纯无机体系下超薄纳米ZSM-5分子筛的合成

doi:10.1016/S1872-2067(26)65176-5

催化学报 ›› 2026, Vol. 89: 464-476.DOI: 10.1016/S1872-2067(26)65176-5

纯无机体系下超薄纳米ZSM-5分子筛的合成

赵嘉琦^a, 申培育^a, 覃正兴^a^,^*(), Camille Longue^b, Nourrdine Chaouati^b, 张锐哲^b, 陈晓^c, Shunsuke Asahina^d^,^e, Natsuko Asano^d^,^e, Gabriel Rueff^b, Eddy Dib^b, 孙洪满^a, 康利彬^g, 王久江^h, 赵红娟^h, 刘宏海^h, 徐舒涛ⁱ, Ludovic Pinard^b, 阎子峰^a, Svetlana Mintova^a^,^b^,^*()

^a中国石油大学(华东)化学化工学院,重质油全国重点实验室,山东青岛 266580,中国
^b卡昂诺曼底大学,卡昂国立高等工程师学院, 法国国家科学研究中心, 催化和光谱化学实验室,卡昂,法国
^c清华大学化学工程系,绿色反应工程与工艺北京市重点实验室,北京 100084,中国
^d日本电子株式会社(JEOL Ltd.)应用规划组,东京,日本
^e东北大学先进材料多学科研究所,先进材料分析共创研究中心,仙台,日本
^f东京都市大学环境应用化学系,城市环境科学研究生院,东京,日本
^g山东科翰硅源新材料有限公司,山东临沂 276000,中国
^h中国石油天然气股份有限公司石油化工研究院,北京 100195,中国
ⁱ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,中国

收稿日期:2026-02-10 接受日期:2026-04-07 出版日期:2026-10-18 发布日期:2026-09-01
通讯作者: *电子信箱: zhengxing.qin@upc.edu.cn (覃正兴),
svetlana.mintova@ensicaen.fr (S. Mintova).
基金资助:
国家自然科学基金(22472202);国家自然科学基金(22178389);辽宁省国际联合实验室项目(2024JH2/102100005);中国石油天然气集团公司(KYWX-22-012);中国石油天然气集团公司(KYWX-22-017);中国石油天然气集团公司(KYWX-24-003)

Ultrathin ZSM-5 zeolite nanocrystals synthesized from purely inorganic precursors

Jiaqi Zhao^a, Peiyu Shen^a, Zhengxing Qin^a^,^*(), Camille Longue^b, Nourrdine Chaouati^b, Ruizhe Zhang^b, Xiao Chen^c, Shunsuke Asahina^d^,^e, Natsuko Asano^d^,^e, Gabriel Rueff^b, Eddy Dib^b, Hongman Sun^a, Libin Kang^g, Jiujiang Wang^h, Hongjuan Zhao^h, Honghai Liu^h, Shutao Xuⁱ, Ludovic Pinard^b, Zifeng Yan^a, Svetlana Mintova^a^,^b^,^*()

^aState Key Laboratory of Heavy Oil Processing, College of Chemistry and Chemical Engineering, China University of Petroleum (East China), Qingdao 266580, Shandong, China
^bUniversité de Caen Normandie, ENSICAEN, CNRS, LCS,Laboratoire Catalyse et Spectrochimie, 14000 Caen, France
^cBeijing Key Laboratory of Green Chemical Reaction Engineering and Technology, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
^dSM Application planning group, JEOL Ltd., Akishima, Tokyo 196-8558, Japan
^eAdvanced Material Analysis Co-creation Research Center, Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Sendai, Japan
^fDepartment of Applied Chemistry for Environment, Graduate School of Urban Environmental Sci-ences, Tokyo Metropolitan University, 1-1 Minami-Osawa, Hachioji, Tokyo 192-0397, Japan
^gShandong Kehan Silicon Source New Material Co.,Ltd. Linyi 276000, China
^hPetrochemical Research Institute, PetroChina Company Limited, Beijing 100195, China
ⁱNational 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

Received:2026-02-10 Accepted:2026-04-07 Online:2026-10-18 Published:2026-09-01
Contact: *E-mail:zhengxing.qin@upc.edu.cn(Z. Qin),svetlana.mintova@ensicaen.fr(S. Mintova).
Supported by:
National Natural Science Foundation of China(22472202);National Natural Science Foundation of China(22178389);Liaoning International Joint Laboratory Project(2024JH2/102100005);PetroChina(KYWX-22-012);PetroChina(KYWX-22-017);PetroChina(KYWX-24-003)

