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Highly Dispersed and Stable Ni/SBA-15 Catalyst for Reverse Water-Gas Shift Reaction

by 1 and 2,3,4,*
School of Food and Pharmacy, Zhejiang Ocean University, Zhoushan 316022, China
Department of Chemical Engineering, School of Petrochemical Engineering and Environment, Zhejiang Ocean University, Zhoushan 316022, China
National-Local Joint Engineering Laboratory of Harbor Oil & Gas Storage and Transportation Technology, Zhejiang Ocean University, Zhoushan 316022, China
Zhejiang Provincial Key Laboratory of Petrochemical Pollution Control, Zhejiang Ocean University, Zhoushan 316022, China
Author to whom correspondence should be addressed.
Crystals 2021, 11(7), 790;
Received: 5 June 2021 / Revised: 28 June 2021 / Accepted: 5 July 2021 / Published: 7 July 2021


A 1%Ni/SBA-15(P) catalyst was synthesized with a P123-assisted impregnation method, which exhibited high CO2 conversion and stability in the reverse water-gas shift reaction. For the 1%Ni/SBA-15(P) catalyst, TEM and TPR characterizations demonstrated that the highly dispersed NiO particles at about 3 nm strongly interacted with the SiO2 support. During reverse water-gas shift reaction, the 1%Ni/SBA-15(P) catalyst exhibited higher CO2 conversion than the 1%Ni/SBA-15 catalyst prepared by the conventional impregnation method without P123. The CO2 conversion of the 1%Ni/SBA-15(P) catalyst at 700 °C was 33.7%, which was three times that of the 1%Ni/SBA-15 catalyst. Moreover, the former catalyst was stable at 700 °C within 1000 min. The good activity and stability of the 1%Ni/SBA-15(P) catalyst was owing to small Ni particles that strongly interacted with SBA-15.

Graphical Abstract

1. Introduction

CO2 may be utilized through the dry reforming of methane [1,2,3] and reverse water-gas shift reaction (RWGS) [4,5,6], which are promising models for CO production. CO can be used as a co-reactant for petrochemical manufacturing (syn-gas for Fischer-Tropsch synthesis, hydroformylation, carbonylation) [7,8]. The RWGS can produce CO from the greenhouse gas carbon dioxide and green hydrogen produced by renewable energy. Nickel-based catalysts show good activity in RWGS [9,10,11,12]. However, the side reactions of CO2 methanation are prone to occur on nickel catalysts [10,12,13]. Highly dispersed small Ni particles are favorable for RWGS, while large Ni particles easily generate methane [14]. The endothermic RWGS reaction has a higher equilibrium conversion at high temperature. In addition, because methanation reaction is exothermic, high temperature is beneficial to inhibit methane formation and improve CO selectivity. However, as highly dispersed Ni is prone to sintering deactivation in the high temperature reaction, it is desired to prepare stable Ni-based RWGS catalysts with high Ni dispersion.
Mesoporous silica-based materials are widely used in catalysis [15,16,17]. The SBA-15 has been widely used as the support of various highly dispersed catalysts [18,19,20]. Ni/SBA-15 catalysts have been used for many reactions, such as CO methanation [21], CO2 methanation [22], CO2 reforming of methane [23], ethanol steam reforming [24], and glycerol steam reforming [25]. Although the low Ni content of Ni/SBA-15 is beneficial to improve the selectivity of RWGS reaction, low Ni content will result in a lower CO2 conversion [26].
In this work, the 1%Ni/SBA-15(P) catalyst was synthesized with the P123-assisted impregnation method. Compared with the conventional 1%Ni/SBA-15 catalyst, the 1%Ni/SBA-15(P) catalyst had smaller NiO particles that interact with SiO2, which were active and stable in the RWGS reaction.

2. Materials and Methods

2.1. Catalyst Preparation

The SBA-15 was synthesized according to the literature [27]. The 1%Ni/SBA-15(P) catalyst was synthesized by the P123-assisted impregnation method [28,29]. Briefly, 0.050 g nickel nitrate hexahydrate and 0.010 g P123 (n(P123):n(Ni) = 1:100) were added to 20 mL deionized water. After stirring the solution for 1 h, 1 g of SBA was added and then stirred for 12 h. The solution was heated at 60 °C for 3 h and 110 °C for 2 h. Finally, the 1%Ni/SBA-15(P) catalyst was prepared by the calcination the sample at 600 °C for 4 h.
For comparison, the 1%Ni/SBA-15 was synthesized by the impregnation method without using P123. In the 1%Ni/SBA-15 and 1%Ni/SBA-15(P) catalysts, the nominal content of nickel was 1 wt%.

