Low-temperature catalytic CO2 dry reforming of methane on Ni-based catalysts: A review

Fuel Processing Technology 169 (2018) 199–206

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Review

Low-temperature catalytic CO2 dry reforming of methane on Ni-based catalysts: A review

MARK

Ye Wanga, Lu Yaob, Shenghong Wanga, Dehua Maob, Changwei Hua,b,⁎ a b

College of Chemical Engineering, Sichuan University, Chengdu, Sichuan 610065, PR China Key Laboratory of Green Chemistry and Technology, Ministry of Education, College of Chemistry, Sichuan University, Chengdu, Sichuan 610064, PR China

A R T I C L E I N F O

A B S T R A C T

Keywords: Ni-based catalyst Low-temperature activity Reduction temperature Active site CO2 dry reforming of methane

CO2 dry reforming of methane (DRM) not only utilized the two greenhouse gases, CO2 and CH4, but also produced synthesis gas, which could be used for Fischer-Tropsch synthesis. Besides, DRM reaction could utilize marsh gas and the gaseous products from pyrolysis of biomass, consequently increasing their value for businesses and reducing environment pollution, thereby providing ways for sustainable development. Nickel based catalyst was widely used in DRM reaction. This paper reviewed the recent progresses of the DRM reaction at low temperature. Suitable supports and promoters improved the catalytic performance by adjusting the interaction between nickel and the support. Besides, the temperature of calcination, the order of materials loading on support, the reduction temperature, and the nickel particle size also altered the performance of the catalysts. It was suggested that by investigating the interaction of supports, promoters with nickel, as well as their structural adjustment, the development of low temperature DRM catalysts was feasible.

1. Importance of the CO2 dry reforming of methane Carbon dioxide reforming of methane also called dry reforming of methane (DRM) is of significant importance because of at least the following reasons. Firstly, since CO2 and CH4 were both greenhouse gases, the utilization of CO2 and CH4 could provide a way to reduce the greenhouse effect [1–4]. Secondly, CO2 and CH4 were also produced in the pyrolysis of biomass, then the utilization of CO2 and CH4 could also make more valuable the pyrolysis gases, enhancing the whole process more practical [5–7]. Thirdly, because the main components of the marsh gas from digestion were CO2 and CH4, the utilization of CO2 and CH4 could provide a way to make the biogas value-added [8,9]. However, if pyrolysis gases and biogas were directly used as fuel, the purification of the gases to remove CO2 was generally needed, since CO2 could not contribute to combustion, providing heat. Gases with high content of CH4 could also be used in fuel cells for electricity generation, and synthesizing organic compounds such as CHFCl2, CCl4, CH3OH and HCOOH [10–13]. On the other hand, in addition to the use of CO2 in beverage additives, CO2 could be used in supercritical extraction agent and synthesizing polyketide and polycarbonate [14–16]. Whereas DRM reaction utilizes directly both CO2 and CH4 simultaneously, which reduces the step of separation. Hence the DRM reaction is an effective way for the protection of environment and the effective utilization of energy resource, thereby providing ways for sustainable development

⁎

[3,17,18]. It is well known that the CeH bond in CH4 is difficult to be activated [19,20], while CO2 is the upmost oxidized state of carbon, which is also very stable [21–23]. The co-activation of both CeH bond in CH4 and CeO bond in CO2 faced challenging difficulties. Besides, because of the thermodynamics limitation, DRM reaction was usually performed at high temperature (~ 800 °C) [24–28]. Much progresses and significant achievements have been made for high temperature DRM [29–33], whereas the development of catalysts for the DRM reaction at low temperatures reaction (below 700 °C) was relatively scarce. In addition to high operating costs, high-temperature operation usually caused metal Ni sintering and coke formation, which would lead to catalyst deactivation [32,34–37]. Although many efforts, such as core-shell structure catalyst, have been made in solving the problems, the solution was far from being perfect [35,38–42]. Sibudjing Kawi [43] reviewed the advances in synthesis of high activity and stability Ni-based catalysts for DRM with emphasis on in-depth mechanism and reaction pathways on high stability and activity. Yasotha Kathiraser [44] underlined the importance of the kinetics and mechanistics in DRM reaction over Ni-based catalysts for the optimization of catalyst design and synthesis. Ziwei Li [45] also stressed the importance of the kinetic and mechanistic on DRM reaction over core/yolk-shell nanocatalysts. According to detailed theoretical thermodynamic calculation of DRM reaction [46], as shown in Fig. 1a, the equilibrium conversions of

Corresponding author at: College of Chemical Engineering, Sichuan University, Chengdu, Sichuan 610065, PR China. E-mail address: [email protected] (C. Hu).

http://dx.doi.org/10.1016/j.fuproc.2017.10.007 Received 4 June 2017; Received in revised form 1 October 2017; Accepted 7 October 2017 0378-3820/ © 2017 Elsevier B.V. All rights reserved.

