Cu-KFI分子筛催化剂上甲烷直接转化高效连续合成甲醇

doi:10.1016/S1872-2067(26)65140-6

催化学报 ›› 2026, Vol. 88: 369-381.DOI: 10.1016/S1872-2067(26)65140-6

Cu-KFI分子筛催化剂上甲烷直接转化高效连续合成甲醇

张心怡^a, 董威辰^b, 曹毅^c, 周彩霞^b^,^*(), 郭家秀^a, 张海龙^a^,^*()

^a 四川大学碳中和未来技术学院, 四川成都 610064
^b 西南民族大学化学与环境学院, 四川成都 610041
^c 宁波大学材料科学与化学工程学院, 浙江宁波 315211

收稿日期:2026-01-07 接受日期:2026-02-27 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: hailongzhang@scu.edu.cn (张海龙),
cx_Zhou123@163.com (周彩霞).
基金资助:
国家自然科学基金(22302134);四川省归国留学人员科技活动项目(2024787-3)

Efficient continuous synthesis of methanol by direct methane conversion on Cu-KFI zeolite catalysts

Xinyi Zhang^a, Weichen Dong^b, Yi Cao^c, Caixia Zhou^b^,^*(), Jiaxiu Guo^a, Hailong Zhang^a^,^*()

^a College of Carbon Neutrality Future Technology, Sichuan University, Chengdu 610064, Sichuan, China
^b College of Chemistry & Environment, Southwest Minzu University, Chengdu 610041, Sichuan, China
^c School of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, Zhejiang, China

Received:2026-01-07 Accepted:2026-02-27 Online:2026-09-18 Published:2026-09-05
Supported by:
The National Natural Science Foundation of China(22302134);Funding for Science and Technology Activities for Returned Overseas Scholars in Sichuan Province(2024787-3)

摘要/Abstract

摘要：

甲烷作为天然气、页岩气和可燃冰的主要成分, 其高效转化合成高值化学品是能源化工领域的重要研究方向. 相较于传统的间接法合成路径, 甲烷直接转化制甲醇具有流程短、能耗低的显著优势, 是多相催化领域追求的理想反应. 然而, 甲烷分子具有高度对称的四面体结构和极高的C-H键离解能(~435 kJ/mol), 其活化非常困难; 同时, 目标产物甲醇的化学性质比甲烷更活泼, 在反应条件下极易发生深度氧化生成CO₂, 导致选择性较低. 近年来, 铜基分子筛催化剂在甲烷连续转化制甲醇反应中展现出巨大潜力, 但活性位点的本征结构与反应条件的协同调控机制仍需深入探究, 以实现高活性与高选择性的统一.
本研究以小孔KFI分子筛为载体, 通过等体积浸渍法制备了系列不同铜负载量的Cu-KFI催化剂, 并在连续的CH₄-H₂O-O₂反应体系中系统考察了其催化甲烷直接制甲醇的性能. 反应条件优化实验发现, 在550 °C调节O₂/H₂O比例, 对于0.34 wt%Cu负载量的催化剂, 甲醇时空产率可达~3120 mmol/mol_Cu/h, 甲醇选择性为71%. 稳定性测试表明, 该催化剂在含12.2%水蒸气的反应气氛中连续运行20 h, 甲醇产率稳定维持在~ 2000 mmol/mol_Cu/h, 选择性保持在~ 70%, 表现出稳定的催化活性. 为进一步解析反应机理, 采用H₂¹⁸O与¹⁶O₂同位素标记的程序升温表面反应技术揭示了O₂是反应的主要氧源, 同时水也作为氧化剂参与了反应. 反应分析表明, 当反应温度高于450 °C或氧气浓度超过1000 ppm时, 甲烷的深度氧化及重整等副反应显著加剧, 导致CO和CO₂大量生成. 提高水蒸气含量可有效抑制该过度氧化现象, 但在高氧浓度(如5000 ppm)下, 水的抑制作用失效. 结合高角环形暗场扫描透射电子显微镜、电子顺磁共振、紫外-可见光谱等表征手段与密度泛函理论计算, 揭示了Cu-KFI催化剂的构效关系: 低铜负载量有利于形成高度分散的孤立Cu位点, 该活性位对甲烷C-H键具有适中的活化能力, 同时能抑制甲醇的过度氧化; 而过高的铜负载量会导致CuO_x团簇乃至纳米颗粒的形成, 促进副反应发生.
综上, 本研究证实了低负载量的Cu-KFI催化剂在甲烷直接连续制甲醇反应中的巨大应用潜力, 并为理解连续催化CH₄-H₂O-O₂反应体系提供了深入的见解, 为设计高效铜基分子筛催化剂及优化连续流反应体系提供了重要的理论基础和实验依据.

