光热协同驱动SrTiOx负载CuCo催化CO2-CH4和H2O共转化制备C2含氧化合物

doi:10.1016/S1872-2067(24)60026-4

催化学报 ›› 2024, Vol. 61: 164-178.DOI: 10.1016/S1872-2067(24)60026-4

光热协同驱动SrTiO_x负载CuCo催化CO₂-CH₄和H₂O共转化制备C₂含氧化合物

朱彦儒^a^,^b, 张志军^a, 张健^a^,^b^,^*(), 蒋双江^a, 安哲^a^,^b, 宋红艳^a, 舒心^a, 习卫^c, 郑黎荣^d, 何静^a^,^b^,^*()

^a北京化工大学化工资源工程国家重点实验室, 北京 100029
^b衢州资源化工创新研究院, 浙江衢州 324000
^c天津理工大学天津市先进功能多孔材料重点实验室/电子显微镜研究中心, 天津 300384
^d中国科学院高能物理研究所, 北京 100049

收稿日期:2024-02-18 接受日期:2024-03-28 出版日期:2024-06-18 发布日期:2024-06-20
通讯作者: * 电子信箱: hejing@buct.edu.cn (何静), zhangjian450924@buct.edu.cn (张健).
基金资助:
国家重点研发项目(2021YFB3801602);国家自然科学基金(22288102)

Photo-thermal cooperation for the conversion of CO₂ and CH₄ with H₂O to C₂ oxygenates over SrTiO_x supported CuCo

Yanru Zhu^a^,^b, Zhijun Zhang^a, Jian Zhang^a^,^b^,^*(), Shuangjiang Jiang^a, Zhe An^a^,^b, Hongyan Song^a, Xin Shu^a, Wei Xi^c, Lirong Zheng^d, Jing He^a^,^b^,^*()

^aState Key Laboratory of Chemical Resource Engineering, & Beijing Advanced Innovation Center for Soft Matter Science and Engineering, Beijing University of Chemical Technology, Beijing 100029, China
^bQuzhou Institute for Innovation in Resource Chemical Engineering, Quzhou 324000, Zhejiang, China
^cCenter for Electron Microscopy and Tianjin Key Laboratory of Advanced Functional Porous Materials, Tianjin University of Technology, Tianjin 300384, China
^dInstitute of High Energy Physics, the Chinese Academy of Sciences, Beijing 100049, China

Received:2024-02-18 Accepted:2024-03-28 Online:2024-06-18 Published:2024-06-20
Contact: * E-mail: jinghe@263.net.cn (J. He), zhangjian450924@buct.edu.cn (J. Zhang).
Supported by:
National Key R&D Program of China(2021YFB3801602);National Natural Science Foundation of China(22288102)