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Fig. 1. The detailed theoretical thermodynamics calculation of DRM reaction. Condition: F(CH4) = F(CO2); p = 1 atm.

particle. Bradford et al. [50] prepared different Ni based catalysts for low temperature DRM reaction, and found that the Ni/TiO2 catalyst showed the highest activity with CH4 conversion of 3.2% at 450 °C, due to the strong interaction of the metal and support, which would increase the electron density in the metal crystallites, thereby enhance the ability to activate CeH bond of methane. They also found that during the reduction process, TiOx species would form, and the interaction of the nickel and TiOx would increase the activity of the catalyst [51]. Ni/ MgO [50] catalyst showed the lowest activity and highest stability. XRD and chemisorption results showed that Ni/MgO possessed strong NieO bond. It could be verified that the solid solution NiO-MgO formed, which directly increased the stability of the NieNi bonds, due to excessive strength of strong electron donor. Besides, Ni/ZrO2 [60] catalyst showed higher activity than Ni/CeO2 at 700 °C due to the high surface area and controlled porosity. The small nickel particles deposited in the hole rather than on the surface of ZrO2, thus achieving nanoparticles and better nickel dispersion. Ni/CeO2 [60] and Ni/SiO2 [69] also possessed high surface area, however they showed lower activity on DRM reaction. It was observed that the interaction of nickel and SiO2 on Ni/ SiO2 catalyst was weak, whereas the strong interaction of the nickel and CeO2 did not contribute to the enhancement of activity of Ni/CeO2 catalyst. The reverse water-gas shift reaction took place preferably at low temperature on Ni/CeO2 catalyst during the process of DRM reaction, which led to decrease of hydrogen selectivity. Zhang et al. [72] reported that the novel Ni/La2O3 catalyst exhibited an excellent activity at 550 °C reaction temperature and the activity increased within 5 h, which suggested that new active site formed under reaction conditions. However, because of the weaker interaction of the nickel and support SiO2 or C [20,50,75], Ni/SiO2 and Ni/C catalysts formed filamentous carbon under reaction conditions leading to the deactivation of the catalysts [50]. The above reports indicated that the nature and strength of the interaction of nickel with the supports would alter the performance of the catalysts. For example, the formation of solid solution NiO-MgO could enhance the stability of the catalyst. Ni/TiO2 catalyst showed high activity attributing to the strong interaction of nickel and TiO2, however, the strong interaction of the nickel and CeO2 did not contribute to the enhancement of activity of Ni/CeO2 catalyst. To adjust the interaction of the nickel and supports, composite carriers were used to obtain higher activity for low temperature DRM reaction. Li et al. [62] prepared a series of Ni/BaTiO3-Al2O3 catalysts with different content of BaTiO3 for low-temperature DRM. At 690 °C, the Ni/32.4%BaTiO3-Al2O3 catalysts showed the best activity and stability during 50 h time-on-stream. It was deemed that BaTiO3 improved the dispersion of the active nickel and the NiOx species with weakened electronic donor intensity, and then enhanced the stability of the catalyst.The initial CH4 conversion on Ni/32.4%BaTiO3-Al2O3, Ni/BaTiO3

CH4 and CO2 at 300 °C for DRM reaction were about 60% and 50%, respectively. Another detailed theoretical thermodynamic calculation of DRM reaction by Patrick Da Costa [2], showed that hydrogen could be generated starting at about 100 °C, while carbon monoxide might be produced starting at about 300 °C, as shown Fig. 1b. So the activation of both CH4 and CO2 at low temperature was thermodynamically feasible, which required the development of new efficient catalyst. Therefore, it is necessary to develop catalysts for low temperature DRM reaction, and more and more researchers [1,2,20,47–76] started to study low temperature (under 700 °C) CO2 dry reforming of methane. Noble metal catalysts such as Pt [2,47], Rh [51,58,64], Ir [56] were widely explored, due to the high activity and preference resistance to deactivation. These active materials showed high activity and stability at low temperature (about 450 °C) for DRM reaction [51]. Taking the cost into account, more and more researchers turned their interests to nickel based catalyst on DRM reaction [77]. However, if nickel catalyst is applied at low temperature for DRM reaction, several challenges arise. Firstly, the activity was very low on the presently investigated nickel based catalysts [20,48,50,51,75]. Secondly, the catalyst deactivates rapidly due to formation of NiO shells covering Ni particles [69,78]. Thirdly, the coke deposition on the active metal owing to the methane direct decomposition reaction (1) and CO disproportionation reaction (2) [32,36,52,53,79,80] also deactivates the catalysts.

