Tuning the crystallite size of monoclinic ZrO2 to reveal critical roles of surface defects on m-ZrO2 catalyst for direct synthesis of isobutene from syngas

doi:10.1016/j.cjche.2021.04.008

Chinese Journal of Chemical Engineering ›› 2021, Vol. 35 ›› Issue (7): 211-219.DOI: 10.1016/j.cjche.2021.04.008

• Catalysis, Kinetics and Reaction Engineering • Previous Articles Next Articles

Tuning the crystallite size of monoclinic ZrO₂ to reveal critical roles of surface defects on m-ZrO₂ catalyst for direct synthesis of isobutene from syngas

Xuemei Wu^1,2, Minghui Tan¹, Bing Xu^1,2, Shengying Zhao^1,2, Qingxiang Ma³, Yingluo He⁴, Chunyang Zeng⁵, Guohui Yang^1,4, Noritatsu Tsubaki⁴, Yisheng Tan¹

1. State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;
2. University of Chinese Academy of Sciences, Beijing 100049, China;
3. State Key Laboratory of High-efficiency Utilization of Coal and Green Chemical Engineering, Ningxia University, Yinchuan 750021, China;
4. Department of Applied Chemistry, School of Engineering, University of Toyama, Gofuku 3190, Toyama 930-8555, Japan;
5. China Petroleum Chemical Industry Federation, Beijing 100723, China

Received:2020-12-29 Revised:2021-04-06 Online:2021-09-30 Published:2021-07-28
Contact: Minghui Tan, Guohui Yang
Supported by:
This work was financially supported by the Natural Science Foundation of China (21978312, 21908235 and 21802155), the Key Research Program of Frontier Sciences, CAS (QYZDB-SSW-JS C043), as well as Foundation of State Key Laboratory of Highefficiency Utilization of Coal and Green Chemical Engineering (2019-KF-05 and 2018-K22). Research Project Supported by Shanxi Scholarship Council of China and Fund Program for the Scientific Activities of Selected Returned Overseas Professionals in Shanxi Province are also greatly appreciated.

Tuning the crystallite size of monoclinic ZrO₂ to reveal critical roles of surface defects on m-ZrO₂ catalyst for direct synthesis of isobutene from syngas

Xuemei Wu^1,2, Minghui Tan¹, Bing Xu^1,2, Shengying Zhao^1,2, Qingxiang Ma³, Yingluo He⁴, Chunyang Zeng⁵, Guohui Yang^1,4, Noritatsu Tsubaki⁴, Yisheng Tan¹

1. State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;
2. University of Chinese Academy of Sciences, Beijing 100049, China;
3. State Key Laboratory of High-efficiency Utilization of Coal and Green Chemical Engineering, Ningxia University, Yinchuan 750021, China;
4. Department of Applied Chemistry, School of Engineering, University of Toyama, Gofuku 3190, Toyama 930-8555, Japan;
5. China Petroleum Chemical Industry Federation, Beijing 100723, China

通讯作者: Minghui Tan, Guohui Yang
基金资助:
This work was financially supported by the Natural Science Foundation of China (21978312, 21908235 and 21802155), the Key Research Program of Frontier Sciences, CAS (QYZDB-SSW-JS C043), as well as Foundation of State Key Laboratory of Highefficiency Utilization of Coal and Green Chemical Engineering (2019-KF-05 and 2018-K22). Research Project Supported by Shanxi Scholarship Council of China and Fund Program for the Scientific Activities of Selected Returned Overseas Professionals in Shanxi Province are also greatly appreciated.

Abstract

Abstract: The effects of crystallite size on the physicochemical properties and surface defects of pure monoclinic ZrO₂ catalysts for isobutene synthesis were studied. We prepared a series of monoclinic ZrO₂ catalysts with different crystallite size by changing calcination temperature and evaluated their catalytic performance for isobutene synthesis from syngas. ZrO₂ with small crystalline size showed higher CO conversion and isobutene selectivity, while samples with large crystalline size preferred to form dimethyl ether (DME) instead of hydrocarbons, much less to isobutene. Oxygen defects (O_Defects) analyzed by X-ray photoelectron spectroscopy (XPS) provided evidence that more O_Defects occupied on the surface of ZrO₂ catalysts with smaller crystalline size. Electron paramagnetic resonance (EPR) and ultraviolet-visible diffuse reflectance (UV-vis DRS) confirmed the presence of high concentration of surface defects and Zr³⁺ on m-ZrO₂-5.9 sample, respectively. In situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS) analysis indicated that the adsorption strength of formed formate species on catalyst reduced as the crystalline size decreased. These results suggested that surface defects were responsible for CO activation and further influenced the adsorption strength of surface species, and thus the products distribution changed. This study provides an in-depth insight for active sites regulation of ZrO₂ catalyst in CO hydrogenation reaction.

Key words: Syngas, Isobutene, ZrO₂ catalyst, Crystallite size, Surface defects

摘要： The effects of crystallite size on the physicochemical properties and surface defects of pure monoclinic ZrO₂ catalysts for isobutene synthesis were studied. We prepared a series of monoclinic ZrO₂ catalysts with different crystallite size by changing calcination temperature and evaluated their catalytic performance for isobutene synthesis from syngas. ZrO₂ with small crystalline size showed higher CO conversion and isobutene selectivity, while samples with large crystalline size preferred to form dimethyl ether (DME) instead of hydrocarbons, much less to isobutene. Oxygen defects (O_Defects) analyzed by X-ray photoelectron spectroscopy (XPS) provided evidence that more O_Defects occupied on the surface of ZrO₂ catalysts with smaller crystalline size. Electron paramagnetic resonance (EPR) and ultraviolet-visible diffuse reflectance (UV-vis DRS) confirmed the presence of high concentration of surface defects and Zr³⁺ on m-ZrO₂-5.9 sample, respectively. In situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS) analysis indicated that the adsorption strength of formed formate species on catalyst reduced as the crystalline size decreased. These results suggested that surface defects were responsible for CO activation and further influenced the adsorption strength of surface species, and thus the products distribution changed. This study provides an in-depth insight for active sites regulation of ZrO₂ catalyst in CO hydrogenation reaction.

关键词: Syngas, Isobutene, ZrO₂ catalyst, Crystallite size, Surface defects

Xuemei Wu, Minghui Tan, Bing Xu, Shengying Zhao, Qingxiang Ma, Yingluo He, Chunyang Zeng, Guohui Yang, Noritatsu Tsubaki, Yisheng Tan. Tuning the crystallite size of monoclinic ZrO₂ to reveal critical roles of surface defects on m-ZrO₂ catalyst for direct synthesis of isobutene from syngas[J]. Chinese Journal of Chemical Engineering, 2021, 35(7): 211-219.

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Tuning the crystallite size of monoclinic ZrO₂ to reveal critical roles of surface defects on m-ZrO₂ catalyst for direct synthesis of isobutene from syngas

Tuning the crystallite size of monoclinic ZrO₂ to reveal critical roles of surface defects on m-ZrO₂ catalyst for direct synthesis of isobutene from syngas

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