摘要/Abstract

摘要：

催化转化CO₂为乙醇、乙醛等高值C₂含氧化合物是一个具有科学意义和经济价值的化学过程. 然而, 由于碳氧键活化难、多电子(≥10)转移过程复杂以及C-C偶联动力学缓慢等问题, 导致该过程的反应效率低. CO₂因热力学稳定、动力学惰性, 其加氢活化通常是强吸热过程(如CO₂活化成CO的ΔH_298K = 42.1 kJ mol^‒1), 因此需要在一定温度下才能获得满意的CO₂转化率. 与此同时, CH₄作为碳化学价态最低的化合物, 其氧化过程与CO₂的还原过程可以耦合, 共同转化为高值化学品, 同样受到了广泛关注. 但CH₄的活化同样需要高温等苛刻条件, 因此, 在温和条件下共转化CO₂和CH₄, 选择性构建高值C₂含氧化合物, 是一个重要且具有挑战性的研究方向.
本文提出利用光外场和水活化策略, 即利用光解水产生的活性氢和活性氧物种, 在温和条件下实现CO₂和CH₄的高效、高选择性活化及共转化. 光照下, 在钛酸锶(SrTiO_x)负载的具有丰富Cu-Co界面的催化剂上, 光解水产生的活性氢和活性氧物种, 分别活化CO₂的碳氧键和CH₄的碳氢键, 在Cu和Co位点上分别形成*CH_xO和*CH₃物种, 进而通过C-C偶联高效生成C₂含氧化合物. 在200 °C和光照条件下, C₂含氧化合物(CH₃CHO和CH₃CH₂OH)的生成速率高达2.05 mmol g^‒1 h^‒1, 同时产物选择性> 86%. 同位素标记、红外光谱示踪的原位反应和催化实验结果表明, 紫外光激发下, SrTiO_x上的金属位点促进了光催化水裂解, 生成活性氢和活性氧物种(该过程为整个反应的决速步骤). 活性氢物种使吸附在SrTiO_x上的CO₂活化并转化为CO; 随后, 在Cu^I/Cu⁰对上, CO加氢生成*CH_xO中间体. 另一方面, 在Co位点上, CH₄与活性氧物种发生反应, 被活化为*CH₃中间体. 最后, *CH_xO与*CH₃两种中间体在CuCo界面处发生C-C偶联反应, 进而形成C₂含氧化合物. 与传统的热催化下的CO₂和CH₄共转化过程相比, 光热协同策略使该反应温度降低了超过600 °C, 并且反应活化能降低了约12 kJ mol^‒1, 表明光热协同策略不仅可以大幅降低反应温度, 还能极大提升反应动力学, 为强吸热反应过程提供了一条提效降耗的反应途径.
综上所述, 本工作通过构建结构精准可控的SrTiO_x负载的CuCo邻近界面结构, 同时利用光解水产生的活性氢/氧物种促进CO₂和CH₄活化, 实现了高效定向共转化. 本文提出的“光热协同”策略为高效活化CO₂制高值化学品提供了新的研究思路, 同时显著降低了能耗, 对解决强吸热催化反应高能耗问题提供了参考.

关键词: 光热协同, CO₂和CH₄共转化, SrTiO_x负载CuCo, 水裂解, C₂含氧化合物

Abstract:

Photosynthesis is a potential strategy to enable endergonic process that usually needs high-temperature in thermochemistry to supply the energy for inert-bond activation and/or strong endothermic reaction. The conversion of CO₂ into value-added C₂-oxygenates is a promising process to realize artificial photosynthesis, but suffers from relatively lower efficiency due to complex multi-electron (≥ 10) transfer processes and sluggish kinetics of C-C coupling. This work proposes an all-new H₂O-promoted strategy for efficient production of C₂ oxygenates from the concurrent activation and subsequent co-conversion of CO₂ with CH₄ under photo-thermal cooperation, in which photocatalytic H₂O-splitting derived active hydrogen species for CO₂ activation, and concomitant active oxygen species for CH₄ activation. A formation rate of as high as 2.05 mmol g^-1 h^-1 for C₂-oxygenates (CH₃CHO and CH₃CH₂OH) in a selectivity of > 86% has been afforded over SrTiO_x supported CuCo under 200 °C and ultraviolet-visible illumination. It has been revealed that SrTiO_x drives photocatalytic H₂O-splitting under the excitation primary from ultraviolet light, paired Cu^I/Cu⁰ sites promote the formation of *CH_xO intermediate from CO₂, Co sites conduct CH₄-to-*CH₃, and C-C coupling of *CH_xO and *CH₃ on adjacent Cu-Co facilitates the generation of C₂-oxygenates.

Key words: Photo-thermal cooperation, Co-conversion of CO₂ and CH₄, SrTiO_x supported Cu-Co, Water-splitting, C₂-oxygenates

朱彦儒, 张志军, 张健, 蒋双江, 安哲, 宋红艳, 舒心, 习卫, 郑黎荣, 何静. 光热协同驱动SrTiO_x负载CuCo催化CO₂-CH₄和H₂O共转化制备C₂含氧化合物[J]. 催化学报, 2024, 61: 164-178.