CH4 → C + 2H2

(1)

2CO → C + CO2

(2)

In the present work, we reviewed the recent advances in the development of Ni-based catalysts for low temperature DRM, with emphasis on the relationship between composition structure and performance of the catalyst. The effects of supports, promoter and several other preparation parameters on the low temperature DRM reaction were also discussed. Several suggestions for further development of low temperature DRM catalysts were provided. 2. The effect of several parameters on low temperature DRM Many attempts had been made to achieve activation of both CH4 and CO2 on Ni-based catalysts at relatively low temperature. The activity of most of the previously reported Ni-based catalysts for low temperature DRM reaction is shown in Table. 1. 2.1. The effect of nickel-support interaction on the performance of DRM Researchers investigated mechanistically the interaction between nickel and various supports. The interaction of metal and support would have effect on the electronic effects, dispersion and size of nickel 200

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Table 1 The property of the different catalyst at various temperature. Catalysts

Ni/32.4%BaTiO3-Al2O3 5% Ni/Ce0.6Zr0.4O2 HN3(La/Ni-Mg-Al) Ni/SBA-15(RM) Ni/SBA-15(PM) Ni-Ce/SBA-15 HN2(La/Ni-Mg-Al) H-19Ni TH-25Ni HT-NiAl HTNi-Ce Ni/Al2O3-CeO2 H-ZrCe0.3 Ni/SiO2 Pt/Ni/Mg/Ce0.6Zr0.4O2 Ni/ƴ-Al2O3 ZrOx/Ni-MnOx/SiO2 Ni-CaO/La2O3-ZrO2 NiSc/Al2O3 Ni-Zr/SiO2 6.8%Ni/SiO2 1.2%Ni/TiO ZrOx/Ni-MnOx/SiO2 Ni-Zr/SiO2 Ni/ƴ-Al2O3 1%Ni/10%La-ZrO2 a b c

Usage amount (g)

0.15 0.55 nd nd nd 0.2 nd nd 0.2 nd nd 0.1 nd 0.12 0.08 0.2 0.25 0.01 0.15 0.25 nd nd 0.25 0.25 nd 0.2

Ni loading (%)

5 5 15 10 10 5 15 19.5 25 63.5 7.2 10 17.5 1 8 5 10 5 11 10 6.8 1.2 10 10 10 1

Reduction conditions (°C)

700 650 900 750 750 650 900 900 900 900 900 700 900 500 300 500 550 500 900 450 500 500 550 550 270(50w) 750

Reaction conditions

Conversion/%

Temp. (°C)

CH4:CO2:N2(Ar)

GHSV/h− 1

CH4

CO2

690 650 600 600 600 600 550 550 550 550 550 550 550 500 454/432a 500 500 450 450 450 450 450 400 400 270(50w)b 150(80w)

1:1:0 1:1:0 1:1:8 1:1:0 1:1:0 1:1:0 1:1:8 1:1:8 1:1:8 2:1:7 1:1:8 1:1:0 1:1:8 2.2:1.8:6 7:7:86 15:15:70 1:1:0 1:1:1 1:1:0 1:1:0 1:1:1.8 1:1:1.8 1:1:0 1:1:0 1:1:0 1:1:2

24,000 37,600 20,000 20,000 20,000 264,000 20,000 20,000 20,000 20,000 20,000 24,000 20,000 180,000 68,000 18,000 24,000 5882 nd 24,000 nd nd 24,000 24,000 20,000 nd

88 53 49 65 68 100 33 41 45 48 30 50 23.5 7 10 12 17.9 9.8 10 6.5 2.9 3.2 2.2 2 56.4 74.5

88 53 52 88 75 90 36 45 40 54 37 55 31 13 10 15 23.6 12.9 12 9.1 6.5 5.9 4.9 2 30.2 85.3

H2/CO

Ref.

ndc 0.92 0.87 0.83 0.87 0.96 0.85 0.88–1.23 0.8–1.25 1.05 0.74 0.64 0.7 0.4–0.15 0.23 nd 0.64 nd nd 0.61 nd nd 0.56 0.67 0.91 0.83

[62] [60] [63] [57] [57] [59] [63] [54] [53] [52] [90] [91] [85] [1] [2] [48] [75] [49] [89] [20] [50] [50] [75] [20] [77] [93]

The lowest CH4 and CO2 conversion (×10) were achieved at 454 °C and 432 °C. The condition of plasma at 50 w was correspond to 270 °C. No data.

greater than that in the Al2O3 support. Comparing to one-component carriers, composite carriers could modify the interaction of nickel and supports more easily, thereby enhancing the dispersion and reducibility of nickel and then improving the property of catalysts. However, it is very difficult to modify the evenness of inner tissue of composite carriers. Supports with special structure were also employed to enhance the performance of catalysts for low temperature DRM reaction. Mesoporous material could limit the nickel particle in the hole of the mesoporous leading to the nickel particle maintaining the original state during the reaction [49,57,59,69], thus improve the performance of the catalysts. Sokolov et al. [69] studied DRM reaction at 400 °C, and discussed the influence of the morphology of the La2O3-ZrO2 support on catalytic stability. They prepared nonstructured (LaZr-ns), mesostructured (LaZr-meso) and macropore skeleton (LaZr-macro) supported Ni catalysts, and tested the stability of the catalyst at 400 °C for 100 h. Ni/LaZr-meso catalyst not only showed as high activity as Ni/LaZr-ns catalyst, but also remained high stability in 180 h. Those facts indicated that Ni/LaZr-meso catalyst exhibited high stability for DRM reaction at low temperature. Sokolov et al. found that the interaction of NiOx species and mesoporous support promoted the stability of mesoporous Ni/La2O3-ZrO2 catalyst due to the pore confinement effect and high dispersion of NiOx species. Galvez et al. [57] compared three preparation methods of Ni/SBA-15 catalysts (IM, PM and RM) for DRM reaction,and analyzed the influence of preparation method on activity, stability and selectivity at 600 °C DRM reaction. IM catalyst was prepared by the traditional wetness impregnation method, PM catalyst by the precipitation method, and RM catalyst by chemical reduction-precipitation method with the ascorbic acid reductant. They found that the conversion of methane decreased from 52% to 40% in 24 h, and the CO2 conversion decreased from 87% to 69% on IM catalyst. However, the PM and RM catalysts showed a higher stability over time on stream. The activity of PM catalyst was a little higher than that of RM catalyst. They found that the nickel particle restrained by the pore on the PM

