通过介孔结构设计强化丙烷耦合CO2芳构化中CO2介导的芳烃循环

doi:10.1016/S1872-2067(26)64950-9

催化学报 ›› 2026, Vol. 84: 226-235.DOI: 10.1016/S1872-2067(26)64950-9

通过介孔结构设计强化丙烷耦合CO₂芳构化中CO₂介导的芳烃循环

杨璐源^a^,¹, 杨镒涛^a^,¹, 杨敏^a, 秦玉才^b, 张晓欣^b, Saeed Soltanali^e, 刘坚^a(), 宋卫余^a^,^c^,^d()

^a 中国石油大学(北京)理学院, 重质油国家重点实验室, 北京市油气光学检测重点实验室, 北京 102249, 中国
^b 辽宁石油化工大学石油化工学院, 辽宁抚顺 113001, 中国
^c 中国石油大学(北京)克拉玛依校区, 重质油国家重点实验室克拉玛依分室, 新疆克拉玛依 834000, 中国
^d 山东石油化工学院碳中和研究所, 山东东营 257061, 中国
^e 石油工业研究院, 催化技术开发部, 德黑兰, 伊朗

收稿日期:2025-09-07 接受日期:2025-10-28 出版日期:2026-05-18 发布日期:2026-04-16
通讯作者: *电子信箱: songwy@cup.edu.cn (宋卫余),
liujian@cup.edu.cn (刘坚).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22035009);国家自然科学基金(22178381);国家重点研发计划(2021YFA1501301);国家重点研发计划(2021YFC2901100);山东省重点研发计划(2024CXGC010410);碳中和研究所基金(CNIF20240106)

Boosting CO₂-mediated aromatic cycle via mesoporous design in propane aromatization catalysis

Luyuan Yang^a^,¹, Yitao Yang^a^,¹, Min Yang^a, Yucai Qin^b, Xiaoxin Zhang^b, Saeed Soltanali^e, Jian Liu^a(), Weiyu Song^a^,^c^,^d()

^a State Key Laboratory of Heavy Oil Processing, Key Laboratory of Optical Detection Technology for Oil and Gas, China University of Petroleum (Beijing), Beijing 102249, China
^b School of Petrochemical Engineering, Liaoning Petrochemical University, Fushun 113001, Liaoning, China
^c State Key Laboratory of Heavy Oil Processing at Karamay, China University of Petroleum (Beijing) at Karamay, Karamay 834000, Xinjiang, China
^d Carbon Neutrality Research Institute, Shandong Institute of Petroleum and Chemical Technology, Dongying 257061, Shandong, China
^e Catalysis Technologies Development Division, Research Institute of Petroleum Industry (RIPI), Tehran 14665-1998, Iran

Received:2025-09-07 Accepted:2025-10-28 Online:2026-05-18 Published:2026-04-16
Contact: * E-mail: songwy@cup.edu.cn (W. Song),
liujian@cup.edu.cn (J. Liu).
About author:¹Contributed equally to this work.
Author contributions
The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript.
Supported by:
National Natural Science Foundation of China(22035009);National Natural Science Foundation of China(22178381);National Key R&D Program of China(2021YFA1501301);National Key R&D Program of China(2021YFC2901100);Key R&D Program of Shandong Province, China(2024CXGC010410);Carbon Neutrality Research Institute Fund(CNIF20240106)

摘要/Abstract

摘要：

轻质烷烃催化芳构化是将页岩气衍生物转化为高值芳烃的关键途径. 然而传统丙烷脱氢芳构化(PDA)存在积碳速率快、苯-甲苯-二甲苯(BTX)选择性低等固有缺陷. 虽然二氧化碳(CO₂)共进料被广泛认为是抑制积碳、提升芳烃收率的有效策略, 但其对传质行为的影响机制尚不明确. 值得注意的是, CO₂可能诱导生成大分子动力学直径产物的副反应路径, 加剧微孔分子筛内的扩散限制, 最终影响产物选择性. 尽管现有研究通过活性位点工程和反应路径调控提升芳烃选择性, 但传统催化剂设计普遍忽视反应-传质协同机制.

