Bio-Oil Steam Reforming over a Mining Residue Functionalized with Ni as Catalyst: Ni-UGSO
Abstract
:1. Introduction
2. Results and Discussion
2.1. Bio-Oil Properties
2.2. Steam Reforming Results
- Increased temperature evoked higher C conversion (XC), CO and H2 yields (, ) for both bio-oils. This was in agreement with the thermodynamic analysis of bio-oil model compounds studied by many authors [20,23,40] where it is found that the reaction is endothermic. The decrease in XC, and at 850 °C in Figure 1B is an outlier; we attribute that to experimental errors, which led to higher error in the mass balance than the average.
- CO and H2 were favored at low WHSV because of increased residence time over the catalyst bed. In the MemU bio-oil (Figure 3), we observe a decrease of CO2. A higher CO, H2 production through reforming means that there is a higher H2O consumption. If the increase of CO and H2 is equal, the WGS reaction (CO + H2O = CO2 + H2) will shift in such a way to compensate the H2O decrease; this means that the CO2 will decrease. This is the case for the MemU oil whose H2O/C is low; thus, the consumption of H2O by the reforming reaction has a higher impact on WGS. In the case of WU, we do not observe this behavior because the H2O/C is much higher.
- The amount of H2O and O in the two bio-oils had a significant impact on SR performance. Comparison of bio-oil MemU (Figure 1) and bio-oil WU (Figure 2) showed that the former gave better results in terms of H2 selectivity (up to 94%) and CO selectivity (up to 84%), while selectivity was maximum 43% and 36%, respectively, for bio-oil WU SR. It appeared that a ratio of O/C ≈ 1 (bio-oil MemU) was good enough for SR with Ni-UGSO compared to O/C ≈ 3 (bio-oil WU), which suggested that the catalyst was more active at low H2O or O content.
2.3. Catalyst Characterization
2.3.1. Scanning Electron Microscopy
2.3.2. X-ray Diffraction
2.3.3. TGA Analysis
2.3.4. BET Measurement
3. Materials and Methods
3.1. Bio-Oils
3.2. Catalyst Preparation and Characterization
3.2.1. UGSO
3.2.2. Ni-UGSO
3.3. Experiments and Calculations
3.3.1. Experimental Set-Up
3.3.2. Test Conditions
3.3.3. Calculations
- The injection flowrate of the bio-oil was adjusted to ~0.1 mL/min; the amounts of C, H and O injected were calculated by multiplying mass flowrate, and the mass fraction of each element was determined by elemental analysis.
- Concentration measurements of gases by GC are reported in Table 7: the interval between each measurement was 30 min.
- The flowrate of the produced gas was measured by massflow meter and recorded.
- Using the ideal gas equation, we calculated the molar flow of each gas at 1 atm and 20 °C, and, by multiplying the stoichiometric number, we got the amount of each element at each time t, and we then summed it to obtain the total (Table 8).
- We weighed solid C deposited on the reactor wall and the liquid produced in the condenser, considering that it was composed 100% of H2O. In this example, mC = 1.63 g (0.135 mol) and mH2O = 3.43 g (nH = 0.38 mol, nO = 0.19 mol).
- We calculated the yield at each time t and for each product with Equations (6)–(9) (Table 9).
- Then, we calculated relative error between input and output and we got (Table 10).
4. Conclusions
- The catalyst was activated quickly (without a pre-reduction step).
- It was efficient at H2O/C, being 2–5 times lower than those used in industrial H2 production.
- No severe deactivation was observed in all tests, even after C formation.