and Ni/Al2O3 catalysts at 690 °C was 88%, 80% and 86%, respectively. The activity and the stability of the catalyst were enhanced by adding BaTiO3 to Al2O3, due to the discontinuous dispersion of BaTiO3 particles on the surface of γ-Al2O3 forming individual isolated BaTiO3 particles, and the simultaneous formation of BaAl2O4, thereby decreasing the formation of NiAl2O4. Besides, the interaction of nickel and support could be adjusted by introducing BaTiO3 to γ-Al2O3, because the interaction of nickel and BaTiO3 was weaker than γ-Al2O3. Consequently, NiOx species would be reduced easier, which increased the activity of the catalyst. Kumar et al. [60] found that the 5% Ni/Ce0.6Zr0.2O2 (CTAB) catalyst showed higher activity at 650 °C and 700 °C than Ni/ CeO2 or Ni/ZrO2. The conversion of CH4 after 70 h was above 68% at 700 °C. Kumar et al. suggested that the nickel particle was smaller on CexZr1 − xO2 support than that on CeO2 or ZrO2 supports, due to the interaction of the nickel and support, and the enhanced nickel dispersion. CexZr1 − xO2 support also possessed defect structure due to the formation of the solid solution and the high oxygen mobility, which led to celerity oxidoreduction ability by releasing and getting oxygen rapidly [60,67,81,82]. The 5% Ni/Ce0.6Zr0.2O2 (CTAB) catalyst showed remarkable stability due to the cubic CexZr1 − xO2 support possessing the ability to offer mobile oxygen species to nickel particles. TPO experiment indicated that Ni/CexZr1 − xO2 catalyst inhibited carbon deposition and H2-TPR analyses showed that CexZr1 − xO2 solid solution could enhance reducibility. Elsayed [2] also found that Ce would enhance the medium base site due to the ability of rapidly releasing and getting oxygen. Lemonidou et al. [61] studied the 5 wt% Ni/CaO-Al2O3 catalyst for DRM reaction. At 600 °C, the 5 wt% Ni/CaO-Al2O3 catalyst exhibited high stability and the activity did not decrease even over testing time of 50 h. It was found that CaO-Al2O3 support increased the stability of the catalyst due to the strong interaction between the support and metal. Z L Zhang [73] and co-workers also studied the influence of CaO promoter consisted in Ni/Al2O3 catalyst, and indicated that in the presence of CaO, the catalyst activity and stability increased because the fraction of free Ni existed in CaO/Al2O3 support was 201