关键词: 甲烷转化, 甲醇, Cu-KFI分子筛, 选择性, 过度氧化

Abstract:

The direct conversion of methane to methanol (DMTM) is a key technology for the efficient utilization of natural gas resources, which remains a significant challenge in heterogeneous catalysis. Here, we report the selective catalytic oxidation of methane over Cu-KFI zeolites in a continuous CH₄-H₂O-O₂ reaction system. A high methanol space-time yield of ~3120 mmol/mol_Cu/h with methanol selectivity of 71% is achieved with a low Cu loading of 0.34 wt% at 550 °C via regulating O₂/H₂O ratio. Such a high-performance catalyst further shows a highly-stable catalytic activity in a longtime continuous operation under high water content (~12.2%). The isotope labelling with H₂¹⁸O and ¹⁶O₂ reveals that O₂ is the dominant oxygen source while water is also the oxidant for methane selective oxidation. Reaction analysis indicates that high reaction temperatures (> 450 °C) and high O₂ concentrations (> 1000 ppm) lead to an apparent overoxidation and side reactions of methane into CO₂ and CO. Fortunately, this phenomenon can be inhibited via increasing water vapor content, which, however, is ineffective at higher O₂ concentrations (e.g., 5000 ppm). Besides, the present study also reveals that the catalytic performance of Cu-KFI zeolites is related to both the Cu site sizes and ring window sizes based on the experimental results and density functional theory calculations. This work evidences a great potential of Cu-KFI zeolites with low Cu loadings in methane-selective conversion to methanol and provides an insightful understanding of continuous catalytic CH₄-H₂O-O₂ reaction system.

Key words: Methane conversion, Methanol, Cu-KFI zeolite, Selectivity, Overoxidation

张心怡, 董威辰, 曹毅, 周彩霞, 郭家秀, 张海龙. Cu-KFI分子筛催化剂上甲烷直接转化高效连续合成甲醇[J]. 催化学报, 2026, 88: 369-381.

Xinyi Zhang, Weichen Dong, Yi Cao, Caixia Zhou, Jiaxiu Guo, Hailong Zhang. Efficient continuous synthesis of methanol by direct methane conversion on Cu-KFI zeolite catalysts[J]. Chinese Journal of Catalysis, 2026, 88: 369-381.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65140-6

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Fig. 1. (a) Continuous DMTM on 0.5%Cu-KFI zeolite (actual Cu loading = 0.34 wt%) upon elevating reaction temperatures from 300 to 600 °C. Bars and orange stars refer to the STY of products (mmol/molCu/h) and methanol selectivity (%), respectively. (b) The methanol yield and selectivity of Cu-KFI samples as a function of copper loading. Reaction conditions: 100 mg catalyst, total flow rate of 50 mL/min; 80% CH4, 500 ppm O2, 4.2% H2O and Ar balance. (c) Methanol yield (mmol/molCu/h) and selectivity (%) of 0.5%Cu-KFI and 1%Cu-KFI samples in continuous DMTM with different water contents. Reaction conditions: 100 mg catalyst, total flow rate = 50 mL/min; 80 % CH4, 500 ppm O2, 4.2% or 12.2% H2O; reaction temperature = 550 °C. (d) The yields of COx and H2 products in (c) reaction systems. (e) Continuous DMTM over Cu-KFI zeolites with different Cu loadings. Reaction conditions: 80% CH4, 4.2% H2O and 100-10000 ppm O2, reaction temperature of 450 °C.

Fig. 2. Catalytic stability of 0.5%Cu-KFI catalyst in continuous DMTM. Reaction conditions: 100 mg catalyst, total flow rate = 50 mL/min; 80% CH4, 1000 ppm O2, 12.2% H2O; reaction temperature = 500 °C. Note: No regeneration treatments were performed after leaving the reaction for 15 d.

Fig. 3. (a) Temperature-programmed surface reactions (TPSR) of continuous DMTM on 0.5%Cu-KFI with isotopically labelled system of CH4 + H218O + O2. Reaction conditions: 100 mg catalyst, total flow rate = 50 mL/min; 80% CH4, 4.2% H218O, 500 ppm O2, Ar as the balance. (b) The ratio of dihydrogen to methanol in continuous DMTM over 0.5%Cu-KFI zeolite at different reaction temperatures. Reaction conditions: 100 mg catalyst, total flow rate = 50 mL/min; 80% CH4, 4.2% H2O, 500 ppm O2. (c) The product yields in continuous DMTM reaction over Cu-KFI zeolites. Reaction conditions: 80% CH4, 4.2% H2O, 100-10000 O2, reaction temperature of 450 °C. (d) The ratio of dihydrogen to methanol in continuous DMTM over 0.5%Cu-KFI zeolite under the reaction conditions of (c).

Fig. 4. The representative HAADF-STEM images of 0.5%Cu-KFI (a-c) and 1%Cu-KFI (d-f) samples. (c) and (f) energy distribution maps obtained through image-matrix transformation for the red boxes in (b) and (e). (g) Element mappings of Cu, O and Al in 1%Cu-KFI.

