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catalyseurs au nickel
Mathilde Luneau
COMPOSANTES SANTE
Faculté de Médecine Lyon Est – Claude Bernard Directeur : M. le Professeur J. ETIENNE
Faculté de Médecine et de Maïeutique Lyon Sud – Charles Directeur : Mme la Professeure C. BURILLON
Mérieux
Directeur : M. le Professeur D. BOURGEOIS
Faculté d’Odontologie
Directeur : Mme la Professeure C. VINCIGUERRA
Institut des Sciences Pharmaceutiques et Biologiques
Directeur : M. le Professeur Y. MATILLON
Institut des Sciences et Techniques de la Réadaptation
Directeur : Mme la Professeure A-M. SCHOTT
Département de formation et Centre de Recherche en Biologie
Humaine
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Catalysis
Science &
Technology
View Article Online
PAPER View Journal
Received 13th May 2015, The long-term stability of Ni-based catalysts for autothermal reforming of model biogas has been assessed
Accepted 21st June 2015
in a six parallel-flow reactor set-up implemented to test simultaneously six different catalysts at 700 °C
under a feed consisting of 42% H2O, 14% CH4, 9% CO2, and 7% O2 in argon. The reproducibility of catalyst
DOI: 10.1039/c5cy00702j
performance measured in the 6 parallel reactors was ascertained using a commercial Ni-based catalyst. A
www.rsc.org/catalysis screening of 12 catalyst formulations identified 5–0.05 wt% Ni–Rh/MgAl2O4 as a robust catalyst for
autothermal reforming of model biogas over 200 h time-on-stream.
This journal is © The Royal Society of Chemistry 2015 Catal. Sci. Technol.
View Article Online
the catalyst supports and metal–support interaction may play contain large excess of carbonates, ensuring precipitation of
a significant role in the catalytic activity. Alumina is widely all the metallic cations. The precipitate was aged for 3 h at
used as a support. However, the nickel spinel phase IJNiAl2O4) room temperature. After centrifugation and washing with de-
can be formed at high temperature during the reforming ionized water, the powder was dried overnight at 120 °C. The
reaction. NiAl2O4 is inactive and its formation leads to a dry deposit was then calcined at 800 °C for 5 h in air.
faster deactivation.9,10 Therefore, supports have been The same procedure was applied to synthesize ZnAl2O4
designed in order to prevent coking and oxidation. Incorpora- spinel, using nitrates of Al and Zn (Sigma-Aldrich) with an
tion of basic alkali-earth metals such as Mg and Ca into Al : Zn molar ratio of 2 : 1.
Published on 22 June 2015. Downloaded by Université Claude Bernard Lyon on 07/07/2015 16:04:13.
Al2O3-based catalysts has been carried out in order to LaAlO3 was prepared by a modified sol–gel method
improve both stability and activity.11–13 Other supports (Pechini). Ethylenediaminetetraacetic acid (EDTA, Sigma-
exhibiting oxygen mobility properties were studied in order Aldrich) was added to an aqueous solution containing the
to promote the gasification of deposited carbon.14–16 metal nitrates (concentration of 0.5 mol L−1, Sigma-Aldrich)
Biogas composition varies depending on the origin of the with a La : Al molar ratio of 1 : 1. EDTA is used as a chelating
biomass. Although mainly composed of methane and carbon agent. A few milliliters of ammonia solution were added to
dioxide, biogas also typically contains sulphur compounds.17 obtain a clear solution. Finally, a solution of citric acid (2.5
The presence of H2S is a major problem due to its irreversible mol L−1, n(citric acid) = nIJAl) + nIJLa)) was added to the solu-
poisoning effect on metals.18 Biogas can also contain volatile tion containing the chelated metals. The temperature of the
organic compounds such as chlorinated compounds. Methyl solution was slowly heated to 100 °C. Stirring was continued
chloride was shown to impact on the H2/CO ratio by increas- until evaporation of water lead to a transparent gel. The gel
ing the surface acidity of the alumina support.19 Model bio- was then dried and calcined following four different steps
gas composed of clean methane and carbon dioxide (60 : 40 (120 °C – 3 h; 300 °C – 3 h; 400 °C – 3 h; and 800 °C – 5 h).
vol : vol) was used in our study. The same procedure was applied to prepare LaNiO3 with
Many catalysts have been tested for methane or biogas nitrates of lanthanum and nickel with a La : Ni molar ratio of
reforming with different combinations of active metals on 1 : 1.
