锐钛矿型TiO2负载Ni单原子用于催化丙烷脱氢

doi:10.1016/S1872-2067(23)64584-X

催化学报 ›› 2024, Vol. 57: 105-113.DOI: 10.1016/S1872-2067(23)64584-X

锐钛矿型TiO₂负载Ni单原子用于催化丙烷脱氢

张倩^a^,^b, 江训柱^a^,^b, 苏杨^a, 赵阳^c, 乔波涛^a^,^*()

^a中国科学院大连化学物理研究所, 中国科学院应用催化科技重点实验室, 辽宁大连 116023
^b中国科学院大学, 北京 100049
^c中国科学院大连化学物理研究所, 大连洁净能源国家实验室, 辽宁大连 116023

收稿日期:2023-09-28 接受日期:2023-12-18 出版日期:2024-02-18 发布日期:2024-02-10
通讯作者: * 电子信箱: bqiao@dicp.ac.cn (乔波涛).
基金资助:
国家重点研发计划(2021YFA1500503);国家自然科学基金项目(21961142006);国家自然科学基金项目(21972135);国家自然科学基金单原子催化基础研究中心(22388102);中国科学院青年基础研究项目(YSBR-022)

Catalytic propane dehydrogenation by anatase supported Ni single-atom catalysts

Qian Zhang^a^,^b, Xunzhu Jiang^a^,^b, Yang Su^a, Yang Zhao^c, Botao Qiao^a^,^*()

^aCAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China
^cDalian Institute of Chemical Physics, Dalian National Laboratory for Clean Energy, Chinese Academy of Sciences, Dalian 116023, Liaoning, China

Received:2023-09-28 Accepted:2023-12-18 Online:2024-02-18 Published:2024-02-10
Contact: * E-mail: bqiao@dicp.ac.cn (B. Qiao).
Supported by:
National Key Research and Development program of China(2021YFA1500503);National Natural Science Foundation of China(21961142006);National Natural Science Foundation of China(21972135);National Natural Science Foundation of China(22388102);CAS Project for Young Scientists in Basic Research(YSBR-022)

摘要/Abstract

摘要：

丙烯市场需求日益增长, 丙烷脱氢(PDH)被认为是最有前途的丙烯定向生产技术之一. 作为PDH商业催化剂, 贵金属Pt的高成本和CrO_x基催化剂的毒性使它们的发展受到限制. 镍基催化剂因具有廉价、环保的特点, 在多种催化反应的应用中引起了研究人员的广泛关注. 然而, 镍在高温烷烃脱氢反应中的应用较少, 目前, 保持反应中镍(II)物种的稳定存在仍然是镍基PDH催化剂的主要挑战. 近来, 单原子催化剂(SAC)在烷烃碳氢键活化过程中表现出优异的催化性能, 具有较好的丙烯选择性和出色的稳定性. 当镍以单个原子的形式分散在载体上时, 它更有可能以带正电的状态存在, 但金属单原子的稳定存在是具有挑战性的.

本文以锐钛矿型的二氧化钛为载体, 采用等体积浸渍法分别制备了0.05 wt%载量的单个原子分散的催化剂(Ni SAC, Ni₁/A-TiO₂)和5 wt%载量的纳米颗粒(NP)催化剂(Ni_NP/A-TiO₂). 结合球差电镜、原位漫反射傅里叶变换红外光谱和X射线吸收光谱等表征结果表明, Ni SAC催化剂主要含有单个Ni原子, 以Ni(II)价态孤立地分散在载体上, 而Ni_NP/A-TiO₂催化剂中的Ni物种主要以纳米粒子(1 ± 0.2 nm)的形式存在. 在580 °C的PDH反应中, Ni₁/A-TiO₂催化剂表现出较好的本征活性和丙烯选择性, 而且比相应的Ni NPs催化剂具有更好的抗积炭稳定性, 在Ni₁/A-TiO₂上得到的丙烯产率约为1.96 mol_C3H6 g_Ni^-1 h^-1, 超过Ni_NP/A-TiO₂样品(0.03 mol_C3H6 g_Ni^-1 h^-1)的65倍, Ni SAC催化剂的丙烯时空收率(STY_C3H6)约为0.2 kg h^-1 kg_cat^-1, 与文献报道的大部分非贵金属催化剂STY值相当(0.02-0.3 kg h^-1 kg_cat^-1). 还原后的TiO₂载体因具有丰富的氧空位(OVs)和配位不饱和的Ti³⁺表现出一定的活性, 而Ni SAC得到了更高的丙烷转化率, 但Ni单原子的引入并没有增加OVs和Ti³⁺的浓度, Ni单原子催化剂的活化能低于纯载体, 说明两者的活性位不同. 此外, 在还原条件下, 由于Ni NPs与TiO₂载体之间的强相互作用, Ni NPs位点被TiO_x覆盖层(~2 nm)包裹, 从而显示出较差的反应活性.

