富缺陷BN负载的高分散Cu催化乙醇脱氢制乙醛

doi:10.1016/S1872-2067(21)63891-3

催化学报 ›› 2022, Vol. 43 ›› Issue (4): 1092-1100.DOI: 10.1016/S1872-2067(21)63891-3

富缺陷BN负载的高分散Cu催化乙醇脱氢制乙醛

程世群^a, 翁雪霏^a, 王庆楠^a, 周百川^a, 李文翠^a, 李名润^b, 贺雷^a, 王东琪^a, 陆安慧^a^,^*()

^a大连理工大学化工学院, 辽宁省低碳资源高值化利用重点实验室, 精细化工国家重点实验室, 辽宁大连116024
^b中国科学院大连化学物理研究所, 催化基础国家重点实验室, 辽宁大连116023

收稿日期:2021-06-26 接受日期:2021-06-26 出版日期:2022-03-05 发布日期:2022-03-01
通讯作者: 陆安慧
基金资助:
国家自然科学基金中德合作交流项目(21761132011);国家自然科学基金重点项目(21733002);长江学者奖励计划资助项目(T2015036)

Defect-rich BN-supported Cu with superior dispersion for ethanol conversion to aldehyde and hydrogen

Shi-Qun Cheng^a, Xue-Fei Weng^a, Qing-Nan Wang^a, Bai-Chuan Zhou^a, Wen-Cui Li^a, Ming-Run Li^b, Lei He^a, Dong-Qi Wang^a, An-Hui Lu^a^,^*()

^aState Key Laboratory of Fine Chemicals, Liaoning Key Laboratory for Catalytic Conversion of Carbon Resources, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, Liaoning, China
^bState Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China

Received:2021-06-26 Accepted:2021-06-26 Online:2022-03-05 Published:2022-03-01
Contact: An-Hui Lu
Supported by:
a Joint Sino-German Research Project(21761132011);State Key Program of the National Natural Science Foundation of China(21733002);Cheung Kong Scholars Program of China(T2015036)

摘要/Abstract

摘要：

生物乙醇作为平台分子通过催化转化的方法可以制备烯烃、乙醛、丁醇和芳香化学品等, 其中乙醛是生产乙酸、季戊四醇、三氯乙醛、山梨酸等重要化学品的原料. 随着乙醛的需求量逐年增加, 发展以乙醇直接脱氢生成乙醛的工艺, 具有联产氢气、原子经济性高、产物易分离的优点, 符合国际绿色低碳发展战略要求, 有望替代当前乙烯氧化法生产工艺. 乙醇分子比较活泼, 催化过程中通常伴随着脱水、羟醛缩合等副反应, 导致乙醛的选择性降低. 根据文献报道, Cu基催化剂可解离吸附乙醇, 选择性断裂C‒H键, 是有效的乙醇直接脱氢催化剂. 常规氧化物负载的铜基催化剂往往存在乙醛选择性低、Cu物种易团聚失活等问题.
+本文通过球磨方法处理商业六方氮化硼(h-BN), 从而得到表面缺陷, 使其边缘暴露一定的‒OH和‒NH₂等极性官能团, 进而增强金属与载体的相互作用, 抑制Cu物种的团聚, 提高Cu基催化剂在乙醇脱氢反应中的稳定性. 考察了不同负载量下Cu物种的分散情况, 发现当负载量高达5% (5Cu/BNS)时, Cu物种仍然能够保持高分散. 5Cu/BNS催化剂在280 °C, WHSV = 9.6 h^‒1反应条件下, 催化生成乙醛选择性达到98%, 乙醇转化率为82%, 且反应50 h后活性保持不变, Cu物种在BNS载体上仍保持高度分散. 结合红外光谱和X射线光电子能谱(XPS)表征, 证实BNS表面存在B‒OH官能团, 增强了Cu物种与载体的相互作用, 提高了Cu催化剂在乙醇脱氢反应中的稳定性. 通过原位红外实验对反应物在载体上的吸附行为研究, 进一步理解5Cu/BNS表现出优异的乙醛选择性的原因. 结果表明, 乙醛在BNS载体上不发生吸附. 从结构化学的角度来说, BNS富π电子, 与乙醇的羟基相互作用但是与乙醛的富电子的C=O官能团相互排斥, 促进产物乙醛脱附, 因此表现出优异的选择性. 该方法为设计一种高分散Cu基催化剂提供了新策略, 相比于文献报道的催化体系, 该催化剂在乙醇脱氢方面表现出更好的催化性能.

