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1 Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A. This journal is The Royal Society of Chemistry 2018 Supplementary Text and Figures NaCl Induced Nickel-Cobalt Inverse Spinel Structure for Boosting Hydrogen Evolution from Ethyl Acetate and Water Zhiwei Xue,, Yuesong Shen,, * Lin Chu, Yan Wang, Yu Zhang, Zhefei Sun, Jianhai Wang, Yanwei Zeng, Peiwen Li, and Shemin Zhu College of Materials Science and Engineering, Jiangsu Collaborative Innovation Center for Advanced Inorganic Function Composites, Jiangsu National Synergetic Innovation Center for Advanced Materials, Nanjing Tech University, Nanjing , P. R. China Department of Aerospace and Mechanical Engineering, the University of Arizona, Tucson, AZ 85721, United States * address: shenyuesong@njtech.edu.cn, lawrence@njtech.edu.cn This file includes: Supplementary Text S1 and S2 Supplementary Figure S1 to S7 1
2 Supplementary Text S1 Characterizations of NC/N catalyst XPS analysis was taken with the AXIS ULTRA DLD instrument, for which monochromatic Al-Kα radiation was used as the excitation source. The prepared catalyst was dried at 100 C for 24 h to get rid of water, and then was directly analyzed without surface sputtering or etching. In this way, the degree of vacuum in the XPS equipment was maintained at 10-7 Pa. Powder X-ray diffraction (XRD) patterns of the NC/N catalysts were carried out on a D/MAX-RB X-ray diffractometer (Rigaku, Japan) using Cu Kα radiation (λ = Å). The 2θ scans covered the range of 10~80 (5 /min), and the accelerating voltage and applying current were 40 kv and 30 ma, respectively. Temperature programming desorption of ammonia (NH 3 -TPD) was used to investigate the surface acid-base property of NC/N catalyst using CHEMBET-3000 (Quantachrome). The samples (100 mg) were pretreated in a flow of He (30 ml/min) at 450 C for 1 h, and then cooled to 50 C with a flow of NH 3 (30 ml/min) for ammonia adsorption. The NH 3 -TPD profile was measured online by a Thermo ONIX ProLab mass spectrometer when the sample was heated at a rate of 10 C/min from 50 to 750 C with a flow of He (30 ml/min). The combination of temperature programing reduction (H 2 - TPR) and temperature programing oxidation (O 2 -TPO) was used to investigate the redox ability of NC/N catalysts. The samples (100 mg) were treated in He flow at 450 C for 1 h, and then cooled to ambient temperature. H 2 -TPR profile was measured online when the sample was heated at a rate of 10 C/min from 50 to 750 C with a flow of 10%-H 2 /He (70 ml/min). Then, the sample was cooled to 50 C with the H 2 /He flow. After that, O 2 -TPO profile was measured online when the sample was heated at a rate of 10 C/min from 50 to 750 C with a flow of 10 wt. % O 2 /He (70 ml/min). In situ DRIFTS experiments were carried out by a Thermo Nicolet is10 FTIR spectrometer, equipped with a liquid-nitrogen-cooled MCT detector. 32 scans were averaged for each spectrum, which were recorded at a resolution of 4 cm -1. Ethyl acetate was introduced to the reactor by passing nitrogen stream (50 ml/min) through a bubbler containing ethyl acetate to sweep ethyl acetate vapors to the reactor. The micro-structure of the catalysts was measured by SEM (Model JSM-5900, JEOL, Tokyo, Japan) and TEM (a 200 kv Joel 2010F transmission electron microscope). 2