Fig. 5. (a) 29Si MAS NMR spectrum of the as-prepared KFI zeolite. EPR results (b), UV-Vis spectra (c) and H2-TPR results (d) of Cu-KFI zeolites with different Cu loadings. (e) FTIR spectra of Cu-KFI zeolites using KFI zeolite as the background. (f) In-situ FTIR spectra of Cu-KFI zeolites for NO adsorption at 30 °C.

Fig. 6. (a) The selectivities of methanol and COx as a function of Cu loadings on KFI and CHA [37] zeolites. (b) The structure of KFI zeolite and the size of ring windows.

Fig. 7. The energy diagram for the reaction path of methane-steam to methanol on [Cu-OH]+ and hydrated [Cu(OH2)-OH]+ active sites hosted on 6MR in KFI zeolite.

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Cu-KFI分子筛催化剂上甲烷直接转化高效连续合成甲醇

Efficient continuous synthesis of methanol by direct methane conversion on Cu-KFI zeolite catalysts

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[1]	高梓皓, 黄凯, 徐庆玲, 王鑫, 刘志成, 邵斌, 胡军. 催化微环境调控促进高效CO₂捕集与原位乙烷氧化脱氢制乙烯[J]. 催化学报, 2026, 88(9): 322-334.
[2]	魏耀文, 王建伟, 郭皓, 班涛, 岳玉峰, 胡地, 黄海保. 缺陷UiO-66催化剂在温和条件下实现甲烷高选择性氧化制乙酸[J]. 催化学报, 2026, 88(9): 356-368.
[3]	Sathi Chatterjee, 李红梅, 刘康, 林璋, 柴立元, 刘敏. 二维(2D)材料上的单原子催化剂用于光催化CO₂还原: 基础、设计与新兴策略[J]. 催化学报, 2026, 88(9): 86-128.
[4]	张家雨, 王昆, 于晶露, 徐凯洋, 杨璐, 饶佳丽, 宋树芹, 王毅. Mn掺杂调控NiCo LDH活性位点用于H₂O₂与甲酸盐的节能耦合电合成[J]. 催化学报, 2026, 88(9): 307-321.
[5]	王松玲, 黄安华, 尹风星, 卢瑞祥, 刘文刚, 张云, 乔波涛. 原位合成双氧水用于甲烷高选择性氧化制甲醇[J]. 催化学报, 2026, 88(9): 347-355.
[6]	何雯鑫, 鲁元红, 管晨曦, 侯晓慧, 黄瑞, 邓德会. 勃姆石晶格羟基介导水为氢源的肉桂醛选择性加氢[J]. 催化学报, 2026, 87(8): 386-395.
[7]	丁扬, 陆义桢, 余天荣, 张明睿, 赵睿, 杨睿杰, 李其鑫, 吴仕群, 张金龙. 光驱动费托合成中双路径策略实现高选择性烃类产物制备[J]. 催化学报, 2026, 87(8): 22-46.
[8]	秦家祥, 张松培, 李星局, 陈鑫泰, 赵佳, 牟效玲, 宋宪根, 严丽, 林荣和, 丁云杰. 丁二烯半加氢反应中Pd-Ag纳米催化剂结构-选择性耦合关系解析[J]. 催化学报, 2026, 87(8): 342-352.
[9]	Jiyeon Lee, Muhammad Irshad, Wonjoong Yoon, Jaehoon Kim. 高压开关: 将二氧化碳加氢产物从碳氢化合物转向羧酸和醇类[J]. 催化学报, 2026, 87(8): 70-86.
[10]	李天春, 刘天阳, 荆宇. 铜基催化剂上愈创木酚加氢脱氧反应选择性的结构起源[J]. 催化学报, 2026, 87(8): 376-385.
[11]	王子行, 仲伟, 李思齐, 孙斌, 蓝浩, 张晓雨, 王新, 陈煜, 艾轩. C-C键断裂抑制和中间体吸附增强共同促进乙二醇在银钯空心纳米立方体上的选择性电氧化[J]. 催化学报, 2026, 86(7): 191-200.
[12]	敖志锋, 何文轩, 滕志学, 刘熊唯, 沈志刚. 溶剂工程与微波辐射协同促进高结晶度PET低温催化解聚[J]. 催化学报, 2026, 86(7): 125-136.
[13]	李婧宇, 徐艺军. 光催化环氧化合物的区域选择性开环反应[J]. 催化学报, 2026, 85(6): 34-46.
[14]	陈兰兰, 圣利, 周亚男, 罗其全, 李震宇, 张文华, 杨金龙. Ni₁-MoS₂单原子催化剂用于CO₂加氢制甲醇的优越性: 密度泛函理论与微观动力学研究[J]. 催化学报, 2026, 85(6): 143-152.
[15]	何邢晨, 邵俊辉, 李娜君, 陈冬赟, 李华, 徐庆锋, 王浩志, 路建美. 压电增强氢键网络调控氟化氮化碳实现CO₂还原的100% CO选择性[J]. 催化学报, 2026, 85(6): 130-142.