various supports.20 However, these tests were performed CeO2–Al2O3 was prepared by co-precipitation. An aqueous
under different conditions of temperature and pressure with solution containing Ce and Al nitrates (Fluka) with a Ce : Al
different feed ratios, flow rates and reactor designs, making a molar ratio of 1 : 2 (concentrations of 0.17 and 0.34 mol L−1)
fair comparison difficult. was gradually added to an aqueous solution of ammonium
High-throughput catalyst testing has become a widely carbonate under fast stirring. The carbonate solution was
accepted tool in catalyst development. However, it is mainly prepared in order to contain large excess of carbonates,
used in the screening and discovery of new catalyst formula- assuring precipitation of all metallic cations. The precipitate
tions,21,22 less commonly to characterize specific catalyst was aged for 3 h. After centrifugation and several washing
properties23 or long-term performance. On the other hand, cycles with de-ionized water, the precipitated powder was
this technology is hardly reported for the study of long-term dried overnight at 120 °C, then calcined at 800 °C for 5 h.
catalyst stability. This is rather surprising as an obvious gain The same method was used to prepare ZrO2–Al2O3 with
in time can be obtained for these kinds of tests, compared to nitrates of zirconium and aluminium (Aldrich and Fluka)
testing each sample separately. with a Zr : Al molar ratio of 1 : 2.
In the present study, long-term catalyst stability was Ni was deposited on the different supports (spinels, perov-
assessed using a six parallel-flow reactor set-up, specially skites, mixed oxides) by deposition–precipitation using nickel
implemented to test simultaneously six catalysts under essen- nitrate NiIJNO3)2·6H2O (Fluka) and urea (Sigma-Aldrich). Stir-
tially identical flow rate, temperature and feed composition. ring was continued for 4 h while the temperature was
Four types of supports were investigated: spinels, mixed increased to 100 °C in order to remove excess urea. After cen-
oxides, perovskites and hydrotalcite-type precursors. The sup- trifugation and several washing with de-ionized water, the
ports were impregnated with nickel and tested under similar samples were dried at 120 °C overnight and calcined at 550
conditions. °C for 4 h in air.
5 wt% Ni–0.05 wt% Rh/MgAl2O4 and 5 wt% Ni–0.05 wt%
Experimental Rh/LaAlO3 were also prepared by wet impregnation of
MgAl2O4 or LaAlO3 with a solution containing nickel nitrate
Catalyst preparation IJNiIJNO3)2·6H2O, Fluka) and rhodium nitrate IJRhIJNO3)3·2H2O,
Magnesium spinel IJMgAl2O4) was prepared by co-precipita- Alfa Aesar). Stirring was continued for 6 h. After evaporation
tion. An aqueous solution containing Mg and Al nitrates of water, the slurry was dried at 120 °C overnight and cal-
(Sigma-Aldrich and Fluka) with an Al : Mg molar ratio of 2 : 1 cined at 550 °C for 4 h in air.
(concentrations of 0.66 and 0.33 mol L−1, respectively) was Hydrotalcite-type precursors were prepared by co-precipita-
added drop by drop into an aqueous solution of ammonium tion. An aqueous solution containing nitrates of Ni, Mg and
carbonate (Sigma-Aldrich) under vigorous stirring. The Al (Fluka and Sigma-Aldrich) was added dropwise to a satu-
ammonium carbonate solution was prepared in order to rated solution containing NaHCO3 and NaOH. The
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precipitate was aged for 1 h. After centrifugation and washing at 700 °C. After mixing the reactants, the main gas stream
with de-ionized water, the deposit was dried overnight at 120 was split into six flows, each being directed into a reactor.
°C. The dry deposit was then calcined at 800 °C for 5 h in air. Special attention was given to distribute the flows equally,
A commercial Ni-based catalyst (HiFUEL R110, Alfa Aesar, since the six different catalyst beds each create different pres-
ref. 45465) was used as reference catalyst. sure drops and can cause unequal flow distribution. To solve
this issue, six identical stainless steel capillaries with small
Catalyst characterization internal diameters IJ1/16" OD, 0.01" ID, 200 mm length) were
placed upstream to the reactors. The pressure drop created
Powder X-ray diffraction patterns (XRD) were recorded using
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converted to molar flows knowing the molar flow rate of Ar perovskite catalyst (LN) was intended to behave similarly
and the sensitivity coefficient of each m/z fragment relative to (synthesis of a mixed oxide and surface reduction leading to
Ar, which is constant. Accurate water quantification with a well-dispersed metallic Ni particles on LaNi1−xO3), but its very
MS is difficult, but the liquid water flow rate was precisely low SSA might forbid a good dispersion of Ni.
controlled by a calibrated HPLC pump, therefore the molar Since Ni2+ tends to react with alumina at high temperature
flow rate of steam at the reactor inlet was known accurately. to form the inactive spinel NiAl2O4 (and any possible sub-
stoichiometric Ni1−xAl2O4−x composition), MgAl2O4 and
Results and discussion ZnAl2O4 spinels were used as supports because they combine
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Fig. 3 Dry outlet gas concentrations during autothermal reforming of Fig. 5 Methane conversion (%) during autothermal reforming of
model biogas (60%–40%; CH4–CO2) at T = 700 °C with S/C = 3, O/C = model biogas (60%–40%; CH4–CO2) at T = 700 °C with S/C = 3, O/C =
0.5. 0.5.
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