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Properties | Bio-Oil MemU | Bio-Oil WU |
---|---|---|
Density | 1.187 | 1.087 |
% C * | 39.4 | 18.8 |
% H * | 7.0 | 7.9 |
% O * | 53.6 | 73.3 |
% H2O * | 34.3 | 52.3 |
pH | 2.4 | 2.9 |
H2O/C ** | 0.60 | 1.85 |
O/C ** | 1.02 | 2.92 |
Catalyst | Feedstock | Temperature (°C) | H2O/C (mol/mol) | Space Velocity (h−1) | Reactor | TOS (h) | YH2 (%) | Reference |
---|---|---|---|---|---|---|---|---|
Ni-UGSO | RBO MemU | 750–850 | 0.6 | 1.7–6.6 (W) | Fixed bed | 8.3 | 78–95 | This work |
RBO WU | 1.9 | 1.8–7.1 (W) | 16–43 | |||||
C11-NK | BOAq | 800–850 | 7–9 | 0.96–2.7 (W) | Fluidized bed | 4–90 | 77–89 | [12] |
Ni-MgO/Al2O3 | BOAq | 850 | 3.2–4.2 | 30 (W) | Fixed bed | 1 | 12–61 | [20] |
Ni/ceramic foam | RBO | 500–800 | 2.6 | 1.5–4 (W) | Fixed bed | 0.5–2 | 54.5–93.5 | [21] |
ICI 46-1/4 | BOAq | 700–75 | 5–35 | 760–1130 (G) | Fixed bed | 1–6 | 76–100 | [10] |
UCI G-91 | ||||||||
Ce-Ni/Co/Al2O3 + CO2 sorbent | RBO | 650–850 | 9–15 | 0.08–0.23 (L) | Fixed bed | 0.5 | 65–85 | [19] |
Ni/Al2O3 | BOAq | 600 | 0.5–3.5 | 1.5–3.8 (W) | Fixed bed (CLR) | 0.6–1.7 | 59–83 | [44] |
G90LDP | RBO | 550–700 | 3.9–9.7 | 2–24 (W) ** | Fluidized bed | - | 20–95 | [39] |
T = 800 °C WHSV = 2.0 g/gcat/h Δt = 105 h | Bio-Oil MemU | ||||||||
---|---|---|---|---|---|---|---|---|---|
Period (h) | (%) | (%) | (%) | (%) | (%) | (%) | (%) | (%) | (%) |
0–12 | 96.2 | 100 | 81.6 | 14.1 | 0.87 | 52.6 | 39.7 | 6.8 | 0.9 |
30–105 | 96.7 | 66.8 | 52.7 | 25.0 | 6.9 | 43.1 | 32.2 | 14.8 | 9.4 |
NiFeAlO4, MgAl2O4, FeAl2O4 | SiO2 (from quartz wool) | ||
MgO, NiO, NiO-MgO | Fe3C | ||
Ni, FeNi, Fe0.5Ni0.5, FeNi3 | Fe2O3 | ||
Carbone |
Sample | S (m2/g) | Pore Volume (cm3/g) |
---|---|---|
Fresh catalyst | 6.70 | 0.0202 |
Used catalyst (MemU) | 10.49 | 0.0241 |
Used catalyst (WU) | 8.98 | 0.0144 |
Reactant | Catalyst Weight | Temperature (°C) | Injection Flowrate | TOS |
---|---|---|---|---|
Bio-oil WU Bio-oil MemU | 1 g and 4 g | 750, 775, 800, 825, 850 | ~0.1 mL/min | ~500 min |
Bio-oil MemU | 4 g | 800 | ~0.1 mL/min | 105 h |
Time (min) | Concentration (% mol) | |||||
---|---|---|---|---|---|---|
CO2 | CO | H2 | C2H4 | C2H6 | CH4 | |
0 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 |