2.2. Catalyst Characterization

Nitrogen adsorption-desorption analysis was performed on a Quantachrome Autosorb-iQ analyzer at −196 °C (Quantachrome Corporation, Boynton Beach, FL, USA). The sample was degassed at 300 °C for 10 h before analysis. The pore size distribution was obtained using the BJH model. The morphology of the samples was determined by a Tecnai G2 F20 (FEI company, Hillsboro, OR, USA) transmission electron microscope (TEM). The powder X-ray diffraction (XRD) patterns were collected on a DX-2700 X-ray diffractometer (Haoyuan Instrument Co., Ltd., Dandong, China) with Cu Kα radiation at 40 kV and 30 mA. H2 temperature programmed reduction (H2-TPR) measurements were performed on TP-5080 equipment from room temperature to 900 °C (10 °C /min) in 5% H2/Ar (30 mL/min).

2.3. Catalytic Test

Hydrogenation of CO2 was conducted under atmospheric pressure in a fixed bed reactor. Prior to each test, 0.005 g of catalyst and 0.010 g quartz sand were packed in the quartz reactor, and the catalyst was reduced to 650 °C for 2 h under 70% H2/N2 (70 mL/min) flow. When the temperature dropped to 500 °C, the mixed gases (CO2/H2 = 1:1, 100 mL/min) were fed into the reactor for the reaction. The gases product was analyzed by a gas chromatography (GC-7900, Techcomp, Kowloon, Hong Kong). Only CO, CH4, and H2O were produced during the catalytic reaction, and no C2+ hydrocarbon was detected by the GC TCD detector, which was also confirmed by a GC FID detector. Therefore, the conversion and selectivity were estimated as follows:
CO 2   conversion = F in ,   CO 2     F out ,   CO 2   F in ,   CO 2 ×   100 %
CO   selectivity = F out ,   CO F out ,   CO + F out ,   CH 4   ×   100 %
where F in and F out stand for the input and output flow rates.

3. Results and Discussion

3.1. Catalyst Characterization

All the N2 adsorption-desorption isotherms in Figure 1a were type IV isotherms with a hysteresis loop, which confirmed the uniform mesoporous structure of the samples. As shown in Figure 1b, the pore sizes of all the samples were similar, indicating that the mesoporous structure did not change after adding Ni to SBA-15. Table 1 shows that the BET specific surface area decreased with the addition of Ni into SBA-15, while the pore volume was almost unchanged.
Transmission electron microscope (TEM) images in Figure 2 show that both catalysts had the ordered mesoporous structures. As shown in Figure 2a,b, the surface of the 1%Ni/SBA-15 catalyst was covered with NiO particles of 40–60 nm. Meanwhile, there were no large NiO particles in the 1%Ni/SBA-15(P) catalyst (Figure 2c), indicating that small NiO was highly dispersed in the nanochannel of SBA-15. As shown in Figure 2d, small NiO particles about 3 nm in size were observed in the HR-TEM image of 1%Ni/SBA-15(P).
The small-angle XRD patterns of the fresh and reduced catalysts in Figure 3a showed three typical peaks, which indexed to a hexagonal lattice of mesoporous SBA-15 [30]. The results indicate that all the catalysts possessed the ordered mesoporous structure. After reduction, angles of all reflection planes were moved toward higher angle, implying that d-spacing of SBA-15 support must have been contracted.
As shown in Figure 3b, the broad peak at about 22° was assigned to the SiO2 in SBA-15 [24]. The reduced catalysts were treated with 70%H2/N2 at 650 °C for 2 h. NiO and Ni peaks were observed in the fresh and reduced 1%Ni/SBA-15 samples, respectively. On the contrary, there was no peak assigned to NiO in the 1%Ni/SBA-15(P), indicating that the NiO particles were highly dispersed in the 1%Ni/SBA-15(P) [28]. No peak assigned to Ni in the reduced 1%Ni/SBA-15(P) indicates that no large Ni particle was formed, even after reduction at 650 °C.
Figure 4 shows the H2-TPR profiles of the two catalysts. The 1%Ni/SBA-15 had a sharp peak mainly located at 420 °C, assigned to the reduction peak of large particles of NiO [31,32]. The broad reduction peak of the 1%Ni/SBA-15(P) catalyst was between 300–650 °C, and the reduction peak of more than 500 °C was attributed to the reduction of highly dispersed NiO, which had a strong interaction with the SiO2 [31,33,34,35,36]. The TPR results show that Ni was strongly interacted with the support of SiO2 in the 1%Ni/SBA-15(P) [21,37].