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CO2 adsorption. The catalyst showed high activity at 550 °C, and the order of methane conversion was H-19Ni > H-18NiCe > 10Ni/ Al2O3 > 10Ni/CZ ≈ H-8Ni,while the order of CO2 conversion was H18NiCe > H-19Ni > 10Ni/Al2O3 > H-8Ni > 10Ni/CZ. Debek et al. [53] also examined the influence of promoters Ce, Zr and CeZr for NiMg-Al hydrotalcite-derived catalyst for DRM reaction at 550 °C. They evidenced that with the introduction of Zr promoter, CO2 adsorbed preferentially in weak basic sites and formed active carbonate species which could react with methane. Comparing with other catalysts, the catalytic activity on Zr-promoted catalyst decreased obviously with time-on stream and the ratio of H2/CO was the lowest, due to the Zr contributing to both DRM reaction and reverse Boudouard reaction. Liu et al. [63] found that the promoter La would increase the medium strength and weak basicity, thereby enhance the activity of the catalyst. U·Oemar et al. [86] also found that La promoted the adsorption of CO2 and removed coke, due to the basic property of La. It is well known that potassium was a good catalyst for carbon gasification, because the electronic effect of alkali atoms could lead to a weakening of the strength of CeO bond [87]. Barroso-Quiroga et al. [79] prepared Nibased catalysts modified by alkaline (Li or K) for DRM reaction, and found that at 550 °C, Ni/CeO2 catalyst showed the highest initial conversion of both CH4 (11.7%) and CO2 (29.7%) comparing to other catalysts, whereas the Ni/CeO2 catalyst promoted by K or Li showed a better stability during the process of reaction, due to the methane cracking and the enhancement of carbon gasification. However, the activity of modified catalyst was lower than Ni/CeO2 catalyst, because the alkaline metals blocked the Ni active sites [88]. Sc promoter could increase strong and moderate basic sites, thereby enhancing the ability of CO2 adsorption and the stability of the catalysts [89]. Thirdly, promoters could facilitate the formation of low temperature active site. Yao et al. [20] tested Zr promoted Ni/SiO2 catalyst for DRM reaction at 400 °C. They found that the conversion of CH4 and CO2 at 750 °C was 0.7% and 0.2% respectively over Ni/SiO2. With the introduction of Zr promoter, the initial conversion of both CH4 and CO2 on Ni-Zr/SiO2 catalyst could reach 2% at 400 °C. The temperature programmed reaction of the CH4 and CO2 showed that the CH4 activation started at 400 °C on the Ni-Zr/SiO2 catalyst, compared to that at 750 °C on the Ni/SiO2 catalyst. The in situ DRIFTS results showed that Zr promoted the production of COads and Oads at low temperature, and accelerated the formation of reactive intermediate species resulting in increasing reaction of CH4 and CO2 on Ni-ZrO2/SiO2 catalyst. B·Bachiller-Baeza et al. [49] studied the effect of Ca promoter on Ni/ZrO2La2O3 catalyst for DRM reaction at 400 °C, 450 °C and 500 °C. The conversion of CH4 and CO2 over Ni-Ca-ZrLa catalyst was 65% and 85% at 500 °C, respectively. While those were 58% and 75% over non-promoted catalyst. In addition, it was found that CaO would enhance the stability of the catalyst due to CO2 adsorption on calcium forming carbonate to remove carbon deposition, consequently refresh the initial state of Ni species at Ni-O-Ca interphase. Debek et al. [90] found that Ce-promoted Ni-hydrotalcite-derived catalyst showed higher activity at 550 °C DRM reaction, because of the formation of Ni crystallites and prevention of the formation of inactive NiAl2O4 by introducing ceria promoter. Promoters could increase the reduction of nickel, basic site and form low temperature active site and thus enhance the performance of the catalysts. La could increase the reduction of nickel thus the presence of Ni0 species could activate directly the methane decomposition. Ce could increase basic site, thereby enhance the ability of CO2 adsorption. Zr could help to form low temperature active site, then decrease the reaction temperature.

and RM supports, but most nickel particle loaded on the surface of IM support. So IM catalyst gained bigger NiO particle about 12 nm on average size. Nickel particle on RM catalysts existed in small NiO particle about 5 nm on average size. This was the reason why the catalytic activity on the RM catalyst was higher than on IM catalyst. Moreover, PM and RM catalysts were more stable than IM due to the fact that the nickel particle on the PM and RM catalysts were inside the mesoporous of SBA-15, leading to the deposition of carbon on the surface of the silica particles rather than on the nickel particle to slow down the deactivation. Furthermore, amorphous carbon preferred to form on RM catalyst. This was another reason for the high stability of RM catalyst. The addition of reductor ascorbic acid in the preparation of Ni/SBA-15 catalyst would enhance the catalytic activity, selectivity and stability for low temperature DRM reaction, because both NiO and Ni-phyllosilicates formed inside the pore of SBA-15. Hydrotalcite derivative had been widely studied in low temperature DRM reaction [52–54,63]. Debek et al. [52] found that hydrotalcite-derived materials (HT-MgAl) had no catalytic activity at 550 °C. However the Ni-containing hydrotalcite-derived materials (HT-NiAl) showed high activity under the same conditions and the average conversion of the CH4 and CO2 was 48% and 54%, respectively. It was suggested that hydrotalcite derivative was beneficial to the catalytic performance for DRM reaction at low temperature on account of the mixed oxide showing the periclase-like structure. Besides, the interaction between nickel species and supports could be controlled, thereby restraining the sintering of nickel and preventing the inactive phases formattion simultaneously, such as NiAl2O4 or NiO-MgO solid solution [3]. Wang et al. [71] found that the fibrous Ni/Al2O3 catalyst at 500 °C showed high structural stability, because the fibrous structure could cause higher resistance to sintering than traditional supported catalysts. The supports possess the periclase-like structure and mesoporous structure would enhance the activity for low temperature DRM reaction. Those special material supports would exert effect on nickel particle size and dispersion of nickel, thereby improve the property of the catalysts for low temperature DRM reaction. 2.2. The promoter effect on the catalytic performance for low temperature DRM Promoters could enhance the activity of nickel-based catalyst via several mechanisms. Firstly, promoters could increase the reduction of nickel oxide. Liu et al. [63] studied the effect of La promoter for low temperature (550 and 600 °C) DRM reaction. They found that the addition of lanthanum would enhance the reduction of the nickel leading to Ni0 species existing in the La-promoted catalyst. The H2/CO increased with time-onstream, because of the improvement of direct methane decomposition reaction, corresponded to the presence of Ni0 species. The conversion of CH4 and CO2 on HN2 catalyst (Ni0.215La0.012Mg0.535Al0.238) containing 2 wt% La for DRM reaction at 550 °C was 33% and 36%, respectively, which was higher than non-promoted catalyst. Debek et al. [54] also studied the Ce-promoted Ni-containing hydrotalcite derived catalyst for DRM reaction and found that Ce promoter could increase the reduction of the nickel particle. The H2-TPR results showed that the reduction peak of Ni-phase shifted to low temperature in the presence of promoter Ce, because the Ce3 +/Ce4 + redox pairs could transfer electron, which promoted the reduction of nickel oxides in the nearby site [83]. Albarazi et al. [84] researched the effect of Ce0.75Zr0.25O2 mixed oxide on the performance for low temperature DRM reaction. The H2-TPR results showed that Ce0.75Zr0.25O2 mixed oxide could increase the content of nickel that could be reduced below 600 °C, thus enhance the reduction of the nickel particles. Secondly, promoters could increase the basic site, which could perfect the performance of the catalysts. Debek et al. [53,54,85] found that Ce promoter would increase the moderate alkaline sites and new strong low-coordinated oxygen species, thereby enhancing the ability of

