提高Cu-SSZ-39分子筛八元环骨架铝含量增强其低温氨选择催化还原性能

doi:10.1016/S1872-2067(25)64800-5

催化学报 ›› 2025, Vol. 78: 292-302.DOI: 10.1016/S1872-2067(25)64800-5

提高Cu-SSZ-39分子筛八元环骨架铝含量增强其低温氨选择催化还原性能

靳科研^a^,¹, 韩金峰^a^,^e^,¹, 魏颖真^a, 王云峥^b, 李菁^c, 刘忠其^d, 单玉龙^d, 贾然^a, 闫文付^a^,^*(), 于吉红^a^,^e^,^*()

^a吉林大学化学学院, 无机合成与制备化学全国重点实验室, 吉林长春 130012
^b中国石化上海石油化工研究院有限公司, 上海 201208
^c吉林化工学院, 吉林吉林 132012
^d中国科学院生态环境科学研究中心, 大气环境与污染控制重点实验室, 北京 100085
^e吉林大学, 未来科学国际合作联合实验室, 吉林长春 130012

收稿日期:2025-05-10 接受日期:2025-07-14 出版日期:2025-11-18 发布日期:2025-10-14
通讯作者: *电子信箱: yanw@jlu.edu.cn (闫文付), jihong@jlu.edu.cn (于吉红).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2021YFA1500401);国家自然科学基金(22288101);国家自然科学基金(22201095);高等学校学科创新引智计划(B17020)

Enriching framework Al sites in 8-membered rings of Cu-SSZ-39 zeolite to enhance low-temperature ammonia selective catalytic reduction performance

Keyan Jin^a^,¹, Jinfeng Han^a^,^e^,¹, Yingzhen Wei^a, Yunzheng Wang^b, Jing Li^c, Zhongqi Liu^d, Yulong Shan^d, Ran Jia^a, Wenfu Yan^a^,^*(), Jihong Yu^a^,^e^,^*()

^aState Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, Jilin, China
^bSinopec Shanghai Research Institute of Petrochemical Technology Co., Ltd. Shanghai 201208, China
^cJilin Institute of Chemical Technology, Jilin 132012, Jilin, China
^dLaboratory of Atmospheric Environment and Pollution Control, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China
^eInternational Center of Future Science, Jilin University, Changchun 130012, Jilin, China

Received:2025-05-10 Accepted:2025-07-14 Online:2025-11-18 Published:2025-10-14
Contact: *E-mail: yanw@jlu.edu.cn (W. Yan), jihong@jlu.edu.cn (J. Yu).
About author:¹Contributed equally to this work.
Supported by:
National Key Research and Development Program of China(2021YFA1500401);National Natural Science Foundation of China(22288101);National Natural Science Foundation of China(22201095);‘111 Center’(B17020)

摘要/Abstract

摘要：

氮氧化物(NO_x)是主要的空气污染源之一. 2023年, 移动源(主要是柴油车)排放的氮氧化物超过了中国氮氧化物排放总量的60%. 在现有氮氧化物减排技术中, 氨气选择性催化还原技术(NH₃-SCR)被认为是最有效且应用最广泛的方法之一. 柴油发动机冷启动阶段排放的NO_x约占总排放量的80%. 因此, 提高催化剂的低温NH₃-SCR活性是进一步减少NO_x排放的关键. 铜基SSZ-39催化剂因具有出色的水热稳定性, 被认为是下一代可商用的NH₃-SCR催化剂. 但传统方法合成的SSZ-39中, 八元环骨架铝含量较低, 限制了活性物种[Cu(OH)]⁺-Z的形成, 导致其低温活性(150-225 °C)受限. 因此, 开发简单且成本低的策略以提高铜基SSZ-39催化剂八元环骨架铝含量, 进而增强其低温NH₃-SCR性能, 对于其大规模商业应用至关重要.

铜基分子筛催化剂中存在两种铜物种: Cu²⁺-2Z和[Cu(OH)]⁺-Z. 其中, Cu²⁺-2Z具有高水热稳定性, [Cu(OH)]⁺-Z则具有高反应活性, 后者对于促进催化剂的低温NH₃-SCR活性至关重要; 而这两种活性铜物种的生成受分子筛中骨架铝(Al)的分布影响. 基于此规律, 本文开发了一种提高SSZ-39分子筛八元环骨架铝含的新合成策略. 不同于传统的转晶法和晶种辅助法, 该策略以SAPO-18为晶种, 采用胶体二氧化硅和硫酸铝分别作为硅源和铝源, 并创新性使用K⁺作为唯一无机结构导向剂来合成SSZ-39分子筛(SSZ-39-K). 红外光谱和热重数据表明, K⁺可以替代SSZ-39分子筛骨架中aei笼中的质子化有机结构导向剂, 促进八元环中骨架铝的富集. 固体紫外和二维Al固体核磁分析表明, 与传统方法合成的SSZ-39(SSZ-39-T)相比, SSZ-39-K八元环骨架Al含量增加了37.6%; 氢气程序升温还原和密度泛函理论计算表明, 这些八元环上的Al显著促进了[Cu(OH)]⁺-Z活性物种的生成. 在800 °C水热老化16 h后, Cu_3.7-SSZ-39-K在150-225 °C范围内的NO_x还原效率是Cu_3.4-SSZ-39-T的两倍, 展现出优异的低温NH₃-SCR活性. 此外, 目前已报道的晶种辅助法合成SSZ-39的最高产率仅为33%, 而本方法的为65%, 几乎是前者的两倍, 显著提高了原料利用率并降低了SSZ-39的生产成本.