关键词: 乙醇脱氢, 铜, 氮化硼纳米片, 高分散, 原位红外

Abstract:

Copper-based heterogeneous catalysts commonly exhibit uncontrolled growth of copper species under reaction conditions because of the low Hüttig temperature (surface mobility of atoms) and Tamman temperature (bulk mobility) for copper at just 134 and 405 °C, respectively. Herein, we report the use of defect-enriched hexagonal boron nitride nanosheets (BNSs) as a support to anchor the Cu species, which resulted in superior dispersion of the Cu species. The obtained Cu/BNS catalyst was highly stable for ethanol dehydrogenation, with a high selectivity of 98% for producing acetaldehyde and an exceptionally high acetaldehyde productivity of 7.33 g_AcH g_cat^‒1h^‒1under a weight hourly space velocity of 9.6 g_EtOH g_cat^‒1h^‒1. The overall performance of our designed catalyst far exceeded that of most reported heterogeneous catalysts in terms of the stability of the Cu species and the yield of acetaldehyde in this reaction. The hydroxyl groups at the defect edges of BNS were responsible for the stabilization of the copper species, and the metal-support interaction was reinforced through charge transfer, as evidenced by coupling atomic resolution images with probe molecule infrared spectroscopy and X-ray photoelectron spectroscopy. A designed in situ diffuse reflectance infrared Fourier transform spectroscopy study of ethanol/acetaldehyde adsorption further revealed that Cu/BNS favored ethanol adsorption while suppressing acetaldehyde adsorption and further side reactions. This study demonstrates a new method for designing highly dispersed Cu-based catalysts with high durability.

Key words: Ethanol dehydrogenation, Copper, Boron nitride nanosheet, Superior dispersion, In situ DRIFT

程世群, 翁雪霏, 王庆楠, 周百川, 李文翠, 李名润, 贺雷, 王东琪, 陆安慧. 富缺陷BN负载的高分散Cu催化乙醇脱氢制乙醛[J]. 催化学报, 2022, 43(4): 1092-1100.

Shi-Qun Cheng, Xue-Fei Weng, Qing-Nan Wang, Bai-Chuan Zhou, Wen-Cui Li, Ming-Run Li, Lei He, Dong-Qi Wang, An-Hui Lu. Defect-rich BN-supported Cu with superior dispersion for ethanol conversion to aldehyde and hydrogen[J]. Chinese Journal of Catalysis, 2022, 43(4): 1092-1100.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63891-3

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图/表 6

Fig. 1. (a) XRD patterns of the BNS support and xCu/BNS catalysts after H2 treatment at 350 °C; Bright-field AC-STEM image (b) and the corresponding dark-field AC-STEM image (c) of 5Cu/BNS catalyst.

Fig. 2. (a) Light-off profiles of the 5Cu/BNS (red squares indicate the freshly reduced catalyst, red circles indicate the spent catalyst) and 5Cu/BN catalysts; the equilibrium conversions are presented in gray; (b) Productivity of acetaldehyde versus ethanol reaction rate for the catalysts described in this work and in the literature (the numbers in this Fig. refer to the references, Table S2); (c) Ethanol conversion as a function of time-on-stream (TOS) at 240 °C. (d) Arrhenius plots of xCu/BNS catalysts. Reaction conditions: 50 mg of catalyst, 10 vol% C2H5OH/N2, WHSV = 9.8 h-1for (a), (b), and (c); the catalyst weight was carefully varied (WHSV from 35 to 76 h-1) to keep ethanol conversion below 20%.

Fig. 3. (a) H2-TPR profiles of xCu/BNS, 5Cu/BN (8% H2/N2, 10 °C/min); (b) In situ XRD patterns of 5Cu/BNS catalyst under 8% H2/N2 at indicated temperatures; (c) FTIR spectra of CO adsorption on 1Cu/BNS and 5Cu/BNS samples at -173 °C; (d) Cu 2p XP spectra and (inset) Cu LMM XAE spectra of the in situ-reduced 5Cu/BNS; (e) NH3-TPD profiles of BNS and BN supports.

Fig. 4. Bright-field AC-STEM images (a,c) and the corresponding dark-field AC-STEM images (b,d) of the spent 5Cu/BNS catalyst for catalytic performance test.

Fig. 5. Each spectrum was collected immediately after a dose of ethanol to 5Cu/BNS, 5Cu/SiO2, and 5Cu/Al2O3 catalysts. Spectrum recorded before any ethanol dosing was used as the background. Reaction conditions: 240 °C, ~40 mg of catalyst, 5 × 10-8mol of C2H5OH in each dose, N2 as carrier gas.

Fig. 6. Each spectrum was collected immediately after a dose of acetaldehyde to the 5Cu/BNS, 5Cu/SiO2, and 5Cu/Al2O3 catalysts. Spectrum recorded before any acetaldehyde dosing was used as the background. Reaction conditions: 240 °C, ~40 mg of catalyst, 2 × 10-8mol CH3CHO in each dose, N2 as carrier gas.

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富缺陷BN负载的高分散Cu催化乙醇脱氢制乙醛

Defect-rich BN-supported Cu with superior dispersion for ethanol conversion to aldehyde and hydrogen

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