9 | 6.27 | 32.22 | 57.88 | 0.08 | 0.13 | 3.42 |
24 | 13.60 | 38.25 | 47.65 | 0.03 | 0.05 | 0.41 |
54 | 6.39 | 41.00 | 51.89 | 0.01 | 0.03 | 0.66 |
84 | 6.26 | 40.46 | 52.52 | 0.01 | 0.02 | 0.74 |
114 | 6.49 | 40.07 | 52.65 | 0.00 | 0.01 | 0.78 |
144 | 6.77 | 39.85 | 52.56 | 0.00 | 0.01 | 0.81 |
174 | 6.86 | 39.87 | 52.40 | 0.00 | 0.01 | 0.86 |
204 | 7.00 | 39.67 | 52.40 | 0.00 | 0.01 | 0.92 |
234 | 6.96 | 39.74 | 52.37 | 0.00 | 0.00 | 0.92 |
264 | 6.93 | 39.91 | 52.15 | 0.00 | 0.00 | 1.00 |
294 | 6.93 | 39.92 | 52.10 | 0.00 | 0.00 | 1.04 |
324 | 7.35 | 39.05 | 52.42 | 0.00 | 0.00 | 1.17 |
354 | 7.22 | 39.51 | 52.11 | 0.00 | 0.00 | 1.15 |
384 | 7.29 | 39.57 | 51.84 | 0.01 | 0.00 | 1.29 |
414 | 7.21 | 39.69 | 51.82 | 0.01 | 0.01 | 1.27 |
459 | 7.17 | 39.52 | 51.87 | 0.01 | 0.01 | 1.42 |
504 | 7.46 | 39.09 | 51.90 | 0.01 | 0.01 | 1.53 |
Time (min) | Number of Moles | ||||||||
---|---|---|---|---|---|---|---|---|---|
C in | H in | CO2 | CO | H2 | C2H4 | C2H6 | CH4 | ||
0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | |
9 | 0.0347 | 0.0742 | 0.0033 | 0.0169 | 0.0303 | 0.0000 | 0.0001 | 0.0018 | |
24 | 0.0579 | 0.1237 | 0.0153 | 0.0430 | 0.0535 | 0.0000 | 0.0001 | 0.0005 | |
54 | 0.1158 | 0.2474 | 0.0133 | 0.0852 | 0.1078 | 0.0000 | 0.0001 | 0.0014 | |
84 | 0.1158 | 0.2474 | 0.0128 | 0.0828 | 0.1075 | 0.0000 | 0.0000 | 0.0015 | |
114 | 0.1158 | 0.2474 | 0.0128 | 0.0790 | 0.1038 | 0.0000 | 0.0000 | 0.0015 | |
144 | 0.1158 | 0.2474 | 0.0137 | 0.0809 | 0.1067 | 0.0000 | 0.0000 | 0.0016 | |
174 | 0.1158 | 0.2474 | 0.0139 | 0.0810 | 0.1064 | 0.0000 | 0.0000 | 0.0017 | |
204 | 0.1158 | 0.2474 | 0.0151 | 0.0855 | 0.1129 | 0.0000 | 0.0000 | 0.0020 | |
234 | 0.1158 | 0.2474 | 0.0149 | 0.0852 | 0.1123 | 0.0000 | 0.0000 | 0.0020 | |
264 | 0.1158 | 0.2474 | 0.0145 | 0.0835 | 0.1092 | 0.0000 | 0.0000 | 0.0021 | |
294 | 0.1158 | 0.2474 | 0.0153 | 0.0884 | 0.1154 | 0.0000 | 0.0000 | 0.0023 | |
324 | 0.1158 | 0.2474 | 0.0169 | 0.0896 | 0.1203 | 0.0000 | 0.0000 | 0.0027 | |
354 | 0.1158 | 0.2474 | 0.0168 | 0.0917 | 0.1210 | 0.0000 | 0.0000 | 0.0027 | |
384 | 0.1158 | 0.2474 | 0.0171 | 0.0928 | 0.1215 | 0.0000 | 0.0000 | 0.0030 | |
414 | 0.1158 | 0.2474 | 0.0163 | 0.0897 | 0.1171 | 0.0000 | 0.0000 | 0.0029 | |