本工作使用三乙胺、氢氧化钠及复配碱液(四丙基氢氧化铵/氢氧化钠)分别对ZSM-5分子筛进行刻蚀, 并采用浸渍法负载镓(Ga)活性组分, 制备了一系列具有不同介孔孔径及Al_F分布的Ga负载型ZSM-5催化剂. X-射线吸收近边能谱、氢气程序升温还原及Ga 2p_3/2X射线光电子能谱证实, 镓物种主要以(GaO)_x⁺形式存在. 性能测试结果表明, 具有较小介孔(3.7 Å)的Ga/T-ZSM-5催化剂仅获得18%的BTX选择性, 而具备较大介孔(8.9 Å)的Ga/M-ZSM-5实现57%的BTX选择性, 且积碳速率相较于小介孔催化剂显著下降. 基于¹³CO₂同位素示踪、质谱、脉冲反应及原位傅里叶变换红外光谱表征, 证实丙烷-CO₂共芳构化(PCA)遵循双循环烃池机制: 部分CO₂嵌入长链烃中形成含氧中间体, 经脱水环化等多个步骤参与芳烃循环, 最终生成芳烃产物. 值得注意的是, CO₂虽通过促进芳烃循环提升产物收率, 但高碳物种浓度增加导致沸石孔道扩散受限. 反应后催化剂紫外-可见光谱等表征揭示, 小分子量多环芳烃, 以及大分子芳香聚合物严重阻碍传质过程. 解决该问题的关键在于介孔结构的协同调控作用: 介孔结构能够优化分子筛孔道连通性, 有效缩短扩散路径, 加速芳烃产物脱附, 还能够通过缓解产物积聚显著抑制积碳生成. 零长柱色谱测试表明, Ga/M-ZSM-5具有最突出的扩散性能. 当CO₂分压提升13%时, 具有最大介孔的Ga/M-ZSM-5芳烃选择性增幅达16%(高于小孔径对照组), 这证实介孔加速的扩散过程与CO₂对于芳烃循环的促进作用形成深度协同: 介孔结构打破原有扩散限制, 使CO₂强化芳构化的正效应得以充分发挥.

综上, 本研究通过在ZSM-5骨架中构建介孔网络, 使CO₂介导的芳构化强化与产物扩散达成动态协同, 最终实现芳烃选择性提升. 该发现不仅为开发具有高BTX选择性的双功能催化剂提供了设计思路, 还强调了传质过程在催化反应中的关键作用.

关键词: 碱处理, 介孔结构, 芳烃循环, CO₂协同, 传质

Abstract:

Understanding how structure regulates reaction pathways is critical for the rational design of propane (C₃H₈)-coupled CO₂ aromatization (PCA) catalysts. Here, alkaline treatments precisely tuned zeolite pore size (3.8 → 8.9 Å) and Al distribution, boosting benzene, toluene, and xylene selectivity from 18% (Ga-T-ZSM-5) to 57% (Ga/M-ZSM-5). Mechanistic studies, including ¹³CO₂ isotope tracing, mass spectrometry, pulse reactions, and in-situ Fourier transformed infrared confirmed that this reaction follows a dual-cycle hydrocarbon pool mechanism. Critically, CO₂ was inserted into the hydrocarbon pool, generating oxygenated intermediates that underwent dehydration and cyclization to form aromatic intermediate species, thereby accelerating the aromatic cycle. The intensified aromatic cycle generated bulky polycyclic aromatics that may obstruct micropores under diffusion-limited conditions. Introducing mesopores alleviated such accumulation by facilitating rapid molecular transport of these high-carbon species. The synergy between the CO₂-mediated hydrocarbon pool pathway and mesopore-enhanced diffusion of aromatic intermediates significantly boosted aromatic selectivity. This interplay provides fundamental insights for future catalyst design.