Yanru Zhu, Zhijun Zhang, Jian Zhang, Shuangjiang Jiang, Zhe An, Hongyan Song, Xin Shu, Wei Xi, Lirong Zheng, Jing He. Photo-thermal cooperation for the conversion of CO₂ and CH₄ with H₂O to C₂ oxygenates over SrTiO_x supported CuCo[J]. Chinese Journal of Catalysis, 2024, 61: 164-178.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60026-4

https://www.cjcatal.com/CN/Y2024/V61/I6/164

图/表 7

Fig. 1. Illustration of conversion of CO2 and CH4 with H2O splitting derived oxygen and hydrogen species to produce CH3CHxO (X = 1 or 3) over SrTiOx supported heterojunction Cu-Co.

Fig. 2. (a) Schematic illustration for the preparation of SrTiOx (SrTiOx) supported Cu-Co. TEM image with particle size distributions inserted (b), HR-TEM image (c), and EDX element mapping analysis (d) of Cu0.10-Co-SrTiOx. Fourier-transform of the k3-weighted EXAFS spectra (e,f) and normalized XANES spectra (g,h) for Co K-edge and Cu K-edge.

Fig. 3. Conversion of CO2 with H2O. CO2 conversion rates (A) and product formation rates (B) in the conversion of CO2 with H2O on Cu0.10-Co1-SrTiOx, Co-SrTiOx, Cu-SrTiOx, and SrTiOx at 80 °C under illumination (300 W Xe-lamp). FT-IR spectra recorded activation of CO2 at 80 °C in dark or light, with or without H2O, and with Ar purge followed by H2 exposure on Cu0.10-Co1-SrTiOx in range of 3100-2700 cm-1 (C) and 2150-2050 cm-1 (D). (E) Variation of C2 oxygenates formation rates with CuI/Cu0 ratio and the normalized CHxO formation rate (CHxO formation rate/CO2 conversion rate) with CuI/Cu0 ratio on Cu-Co-SrTiOx in the conversion of CO2 with H2O at 80 °C under illumination.

Fig. 4. Conversion of CH4 with H2O and CO2+CH4 with H2O. (A) Product formation rates in the conversion of CH4 with H2O on Cu0.10-Co1-SrTiOx, Co-SrTiOx, Cu-SrTiOx, and SrTiOx. (B) FT-IR spectra recorded activation of CH4 on Cu0.10-Co1-SrTiOx. (C-F) Conversion of CO2 and CH4 with H2O. (C) Product formation rates on Cu0.10-Co1-SrTiOx, Co-SrTiOx, Cu-SrTiOx, and SrTiOx. (D) Product formation rates on Cu0.10-Co1-SrTiOx under varied conditions. (E) Product formation rates on Cu0.02-Co1-SrTiOx at varied temperatures. (F) Variation of CH3CH2OH/CH3CHO and H2 production rate with reaction temperatures on Cu0.02-Co1-SrTiOx under illumination. Reactions in (A) and (C) were performed at 80 °C under illumination (300 W Xe-lamp).

Fig. 5. Photo-thermal cooperation to decrease the reaction temperature and activation energy. Reaction temperature and activation energy of CO2 and CH4 with H2O with photo-thermal cooperation in this work, and the data in similar thermocatalysis reactions reported [69???-73] in the literatures.

Fig. 6. Mass spectrometry results of the reaction products of isotopically labeled CH4+CO2 with H2O using CD4 (A), 13CO2 (B), D2O (C), or H218O (D) on Cu0.10-Co1-SrTiOx; (left) liquid products, (middle) gaseous products, and (right) proposed reaction pathways. Reaction conditions: 80 °C, 4 h, 300 W Xe-lamp. (E) Summarized reaction network of CH4+CO2 with H2O.

Fig. 7. Illustrations of reaction mechanism for the coupling of CO2 and CH4 with H2O on adjacent Cu-Co supported on SrTiOx.

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光热协同驱动SrTiO_x负载CuCo催化CO₂-CH₄和H₂O共转化制备C₂含氧化合物

Photo-thermal cooperation for the conversion of CO₂ and CH₄ with H₂O to C₂ oxygenates over SrTiO_x supported CuCo

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