综上所述, 本文报道了Ni单原子催化剂在丙烷直接脱氢反应中比相应的Ni NP催化剂表现出更好的反应性能, 体现了具有孤立活性位点的单原子催化剂在丙烷脱氢反应中的优势, 为今后探究可用于丙烷脱氢反应的单原子催化剂的制备和应用提供参考.

关键词: 丙烷脱氢, 单原子催化剂, 原子利用率, 丙烯选择性, 稳定性

Abstract:

With the increasing production of propane from shale gas and the growing demand for propylene, propane dehydrogenation (PDH) has gained significant attention as a promising route for the on-purpose production of propylene. As a cheap yet efficient catalyst, Ni-based catalysts have attracted interest because of its ability to activate alkane. Single-atom catalysts (SACs) can maximize the metal atom utilization. Here, we demonstrate that anatase TiO₂ supported Ni SAC (Ni₁/A-TiO₂) exhibits not only superior intrinsic activity and propylene selectivity but also much better stability than the corresponding Ni nanoparticle (NP) catalyst (Ni_NP/A-TiO₂) in PDH reaction at 580 °C. The rate of propylene production on Ni₁/A-TiO₂ is about 1.96 mol_C3H6 g_Ni^-1 h^-1, about 65 times higher than that of Ni_NP/A-TiO₂ sample (0.03 mol_C3H6 g_Ni^-1 h^-1). In combination of high-angle annular dark-field scanning transmission electron microscopy, in-situ diffuse reflectance infrared Fourier transform spectra, in-situ X-ray photoelectron spectroscopy and X-ray absorption spectroscopy characterizations, we confirm that the Ni SAC mainly contains individual Ni atom singly dispersed on the support in positive Ni (II) valence state. In addition, as a result of strong metal-support interaction (SMSI) between Ni NP and TiO₂carrier under reduced conditions, the Ni NPs sites are encapsulated by TiO_x overlayer (~2 nm thick) thus display poor reaction performance.

Key words: Propane dehydrogenation, Single-atom catalysts, Metal atom utilization, Propylene selectivity, Stability

张倩, 江训柱, 苏杨, 赵阳, 乔波涛. 锐钛矿型TiO₂负载Ni单原子用于催化丙烷脱氢[J]. 催化学报, 2024, 57: 105-113.

Qian Zhang, Xunzhu Jiang, Yang Su, Yang Zhao, Botao Qiao. Catalytic propane dehydrogenation by anatase supported Ni single-atom catalysts[J]. Chinese Journal of Catalysis, 2024, 57: 105-113.

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Fig. 1. (a-c) The AC-HAADF-STEM images and corresponding EDS mapping of Ni1/A-TiO2-H600 sample, Ni single atoms are highlighted in yellow circles. The AC-HAADF-STEM images (d,e) and size distribution (f) of NiNP/A-TiO2-H600 sample. (g-i) In-situ CO-DRIFT spectra at saturation coverage and followed by helium (He) purge for 30, 60, 90 and 120 s (as labeled) at low temperature (-115 °C) on A-TiO2 and Ni/A-TiO2 catalysts after 600 °C reduction.

Fig. 2. Ni K-edge FT-EXAFS spectra (a), Wavelet transform (WT)-EXAFS of k2-weighted k-space (b) and Ni K-edge XANES spectra (c) of Ni foil, NiO, Ni1/A-TiO2-H600 and NiNP/A-TiO2-H600. (d) In-situ XPS spectra of Ni 2p3/2 for Ni1/A-TiO2-H600 and NiNP/A-TiO2-H600 samples.

Fig. 3. (a) Propane conversion and propene selectivity as a function of time on stream at 580 °C. Conditions: 250 mg catalyst, C3H8/H2/N2 = 1/1/4, WHSV of propane = 2.0 h-1, total flow of 25 mL min-1. EPR spectra (b), Ti 2p (c) and O 1s (d) spectra of pure A-TiO2 and Ni/A-TiO2-H600 samples.

Fig. 4. (a,b) HRTEM images of spent NiNP/A-TiO2 after PDH reaction. (c) In-situ CO-DRIFT spectra at saturation coverage and followed by He purge at low temperature (-115 °C) on spent NiNP/A-TiO2. (d) Propane conversion and propene selectivity over NiNP/A-TiO2 sample with different reduction. Conditions: 580 °C, 250 mg catalyst, C3H8/H2/N2 = 1/1/4, WHSV of propane = 2.0 h-1, total flow of 25 mL min-1. (e) TG analysis and MS signal for the spent catalysts.

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锐钛矿型TiO₂负载Ni单原子用于催化丙烷脱氢

Catalytic propane dehydrogenation by anatase supported Ni single-atom catalysts

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