摘要/Abstract

摘要：

超薄纳米分子筛因其更高的晶面暴露度和更优异的分子扩散性能, 在催化、吸附及分离领域展现出独特应用优势. 其中, ZSM-5分子筛凭借优异的择形催化性能, 其超薄纳米片结构的制备与应用研究备受关注. 然而, 目前ZSM-5纳米片的制备多依赖有机模板剂或额外添加剂, 存在工艺复杂、成本偏高及绿色放大困难等瓶颈问题. 采用无模板、无添加剂策略合成超薄纳米分子筛, 对于实现其可持续规模化生产具有重要现实意义, 也是该领域长期以来亟待突破的技术难点. 为此, 本研究以焙烧后的纳米Silicalite-1为晶种, 在不使用有机模板剂、氟化物及其他任何添加剂的前提下, 成功合成出b轴厚度薄至10 nm的ZSM-5纳米片.

本研究系统探究了不同状态(含晶种母液、未焙烧及焙烧后)的纳米Silicalite-1分子筛在纯无机体系中的诱导结晶行为, 证实晶种可以经过高温焙烧直接改变其碱性溶解能力, 进而调控纳米ZSM-5晶体的微观生长路径; 同时明确四丙基铵离子在晶体形貌调控中发挥关键作用. 换言之, 晶种中模板剂的保留状态及其存在形式, 会显著影响晶种表面的溶解过程与二次成核行为. 本研究进一步揭示了晶种的双重作用机制: 在碱性条件下, 焙烧后的晶种首先作为成核中心启动成核过程, 随后发生晶面选择性溶解; 其中, (010)晶面与(101)晶面的稳定性差异调控生长单元的各向异性附着, 进而引导晶体沿c轴定向生长并抑制其沿b轴增厚. 基于上述发现, 本文提出“利用晶种溶解性调控晶体取向生长”机制, 通过优化合成参数, 成功制备出b轴厚度低至10 nm的纳米片状ZSM-5分子筛. 烷烃裂解及甲醇制烯烃等催化性能测试证实, 所制备的ZSM-5纳米片具有更优异的本征催化活性和传质性能; 研究发现, 纳米尺度下分子筛细微的形貌差异可转化为显著的产物选择性差异, 突显了结晶化学与催化性能之间的紧密关联, 以及形貌调控在分子筛催化性能优化中的重要作用.

综上, 本文提出的强化晶种溶解、诱导取向生长合成路线, 不仅为无模板、无氟条件下超薄纳米ZSM-5分子筛的构筑提供了新的研究思路, 同时表明晶种处理方式可作为调控分子筛形貌与催化性能的重要手段. 该策略有望拓展至其他二维分子筛材料的制备及绿色催化过程, 为高性能超薄纳米分子筛材料的可持续合成提供方法学支撑, 也为相关领域的基础研究与工业应用奠定基础.

关键词: ZSM-5纳米片, 晶种辅助法, Silicalite-1, 形貌控制, 甲醇制烯烃

Abstract:

Ultrathin zeolite nanocrystals offer distinct advantages in catalysis, adsorption, and separation due to their enhanced exposure of crystal facets and improved molecular diffusion. The synthesis of ultrathin zeolites via template-free and additive-free approaches is highly desirable for sustainable and scalable production, yet remains a longstanding challenge. ZSM-5 nanosheets with a b-axis thickness as small as 10 nm were synthesized via seed-assisted crystallization in a purely inorganic aluminosilicate medium, without the use of organic templates, fluoride, or other additives. The influence of Silicalite-1 seed treatment history, a previously overlooked parameter on ZSM-5 crystallization was systematically investigated. The presence or absence of occluded organic template within the seeds critically modulates crystal morphology by affecting surface dissolution and secondary nucleation at the seed surface. Catalytic testing in methanol conversion indicates that, although structural variations due to nanoscale dimensions are minimal, differences in crystal morphology significantly influence catalytic selectivity. These findings underscore the crucial role of morphology control in tailoring the catalytic performance of zeolites.