Key words: Alkaline treatments, Mesoporous structure, Aromatic cycle, CO₂ synergy, Mass transfe

杨璐源, 杨镒涛, 杨敏, 秦玉才, 张晓欣, Saeed Soltanali, 刘坚, 宋卫余. 通过介孔结构设计强化丙烷耦合CO₂芳构化中CO₂介导的芳烃循环[J]. 催化学报, 2026, 84: 226-235.

Luyuan Yang, Yitao Yang, Min Yang, Yucai Qin, Xiaoxin Zhang, Saeed Soltanali, Jian Liu, Weiyu Song. Boosting CO₂-mediated aromatic cycle via mesoporous design in propane aromatization catalysis[J]. Chinese Journal of Catalysis, 2026, 84: 226-235.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)64950-9

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Fig. 1. XRD patterns (a), pore size distribution curves (b), and nitrogen adsorption-desorption isotherms (c) of M-ZSM-5, N-ZSM-5, T-ZSM-5, ZSM-5, and Ga/ZSM-5. (d) -OH FTIR spectra of samples. P = 1 atm, pCO2:pC3H8:pN2 = 1:1:18, total flow rate: 30 mL/min, T = 150 °C.

Fig. 2. The SEM and TEM spectra of Ga/T-ZSM-5 (a1-a4), Ga/ZSM-5 (b1-b4), Ga/N-ZSM-5 (c1-c4), and Ga/M-ZSM-5 (d1-d4).

Fig. 3. Acid content measured by NH3-TPD (a), Py-IR (b), and the difference between the two measurement methods (c) in zeolite samples. (d) UV-vis-DRS spectra of Co(II) ions for 27Al MAS NMR spectra of ZSM-5, T-ZSM-5, N-ZSM-5, and M-ZSM-5. (e) Schematic diagram of Al-pairs and Single Al adsorbed the product benzene and the intermediate cyclopentanone.

Fig. 4. (a-d) Product distribution (bars) and C3H8 and CO2 conversion under 550 °C, p = 1 atm, C3H8: CO2: N2 = 1:1:1, WHSV= 5.24 h-1 (black and red points, respectively). CO2-TPD (e) and C3H8-TPD (f) profiles of samples.

Fig. 5. (a-d) Mass detection of benzene in the early reaction stage when a propane pulse is injected at 400 °C. (e) Mass detection of benzene when a C3H8/CO2 pulse is injected at 400 °C. (f) In-situ FTIR of Ga/ ZSM-5 under increasing temperature (100-400 °C), p = 1 atm, C3H8: CO2: N2 = 1:1:18, WHSV = 31.72 h-1. (g) In-situ MS of Ga/M-ZSM-5 under 550 °C, 1 atm, C3H8: CO2: N2 = 1:1:1, WHSV = 50.6 h-1. 13C isotope tracing MS spectra of pentanoic acid (h) and cyclopentenone (i) of 13CO2 and 12CO2 during the coupling reaction, 0.05 g Ga/M-ZSM-5, T = 400 °C, p = 1 atm, C3H8: 12CO2(13CO2): N2 = 1.5:1.5:10, WHSV = 22.07 h-1. (j) Schematic diagram of the double cycle involving CO2 in PCA.

Fig. 6. UV-vis spectra (a) and ZLC desorption curve (b) of benzene on the sample at 230 °C. (c) Benzene content with the change in partial pressure of CO2 in C3H8 coupling CO2 aromatization, 0.05 g catalyst, T = 550 °C, P = 0.1 MPa, pC3H8:pCO2 = 5:x:10-x, (x = 5, 6, 8, 10), N2 as an equilibrium gas, total flow rate: 15 mL/min.

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通过介孔结构设计强化丙烷耦合CO₂芳构化中CO₂介导的芳烃循环

Boosting CO₂-mediated aromatic cycle via mesoporous design in propane aromatization catalysis

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