3 Supplementary Text S2: The effect of O 2 /EA molar ratio on catalytic performance Increasing O 2 /C n molar ratio has been considered as an effective method to improve the anti-coke ability of reforming catalysts. 1, 2 Oxidation is an important part of ATR, which provides heat for ATR reaction and promotes the conversion of carbon (Eq.S1~Eq.S5). Fig.S6a shows the S H2 of NC 0.5 /N under different O 2 /EA molar ratios. Obviously, increasing O 2 /EA molar ratio from 1:1 to 1.5:1 leads to a dramatic decline in S H2. The phenomenon may be the result due to the partial oxidation of H 2 by the excess O 2 (Eq.S2). The results in Fig.S7 show that the S CO and S CO2 are slightly affected by O 2 /EA ratio at temperature lower than 650 C. But, a dramatic increase of S CO2 and a dramatic decrease of S CO happen at temperatures of 650 and 750 C. The data reveals that the oxidation of CO may happen at high reaction temperatures. Oxygen seems to preferentially react with the coke once it diffuses to the surface of NC 0.5 /N catalyst, because the enthalpy of Eq.S3 is the highest. However, O 2 is a non-polar molecule, whose diffusion is unconstrained by catalysts. The oxidation of carbon only happens when oxygen molecule diffuses to the surface of NC/N catalysts. Therefore, a feasible O 2 /EA molar ratio is of great significance to maintain equilibrium between heat supply, H 2 yield and anti-coke. CO O 2 CO 2 H O 2 H 2 O C + O 2 CO 2 H 283 kj/mol H kj/mol H kj/mol (1) (2) (3) C O 2 CO H kj/mol C 4 H 8 O 2 (g) + 6H 2 O(g) Catal, 10H 2 (g) + 4CO 2 (g) H kj/mol The reaction with the absence of O 2 is another reforming technology termed Steam reforming (SR, Eq.S5). H 2 yields (Y H2 ) of NC 0.5 /N measured by EAATR and EASR are compared (Fig.S6b). The Y H2 of EASR linearly rises up by increasing the reaction temperature from 500 to 600 C, then linearly descends from 600 to 750 C. EASR obtains the highest Y H2 of 7.64 mol (H2) /mol (EA) at 600 C, which is ~1 mol (H2) /mol (EA) higher than that of EAATR, but slightly lower than the Y H2 tested under H 2 O/EA molar ratio of 8:1 (Fig.2a). The Y H2 of EASR is remarkably lower than that of EAATR at other reaction temperatures. The phenomenon is similar to the result in Fig.2a. The high Y H2 of EASR is mainly caused by the high WGS activity of NC 0.5 /N at 600 C. (4) (5) 3
4 Fig.S1 Fig.S1 The S CO (a), S CO2 (c) and S CH4 (e) of NC/N catalysts with Co/Ni molar ratio from 0:1 to 1:1; The S CO (b), S CO2 (d) and S CH4 (f) of NC/N catalysts with Co/Ni molar ratio from 1:1 to 4:1. The S CO, S CO2 and S CH4 of NC/N catalysts were tested under the reaction condition of 2 g catalyst, H 2 O: EA = 4, O 2 : EA = 1, GHSV = h -1, reaction temperature ranging from 500 to 750 C. 4
5 Fig.S2 Fig.S2 The carbon balance (the sum of S CO, S CO2 and S CH4 ) of NC/N catalysts with Co/Ni molar ratio from 0:1 to 4:1 at 650 C. 5
6 Fig.S3 Fig.S3 The XRD profile of NiO from NiO/NaCl catalyst (washing away the NaCl) 6
7 Fig.S4 Fig.S4 The H 2 -TPR profile of sample 1%-NiO/NaCl 7
8 Fig.S5 Fig.S5 The SEM graph of sample NiO/NaCl 8
9 Fig.S6 Fig.S6 (a) The S H2 of NC 0.5 /N catalyst measured under different O 2 /EA molar ratios; (b) the compare of ATR and SR reaction. The H 2 O/EA molar ratio on EASR is 6:1. 9
10 Fig.S7 Selectivity (%) S CO O 2 /EA=1:1 S CO2 O 2 /EA=1:1 S CO O 2 /EA=1.5:1 S CO2 O 2 /EA=1.5: Temperature ( o C) Fig.S7 The Sco and S CO2 of NC 0.5 /N catalyst tested under O 2 /EA molar ratio of 1:1 and 1.5:1 1. G. Han, S. Lee and J. Bae, Applied Energy, 2015, 156, S. Yoon, I. Kang and J. Bae, International Journal of Hydrogen Energy, 2008, 33,
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