2.3. Several other preparation factors influencing the activity for low temperature DRM Wang et al. [71] studied the effect of different calcination temperature on the performance of Ni/Al2O3 catalyst for DRM reaction. 202

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the formation of separated Ni0 species not the inactive MoNi4. Zhang et al. [72] investigated the influence of various pretreatment (under O2, air, H2, CO2, and CH4) on the activity of Ni/La2O3 catalysts. They found that the activity of all catalysts was increased within 5 h, stabilizing at RCO ~2.0 mmol sg− 1. It was suggested that new active site formed under the reaction conditions. Besides, when the catalyst was exposed to O2 (or H2) at 1023 K, CO2 (or CH4) outflowed, which indicated that the structure of new site was destroyed. However the new site could form again during the process of reaction. Zhang et al. [72] thought that the formed new active site was NieC compound, which would affect the activity for low temperature DRM reaction. Sergey [69] tested in a parallel reactor consisting of 50 single fixedbed with a flow rate of 12 ml/min per reactor, thereby increased the interface of the catalyst and reactants, and enhanced the catalytic activity. X. Tu [77] investigated the influence of plasma-catalyst on activity for low temperature DRM reaction. They found that Ni/γ-Al2O3 catalyst showed high activity at 50 W condition that corresponds to 270 °C, while the synergistic effect of the low-temperature plasma and solid catalyst could improve the activity of catalyst. Yabe [93] found that 1 wt%Ni/10 mol%La-ZrO2 catalyst in 6.9 w electric field equivalently at 423 K showed high DRM activity with about 77.2% CH4 conversion and 87.6% CO2 conversion. The catalyst could be restructured in the electric field, thereby enhancing the performance of the catalysts [94].

They found that the reaction rate at 500 °C decreased with increasing calcination temperature, and the highest CH4 reaction rate was 3.5 mol/g.min when the catalyst was calcined at 700 °C, while reaction rate was 1.0 mol/g.min when the catalyst was calcined at 1000 °C. Wang found that the activity of the fibrous Ni/Al2O3 catalyst decreased with the calcination temperature, because the formation of NiAl2O4 crystal at high temperature led to high reduction temperature to reduce the catalyst. Baudouin et al. [1] investigated the effect of the particle size on Ni/ SiO2 catalyst in low temperature (500 °C) DRM reaction. They found that when the Ni particle sizes varied from 1.6 to 7.3 nm, with the particle size decreasing, the nickel dispersion increased and then the activity for low temperature DRM reaction increased. Kaydouh et al. [59] found that the order of Ni and Ce addition in SBA-15 could influence the activity of the catalyst. The Ni-Ce/SBA-15 (Ce impregnated first) exhibited highest activity on DRM reaction at low temperature. Because the channel blocked by Ce would decrease the size of nickel particles and enhance the nickel reducibility if Ce was impregnated firstly. However, if Ni species deposited previously, nickel would load in the pores and form larger NiO particles thereby hindering the reactants to contact the active sites. Aghamohammadi et al. [91] investigated the effect of synthesis method on DRM reaction and found that the sol-gel synthesized Ni/Al2O3-CeO2 catalyst exhibited higher activity comparing with the traditional impregnation method, due to the former possessing higher dispersion of active phase. Thawatchai Maneerung et al. [29] also found that the smaller and more uniform catalyst particles could contribute to the catalytic performance for decomposition of methane. Optimization of the preparation method of the catalysts could enhance the performance of the catalyst. Such as the calcination temperature, the content of nickel and the order of mater loading. Simultaneously, the size of nickel particles could affect on the performance of the catalyst.