综上, 本文开发了一种实用且可拓展的合成策略, 既能降低SSZ-39的合成成本, 又能增强铜基SSZ-39催化剂的低温NH₃-SCR活性, 从而推动SSZ-39分子筛在NO_x排放控制技术中的商业应用.

关键词: SSZ-39分子筛, 铝调控, 低温活性, NH₃-选择催化还原, 骨架Al富集

Abstract:

The distributions of framework aluminum (Al) in zeolites critically govern the location and speciation of active copper (Cu) centers, thereby influencing their performance in ammonia selective catalytic reduction (NH₃-SCR) of nitrogen oxides (NOₓ). Conventional Cu-SSZ-39 (Cu-SSZ-39-T) exhibits excellent hydrothermal stability but limited low-temperature activity (150-225 °C) due to a low concentration of Al in 8-membered rings (8MRs) that inhibits the formation of active [Cu(OH)]⁺-Z species. Herein, an SSZ-39 zeolite synthesized with potassium ions (SSZ-39-K) achieved a significantly higher 8MR Al fraction (37.6%). Density functional theory calculations and H₂-temperature-programmed reduction analyses confirmed that the increased 8MR Al population facilitated the formation of [Cu(OH)]⁺-Z species. Aged Cu-SSZ-39-K exhibited nearly twice the NO_x conversion of aged Cu-SSZ-39-T in the 150-225 °C range while maintaining comparable high-temperature activity (250-550 °C) under a gas hourly space velocity of 250,000 h^-1. Enhanced low-temperature performance is particularly beneficial for mitigating NO_x emissions during cold-start phase. Moreover, SSZ-39-K was synthesized with a high crystallization yield (~65%), nearly double the highest yield (33%) reported for direct synthesis routes. This work establishes a robust strategy for tailoring Al distributions in SSZ-39 zeolites, offering an effective pathway to improve low-temperature NH₃-SCR performance and promote practical implementation.

Key words: SSZ-39 zeolite, Al regulation, Low-temperature activity, Ammonia selective catalytic reduction, Enriching framework Al sites

靳科研, 韩金峰, 魏颖真, 王云峥, 李菁, 刘忠其, 单玉龙, 贾然, 闫文付, 于吉红. 提高Cu-SSZ-39分子筛八元环骨架铝含量增强其低温氨选择催化还原性能[J]. 催化学报, 2025, 78: 292-302.

Keyan Jin, Jinfeng Han, Yingzhen Wei, Yunzheng Wang, Jing Li, Zhongqi Liu, Yulong Shan, Ran Jia, Wenfu Yan, Jihong Yu. Enriching framework Al sites in 8-membered rings of Cu-SSZ-39 zeolite to enhance low-temperature ammonia selective catalytic reduction performance[J]. Chinese Journal of Catalysis, 2025, 78: 292-302.

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图/表 6

Fig. 1. (a) Simulated XRD pattern of AEI zeolite compared to the experimental XRD patterns of as-synthesized SSZ-39 zeolites. (b) 27Al MAS NMR spectra of SSZ-39-K and SSZ-39-T. (c) 29Si MAS NMR spectra of SSZ-39-K and SSZ-39-T. (d) Influence of the K+/Na+ ratio on crystallization, maintaining constant alkalinity and total inorganic cation content. (e) FT-IR spectra of solid samples isolated during the crystallization process of SSZ-39 over a 24 h period.

Table 1 Influence of K+/SiO2 and Na+/SiO2 ratios on the crystallized products from initial mixtures with the molar compositions: SiO2:0.021 Al2O3: 0.101 DMDMPOH:X KOH:Y NaOH:7.61 H2O, where X + Y = 0.598 a.

Run	K⁺/SiO₂	Na⁺/SiO₂	Phase	OSDA loss (%)	Si/Al
1^b	0.598	0	AEI	6.59	5.3
2	0.478	0.120	AEI	9.62	6.1
3	0.359	0.239	AEI&LTL	—	—
4	0.239	0.359	AEI	9.58	6.9
5	0.120	0.478	AEI	11.3	6.8
6	0	0.598	AEI	12.14	7.3

Fig. 2. NOx conversion as a function of temperature during the NH3-SCR reaction over fresh (a,c) and hydrothermally aged (800 °C for 16 h) (b,d) Cu3.7-SSZ-39-K, Cu3.4-SSZ-39-T, and Cu3.5-SSZ-13 catalysts. Reactions conditions: 0.05% NO, 0.05% NH3, 5 vol% H2O, and 5 vol% O2 balanced with N2, GHSV = 250,000 h?1.

Fig. 3. EPR spectra (a) and UV-vis spectra (b) of the Cu3.4-SSZ-39-T catalyst before and after hydrothermal ageing. EPR spectra (c) and UV-vis spectra (d) of the Cu3.7-SSZ-39-K catalyst before and after hydrothermal ageing.

Fig. 4. (a) Distribution of Al content at different sites in Co-SSZ-39-K and Co-SSZ-39-T. (b) Relative energies for the formation of different Cu species at τ sites. (c) H2-TPR profiles of fresh and hydrothermally aged Cu3.7-SSZ-39-K and Cu3.4-SSZ-39-T catalysts.

Scheme 1. Schematic illustration of the role of K+ and Na+ in directing Al site distribution during the crystallization of AEI zeolite.

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提高Cu-SSZ-39分子筛八元环骨架铝含量增强其低温氨选择催化还原性能

Enriching framework Al sites in 8-membered rings of Cu-SSZ-39 zeolite to enhance low-temperature ammonia selective catalytic reduction performance

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