459 | 0.1737 | 0.3711 | 0.0256 | 0.1414 | 0.1855 | 0.0000 | 0.0000 | 0.0051 | |
504 | 0.1737 | 0.3711 | 0.0257 | 0.1346 | 0.1787 | 0.0000 | 0.0000 | 0.0053 | |
Element | Total Element Produced per Molecule | Total | |||||||
C | 1.9456 | 0.2633 | 1.4511 | 0.0005 | 0.0008 | 0.0400 | 1.7558 | ||
H | 4.1564 | 3.8200 | 0.0011 | 0.0025 | 0.1602 | 3.9837 | |||
O | 0.5266 | 1.4511 | 1.9778 |
Time (min) | Yield (%) | |||||
---|---|---|---|---|---|---|
CO2 | CO | H2 | C2H4 | C2H6 | CH4 | |
0 | 0.0 | 0.0 | 0.0 | 0.2 | 0.5 | 9.7 |
9 | 9.5 | 48.6 | 8.7 | 0.1 | 0.3 | 1.5 |
24 | 26.4 | 74.2 | 86.5 | 0.0 | 0.2 | 2.2 |
54 | 11.5 | 73.6 | 87.2 | 0.0 | 0.1 | 2.4 |
84 | 11.1 | 71.5 | 86.9 | 0.0 | 0.1 | 2.5 |
114 | 11.1 | 68.2 | 83.9 | 0.0 | 0.0 | 2.7 |
144 | 11.9 | 69.8 | 86.2 | 0.0 | 0.0 | 2.8 |
174 | 12.0 | 69.9 | 86.0 | 0.0 | 0.0 | 3.2 |
204 | 13.0 | 73.8 | 91.3 | 0.0 | 0.0 | 3.2 |
234 | 12.9 | 73.6 | 90.8 | 0.0 | 0.0 | 3.4 |
264 | 12.5 | 72.1 | 88.2 | 0.0 | 0.0 | 3.7 |
294 | 13.3 | 76.4 | 93.3 | 0.0 | 0.0 | 4.3 |
324 | 14.6 | 77.4 | 97.3 | 0.0 | 0.0 | 4.3 |
354 | 14.5 | 79.2 | 97.8 | 0.0 | 0.0 | 4.9 |
384 | 14.8 | 80.1 | 98.2 | 0.0 | 0.0 | 4.6 |
414 | 14.1 | 77.4 | 94.6 | 0.0 | 0.0 | 5.5 |
459 | 14.8 | 81.4 | 100.0 | 0.0 | 0.0 | 5.7 |
504 | 14.8 | 77.5 | 96.3 | 0.2 | 0.5 | 9.7 |
C in (mol) | C out (mol) | Error (%) |
1.96 | 1.89 | 3.73 |
H in (mol) | H out (mol) | Error (%) |
4.20 | 4.36 | 3.98 |
O in (mol) | O out (mol) | Error (%) |
2.00 | 2.17 | 8.25 |
Bio-Oil in (g) | Bio-Oil out (g) | Error (%) |
59.82 | 61.76 | 3.23 |
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Bali, A.; Blanchard, J.; Chamoumi, M.; Abatzoglou, N. Bio-Oil Steam Reforming over a Mining Residue Functionalized with Ni as Catalyst: Ni-UGSO. Catalysts 2018, 8, 1. https://doi.org/10.3390/catal8010001
Bali A, Blanchard J, Chamoumi M, Abatzoglou N. Bio-Oil Steam Reforming over a Mining Residue Functionalized with Ni as Catalyst: Ni-UGSO. Catalysts. 2018; 8(1):1. https://doi.org/10.3390/catal8010001
Chicago/Turabian StyleBali, Amine, Jasmin Blanchard, Mostafa Chamoumi, and Nicolas Abatzoglou. 2018. "Bio-Oil Steam Reforming over a Mining Residue Functionalized with Ni as Catalyst: Ni-UGSO" Catalysts 8, no. 1: 1. https://doi.org/10.3390/catal8010001