4. Carbon deposition Carbon deposition was one of the main issue for the deactivation of Ni-based catalysts on low temperature DRM reaction. Thus, many researchers investigated how to decrease the coke or restrain the formation of coke, as shown in Table 2. Generally, there were several methods to decrease the carbon deposition [62,63,69,85,93,95,96]. Firstly, the enhancement of the ability for carbon deposition elimination could decrease the formed coke during the low temperature DRM reaction. Debek [85,96] found that Ce and Zr promoters could increase the basic sites, thereby enhancing the ability of CO2 adsorption, which contributed to eliminating carbon deposition, and, as a consequence, could enhance the stability of Ni-based catalysts. Besides, the ratio of Ce/Zr could also influence the carbon deposition, and the HZrCe1.2catalyst (Ce/Zr loading of 1.2) exhibited the least carbon deposition and highest stability comparing to those on H-ZrCe0.6 (Ce/Zr loading of 0.6) and H-ZrCe0.6 (Ce/Zr loading of 0.3) catalysts. According to the results of CO2-TPD, H-ZrCe0.6 and H-ZrCe0.6 catalysts showed higher concentration of strong basic sites than HZrCe1.2catalyst, leading to too strong CO2 adsorption on H-ZrCe0.6 and H-ZrCe0.6 catalysts, and then promoting carbon deposition. Liu et al. [63] found that a moderate amount of La promoters could increase the formation of strong and medium strength basic sites, thereby enhancing the ability of CO2 adsorption and elimination of carbon deposition. Thus, the content of coke on La-promoted catalyst (12.6 mg) was lower than non-promoted catalyst (16 mg). In addition, La-modified Ni-based catalysts could promote the formation of oxycarbonate species to gasification of amorphous carbon deposition, and, as a consequence, showed lower carbon deposition at 550 °C DRM reaction for 500 min. K. Stthiumporn et al. [31] found that La0.8Sr0.2Ni0.8M0.2O3 perovskite modified by Fe could contribute to the formation of abundant lattice oxygen species, which reacted with CO2 forming La2O2CO3, thereby removed the surface carbon. U·Oemar [33] also found that the surface oxygen species on catalysts could react with the coke, thereby decrease the carbon deposition. Scondly, the enhancement of the ability of carbon deposition resistance could decrease the formed coke during the low temperature DRM reaction. Xu et al. [95] found that core-shell structure NiO-MgO@ SiO2 catalyst exhibited higher carbon deposition resistance than traditional NiO-MgO/SiO2 catalyst at 670 °C. Thus, the former showed lower coke (only 5% weight loss in TG), whereas NiO-MgO/SiO2 catalyst with

3. The effect of process parameters on the property of the catalyst Yao et al. [75] found that ZrOx/Ni-Mn/SiO2 catalyst was effective for DRM reaction at low temperature, and the reduction temperature of the catalyst would affect the catalytic activity. When reduction temperature increased from 400 °C to 550 °C, the initial conversion of CH4 and CO2 at 400 °C increased from 1.6% and 1.5% to 3.3% and 4.9%, respectively. Besides, the catalytic activity decreased remarkably when the reduction temperature further increased (above 550 °C). When the reduction temperature increased to 800 °C, the low temperature (400 °C) catalytic activity of the catalyst was lost completely. At both 500 °C and 400 °C (reaction temperature), the ZrOx/Ni-MnOx/SiO2 catalyst showed the highest catalytic activity after reduction at 550 °C. The XRD and TEM results showed that the nickel particle size distribution on ZrOx/Ni-MnOx/SiO2 catalyst were quite narrow about 5–6 nm after reduction at 550 °C, whereas those was wide about 4–10 nm after reduction at 400, 450, 500 and 600 °C. Moreover, much large nickel particle size (larger than 10 nm) species was observed after reduction at 800 °C. The reduction temperature could affect the nickel particle size and the content of the surface nickel species consequently influenced the CO2 and CH4 conversion. Debek et al. [52] found that the reduction temperature could affect the catalytic activity of the catalyst, and the catalyst reduced at 550 °C exhibited lower activity than that reduced at 900 °C due to the incomplete reduction of NiO species at 550 °C. Wang [71] studied the influence of preparation methods on the reduction temperature of Ni/Al2O3 catalyst for DRM reaction. Suitable high reduction temperature would increase the catalytic activity of the fibrous Ni/Al2O3 catalyst, because high reduction temperature could enhance the dispersion of Ni particles. Yao et al. [92] found that the Ni-Mo/Al2O3 catalyst showed improved activity after reducing at low temperature (600 and 700 °C), whereas the opposite was observed after reducing at high temperature (900 °C), due to 203

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Table 2 The relationship of stability and carbon deposition. Catalysts

5wt%Ni/BaTiO3 5wt%Ni/γ -Al2O3 5wt%Ni/32.4%BaTiO3-Al2O3 Ni-MgO/SiO2 Ni-MgO@SiO2 H-ZrCe0.3 H-ZrCe0.6 H-ZrCe1.2 H-Ni NiLaMgAl(NH3) NiMgAl(HN4) HTNi25 HTNi25-Ce HTNi100 HTNi100-Ce Ni/La2O3-ZrO2-ns Ni/La2O3-ZrO2-meso Ni/La2O3-ZrO2-marco 1wt%Ni/La-ZrO2

a b c d

Reaction temperature (°C)

Reaction time (h)

Stability (h)

670

1.5 10 10 40

550

5

< 1b < 10 50 < 10 40 5

550

8.3

<5 8.3

550

5

5

400

100

700 150(8.1w)a

2.3

< 100 180 < 100 ndd

690

Carbon deposition (%)

41 17 4 23 5 40.7 43.6 11.3 ~ 55c 87.5 86.1 ~ 52 ~ 60 ~ 85 ~ 90 0.5 1.38 4.03 > 3.81 0.15

Conversion (%) CH4

CO2

~ 79 ~ 82 ~ 87 80 ~ 80 ~ 22.5 ~ 27 ~ 23 ~ 46 ~ 45 ~ 40 ~ 44 ~ 40 ~ 53 ~ 55 nd nd nd 64 77.2

nd nd nd 70 ~ 70 ~ 29 ~ 31 ~ 27.5 ~ 39 ~ 37 ~ 37 ~ 36 ~ 41 ~ 37 ~ 40 nd nd nd 77 87.6

Ref.

