决于磷酸铝骨架中的Si原子取代量和取代方式(形成不同的硅化学环境). 尽管已发展了多种新型模板剂和合成方法, 精准地协同调控SAPO材料的晶相、Si引入量和Si分布仍是研究者孜孜以求的目标.

本文发展了一种SAPO前驱体协同双模板剂(结构导向剂)辅助的合成新策略(SPDT), 实现了一系列强酸性SAPO分子筛, 包括SAPO-34/56共晶、SAPO-56和SAPO-17的合成. SAPO前驱体作为唯一的无机源为合成体系提供了丰富的富含Si−O−Al键的结构单元, 不仅调节结晶动力学还促进了Si原子的骨架引入. 第二模板剂同时起到晶相选择的作用. 在第一模板剂相同的合成体系中, 当不含第二模板剂时得到了SAPO-34/56共晶产物; 以二甲胺或三甲胺为第二模板剂时, 生成SAPO-56; 而引入氯化铵或氯化钾作为第二模板剂时则生成了高硅含量的SAPO-17分子筛. 利用积分差分相位衬度成像技术、二维固体核磁共振和连续旋转电子衍射等先进表征技术对合成的SAPO材料进行了详细表征. 值得关注的是, 基于SPDT策略制备的负载型Cu-SAPO-17分子筛(Cu_1.6-S17-N)在NH₃选择性催化还原(NH₃-SCR)反应中展现出超宽的活性温度窗口: 在180000 h^-1空速条件下, NO_x转化率90%以上的温度区间覆盖175-700 °C. 进一步的对比研究和表征显示Cu-SAPO-17优异的催化性能主要归因于SAPO-17独特的ERI结构和改善的酸性.

综上, 本文发展了一种强酸性SAPO分子筛的合成新策略, 实现了系列强酸性SAPO分子筛的合成. 基于该策略制备的SAPO-17分子筛在铜负载后展现出卓越的NH₃-SCR催化性能. 本工作不仅为合成高酸性SAPO分子筛提供了一种高效通用的策略, 还为SAPO材料在多相催化领域的应用开拓了更多可能; 同时也为拓展NH₃-SCR反应的活性温度窗口提供了全新的研究思路, 对基础研究与工业应用均具有重要意义.

关键词: SAPO分子筛, 氨选择性催化还原, 超宽活性温度窗口, Si分布, 酸性

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

王冶, 高攀, 赵丹, 刘桐睿, 周思彤, 杨淼, 刘世平, 李冰, 周易达, 崔文浩, 侯广进, 田鹏, 刘中民. 前驱体协同双模板剂辅助合成强酸性SAPO-17分子筛及其铜交换后优异的NH₃-SCR催化性能[J]. 催化学报, 2025, 78: 279-291.

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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图/表 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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前驱体协同双模板剂辅助合成强酸性SAPO-17分子筛及其铜交换后优异的NH₃-SCR催化性能

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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