Key words: ZSM-5 nanosheets, Seed assisted synthesis, Silicalite-1 zeolite, Morphology control, Methanol to olefins

赵嘉琦, 申培育, 覃正兴, Camille Longue, Nourrdine Chaouati, 张锐哲, 陈晓, Shunsuke Asahina, Natsuko Asano, Gabriel Rueff, Eddy Dib, 孙洪满, 康利彬, 王久江, 赵红娟, 刘宏海, 徐舒涛, Ludovic Pinard, 阎子峰, Svetlana Mintova. 纯无机体系下超薄纳米ZSM-5分子筛的合成[J]. 催化学报, 2026, 89: 464-476.

Jiaqi Zhao, Peiyu Shen, Zhengxing Qin, Camille Longue, Nourrdine Chaouati, Ruizhe Zhang, Xiao Chen, Shunsuke Asahina, Natsuko Asano, Gabriel Rueff, Eddy Dib, Hongman Sun, Libin Kang, Jiujiang Wang, Hongjuan Zhao, Honghai Liu, Shutao Xu, Ludovic Pinard, Zifeng Yan, Svetlana Mintova. Ultrathin ZSM-5 zeolite nanocrystals synthesized from purely inorganic precursors[J]. Chinese Journal of Catalysis, 2026, 89: 464-476.

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https://www.cjcatal.com/CN/Y2026/V89/I10/464

图/表 6

Fig. 1. SEM (a-j) and TEM (k-o) images showing the crystal size and morphology of ZSM-5 zeolites synthesized using Silicalite-1 seeds in the presence or absence of tetrapropylammonium cations: (a,f,k) Z1 zeolite synthesized using S1; (b,g,l) Z2 zeolite synthesized using S2; Z3 zeolite synthesized using S3 (c,h,m); Z4 (d,i,n) and Z5 (e,j,o) zeolites synthesized using S4 and S5, respectively.

Fig. 2. HAADF-STEM images and corresponding elemental maps of ZSM-5 zeolite samples: Z1 (a), Z2 (b), Z3 (c), Z4 (d), and Z5 (e).

Table 1 Acidic properties and catalytic descriptor values obtained from n-hexane and 3-methylpentane cracking (initial activity, turnover frequency, paraffin-to-olefin ratio, and constraint index).

	[PyH⁺] ^a	[PyL] ^a	EFAls (δ = 0) ^b	A₀ (n-hex) ^c	TOF (n-hex) ^c	P/O (n-hex) ^c	A₀ (3-MP) ^d	TOF (3-MP) ^d	P/O (3-MP) ^d	CI ^e
Unit	µmol·g_cat^-1	µmol·g_cat^-1	%	mmol·h^-1·g_cat^-1	h^-1	mol/mol	mmol·h^-1·g_cat^-1	h^-1	mol/mol
Z_ref	335	21	4.6	129	384	0.52	169	504	0.20	0.76
Z1	305	135	13.5	246	1001	0.54	384	1560	0.15	0.46
Z2	318	186	14.1	315	1000	0.42	770	2444	0.14	0.41
Z3	357	181	15.9	329	1000	0.46	738	2242	0.14	0.45

Fig. 3. (a) MeOH and DME conversion over the TOS. Cumulative products selectivity and E/P ratio at 100% conversion of MeOH and DME at the initial time (b), 100% conversion before deactivation (c), and 18%-20% iso-conversion and deactivation conditions (d). Black crosses corresponding to conversions on products selectivity. Reaction conditions: 723 K, WHSV: 2.1 g CH3OH gcat-1 h-1; N2/CH3OH = 23 and Ptotal =1 atm.

Fig. 4. Schematic illustration of hydroxyl group adsorption on (010) (a,c) and (100) (b,d) surfaces of MFI zeolite structure. The adsorption modeling was performed without (a,b) and with (c,d) TPA+ occluded.

Fig. 5. SEM (a,d,g) and TEM (b,c,e,f,h,i) images of ZSM-5 zeolites synthesized with varied OH-/SiO2 ratios following the procedure applied for Z3 sample: (a,b,c) Z3-0.33, (d,e,f) Z3-0.3, (g,h,i) Z3-0.25; the suffix corresponds to the respective OH-/SiO2 ratios. (j) SEM and (k,l) TEM images of ZSM-5 zeolite synthesized using 20 nm-sized calcined Silicalite-1 as seeds.

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纯无机体系下超薄纳米ZSM-5分子筛的合成

Ultrathin ZSM-5 zeolite nanocrystals synthesized from purely inorganic precursors

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