[62]

[95] [85]

[63] [96]

[69]

[93]

The condition of plasma at 8.1 w was correspond to 150 °C. Estimated by the graph of TOS. Estimated by the graph of TG. No data.

supports and the basic site, however too strong the electronic donor ability and too weak interaction would contribute to the deactivation of catalyst. Suitable intensity of basic site and the interaction between nickel and support could be obtained by controlling the content of nickel, the state of precursor, the kinds and content of promoter, and synthetic method.

23% weight loss. In addition, NiO-MgO@SiO2 catalyst exhibited higher stability with no lost of activity even for 40 h reaction, while the activity of NiO-MgO/SiO2 catalyst decreased within 10 h. Sokolov et al. [69] found that mesoporous supports could promote resisting formation of graphitic carbon, due to the strong interaction between nickel and mesoporous supports and highly dispersed NiOx species. As a result, Ni/ La2O3-ZrO2-meso catalyst did not lost its activity for even 180 h reaction, while the activity of Ni/La2O3-ZrO2-ns and Ni/La2O3-ZrO2-marco catalysts decreased within 100 h with a similar deactivation trends. Li et al. [62] found that the CH4 conversion on Ni/BaTiO3 catalyst at 690 °C were declined sharply, with a drop of about 45% during 4 h time on stream. Similar phenomena were observed on Ni/Al2O3 catalyst with a drop of about 11% in CH4 under the same conditions. While, the optimum Ni/32.4%BaTiO3-Al2O3 catalyst exhibited the best stability, even maintaining its activity for 50 h reaction. In parallel, the Ni/32.4% BaTiO3-Al2O3 catalyst exhibited the best carbon deposition resistance property on low temperature DRM reaction with 4% coke after reaction for 10 h at 690 °C. Because BaTiO3 could adjust the electronic donor intensity of Ni/BaTiO3-Al2O3 catalysts, thereby modified the interaction between nickel and supports and enhanced the dispersion of Ni species, resulting in higher carbon deposition resistance and stability on low temperature DRM reaction. Thirdly, optimum process parameters could decrease the carbon deposition. Yabe [93] found that Ni/La-ZrO2 catalyst showed lower carbon deposition in the electric field than traditional conditions for DRM reactions. The content of coke were 0.15% and above 3.81% in the electric field and no electric conditions, respectively. The catalyst could be restructured in the electric field, thereby decreasing the carbon deposition. T. Maneerung et al. [30] discovered that the introduction of hydrogen into feed gas enhanced the stability of catalysts, where hydrogen could react with the excess carbon, thereby reduced the rate of catalyst deactivation. Enhancement of the ability of carbon deposition elimination and carbon deposition resistance, and optimum process parameters, could decrease the carbon deposition. Ce and Zr promoters could enhance CO2 adsorption to eliminate carbon deposition. The catalysts modified by alkaline earth or rare earth could adjust the electronic donor ability, the interaction between nickel and

5. Perspectives The results of detailed theoretical thermodynamic calculation of DRM reaction [46,63] indicated that the activation of both CH4 and CO2 at low temperature was thermodynamically feasible (about 300 °C), which required the development of efficient catalyst. The above reports also suggested that low temperature DRM reaction was practicable, and the lowest temperature for the activation of both CH4 and CO2 would be about 400 °C [20,69,75]. The types and strength of interaction of nickel and supports could affect the property of the catalyst, whereas composite carriers could adjust the interaction between nickel and the supports. Besides, the stability of the catalyst could also be improved by limiting the nickel in the hole of the mesoporous of the support or by confinement of promoters to a net-barrier-like environment. Promoters could increase the reduction of nickel, the amount of basic site, and form low temperature active site and thus enhance the performance of the catalysts. In addition to the influence of supports and promoters, the temperature of calcination, the order of mater loading on support, the reduction temperature, and then the nickel particle size would influence the performance of the catalyst at low temperature. Although there are many methods to improve the performance, the low temperature CO2 dry reforming methane faced hereinafter challenges. It was unclear how the structure of the active phase at atomic level influenced on the performance of the catalyst. What is the nature of active phase at atomic level? The following are proposed to be important for the development of new lower temperature Ni-based DRM reaction catalysts. i. Design and investigation of new Ni-based low temperature (lower than 400 °C) DRM reaction catalysts via controlling and adjusting proper composition. 204

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