3.2. Catalytic Performance

The catalytic results are shown in Figure 5. The CO2 conversion and CO selectivity of the two catalysts increased gradually with the increase of temperature. The 1%Ni/SBA-15(P) catalyst showed higher CO2 conversions than the 1%Ni/SBA-15 catalyst at the same temperature. The CO2 conversion of the 1%Ni/SBA-15(P) catalyst at 700 °C was 33.7%, which was three times that of the 1%Ni/SBA-15 catalyst. Because methanation is an exothermic reaction, low temperatures are more conducive to producing methane on the basis of thermodynamics. The CO selectivity of the 1%Ni/SBA-15(P) catalyst was 96.7% at 500 °C, and it increased to 99.8% at 700 °C. Combined with characterization results, the high activity of 1%Ni/SBA-15(P) was due to the small nickel particles in the catalyst.
The stability study of the 1%Ni/SBA-15(P) catalyst is shown in Figure 6. The CO2 conversion was about 35%, and the CO selectivity was higher than 99.8% during 1000 min. The catalytic results show that the 1%Ni/SBA-15(P) catalyst was stable in the RWGS reaction at 700 °C. Combined with characterization results, the excellent stability should be attributed to the confined effect of SBA-15. The mesoporous confinement and metal-support interaction [38] can enhance the thermal stability of the nickel particles and inhibit sintering.
Table 2 lists the catalytic performance of 1%Ni/SBA-15(P) and recently reported RWGS catalysts, and the 1%Ni/SBA-15(P) catalyst exhibits excellent RWGS catalytic performance.
In summary, the 1%Ni/SBA-15(P) was active and stable during the RWGS at high-temperature. The characteristic results proved that the NiO particles were highly dispersed and confined in mesoporous SiO2 channels for the 1%Ni/SBA-15(P) catalyst, and the nickel strongly interacted with SiO2 support. Based on the characterization and catalytic test results, the good activity and stability of the 1%Ni/SBA-15(P) catalyst was due to the small Ni particle and enhanced interaction between Ni and SiO2.

4. Conclusions

A highly dispersed 1%Ni/SBA-15(P) catalyst, with Ni particle size at about 3 nm, was synthesized, which was highly active and stable during the high-temperature RWGS reaction. Based on the characterizations, it was proposed that the excellent catalytic performance was due to the small Ni particles and the metal-support interaction.

Author Contributions

Conceptualization, L.W.; data curation, H.L.; funding acquisition, L.W.; investigation, H.L.; writing—original draft, H.L. and L.W.; writing—review and editing, H.L. and L.W. All authors have read and agreed to the published version of the manuscript.


This research was funded by the Natural Science Foundation of China, grant number 21406206.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

All data included in this study are available upon request by contact with the corresponding author.


We thanks Han Ye for catalytic performance measurements.

Conflicts of Interest

The authors declare no conflict of interest.


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Figure 1. (a) N2 adsorption-desorption isotherms and (b) pore size distributions of SBA-15, 1%Ni/SBA-15, and 1%Ni/SBA-15(P).
Figure 1. (a) N2 adsorption-desorption isotherms and (b) pore size distributions of SBA-15, 1%Ni/SBA-15, and 1%Ni/SBA-15(P).
Crystals 11 00790 g001
Figure 2. TEM images of fresh catalysts: (a,b) 1%Ni/SBA-15 and (c,d) 1%Ni/SBA-15(P).
Figure 2. TEM images of fresh catalysts: (a,b) 1%Ni/SBA-15 and (c,d) 1%Ni/SBA-15(P).
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Figure 3. (a) Small-angle and (b) wide-angle XRD patterns of fresh and reduced catalysts.
Figure 3. (a) Small-angle and (b) wide-angle XRD patterns of fresh and reduced catalysts.
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Figure 4. H2-TPR profile of the fresh 1%Ni/SBA-15 and 1%Ni/SBA-15(P) catalysts.
Figure 4. H2-TPR profile of the fresh 1%Ni/SBA-15 and 1%Ni/SBA-15(P) catalysts.
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Figure 5. The catalytic performances of 1%Ni/SBA-15 and 1%Ni/SBA-15(P) catalysts in the RWGS reaction: (a) CO2 conversion, (b) CO selectivity.
Figure 5. The catalytic performances of 1%Ni/SBA-15 and 1%Ni/SBA-15(P) catalysts in the RWGS reaction: (a) CO2 conversion, (b) CO selectivity.
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Figure 6. The catalytic stability of the 1%Ni/SBA-15(P) catalyst at 700 °C: (a) CO2 conversion, (b) CO selectivity.
Figure 6. The catalytic stability of the 1%Ni/SBA-15(P) catalyst at 700 °C: (a) CO2 conversion, (b) CO selectivity.
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Table 1. Physicochemical properties of catalysts.
Table 1. Physicochemical properties of catalysts.
SamplesBET Surface Area (m2 g−1)Pore Volume (cm3 g−1)
Table 2. CO2 conversion rate and CO selectivity of 1%Ni/SBA-15(P) and reported RWGS catalysts in References.
Table 2. CO2 conversion rate and CO selectivity of 1%Ni/SBA-15(P) and reported RWGS catalysts in References.
CatalystsMetal Loading
CO2 Conversion Rate
CO Selectivity
1%Ni/SBA-15(P)15003.2196.7This work
6005.3698.0This work
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Liu, H.; Wang, L. Highly Dispersed and Stable Ni/SBA-15 Catalyst for Reverse Water-Gas Shift Reaction. Crystals 2021, 11, 790.

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Liu H, Wang L. Highly Dispersed and Stable Ni/SBA-15 Catalyst for Reverse Water-Gas Shift Reaction. Crystals. 2021; 11(7):790.

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Liu, Hui, and Luhui Wang. 2021. "Highly Dispersed and Stable Ni/SBA-15 Catalyst for Reverse Water-Gas Shift Reaction" Crystals 11, no. 7: 790.

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