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Reformage autotherme de biogaz modèle sur des

catalyseurs au nickel
Mathilde Luneau

To cite this version:


Mathilde Luneau. Reformage autotherme de biogaz modèle sur des catalyseurs au nickel. Catalyse.
Université de Lyon, 2016. Français. �NNT : 2016LYSE1129�. �tel-01570864�

HAL Id: tel-01570864


https://theses.hal.science/tel-01570864
Submitted on 1 Aug 2017

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N°d’ordre NNT :

THESE de DOCTORAT DE L’UNIVERSITE DE LYON


opérée au sein de
l’Université Claude Bernard Lyon 1

Ecole Doctorale N° 206


Ecole Doctorale de Chimie de Lyon

Soutenue publiquement le 22/07/2016, par :


Mathilde Luneau

Reformage autotherme de biogaz


modèle sur des catalyseurs au nickel

Devant le jury composé de :

Anne Giroir-Fendler Professeur Université Lyon 1

Florence Epron Directrice de Recherche CNRS, Poitiers rapporteur


Anne-Cécile Roger Professeur Université Strasbourg rapporteur

Patrick Da Costa Professeur UPMC


Daniel Gary Ingénieur de Recherche Air Liquide

Nolven Guilhaume Chargée de Recherche IRCELyon Directrice de thèse


Frédéric Meunier Chargé de Recherche IRCELyon Co-directeur de thèse
Yves Schuurman Directeur de Recherche IRCELyon
UNIVERSITE CLAUDE BERNARD - LYON 1
Président de l’Université M. le Professeur Frédéric FLEURY

Président du Conseil Académique M. le Professeur Hamda BEN HADID

Vice-président du Conseil d’Administration M. le Professeur Didier REVEL


Vice-président du Conseil Formation et Vie Universitaire M. le Professeur Philippe CHEVALIER
Vice-président de la Commission Recherche M. Fabrice VALLÉE
Directeur Général des Services M. Alain HELLEU

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

COMPOSANTES ET DEPARTEMENTS DE SCIENCES ET TECHNOLOGIE

Faculté des Sciences et Technologies Directeur : M. F. DE MARCHI


Département Biologie Directeur : M. le Professeur F. THEVENARD
Département Chimie Biochimie Directeur : Mme C. FELIX
Département GEP Directeur : M. Hassan HAMMOURI
Département Informatique Directeur : M. le Professeur S. AKKOUCHE
Département Mathématiques Directeur : M. le Professeur G. TOMANOV
Département Mécanique Directeur : M. le Professeur H. BEN HADID
Département Physique Directeur : M. le Professeur J-C PLENET
UFR Sciences et Techniques des Activités Physiques et Sportives Directeur : M. Y.VANPOULLE
Observatoire des Sciences de l’Univers de Lyon Directeur : M. B. GUIDERDONI
Polytech Lyon Directeur : M. le Professeur E.PERRIN
Ecole Supérieure de Chimie Physique Electronique Directeur : M. G. PIGNAULT
Institut Universitaire de Technologie de Lyon 1 Directeur : M. le Professeur C. VITON
Ecole Supérieure du Professorat et de l’Education Directeur : M. le Professeur A. MOUGNIOTTE
Institut de Science Financière et d'Assurances Directeur : M. N. LEBOISNE
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Catalysis
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High-throughput assessment of catalyst stability


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during autothermal reforming of model biogas


Cite this: DOI: 10.1039/c5cy00702j
M. Luneau, Y. Schuurman, F. C. Meunier, C. Mirodatos and N. Guilhaume*

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.

Introduction Partial oxidation is a slightly exothermic reaction, actually


the result of two consecutive reactions: first the highly exo-
Biogas is a complex gas mixture produced from the anaerobic thermic combustion of methane at the beginning of the cata-
digestion of biomass, which contains methane and carbon lyst bed, followed by steam and CO2 reforming of the
dioxide as main components.1 Biogas can be combusted remaining methane and the WGS reaction.
directly, although exhibiting a lower heating value than natu- Catalytic partial oxidation (CPO):
ral gas. Biogas can also be reformed into hydrogen, which is
a base feedstock for the chemical industry and can also be CH4 + 1/2 O2 ↔ CO + 2H2 ΔH = − 36 kJ mol−1 (4)
used as a fuel in fuel-cells to produce electricity.2
Since biogas essentially contains methane and carbon Autothermal reforming (ATR) is seen as a practical option
dioxide, the dry reforming (DR) of methane (eqn (1)) is an to minimize energy supply to the reactor. ATR consists of
obvious pathway to produce syngas: adding oxygen (or air), which results in combustion of a por-
tion of methane into carbon dioxide and water followed by
CH4 + CO2 ↔ 2CO + 2H2 ΔH = + 247 kJ mol−1 (1) reforming and WGS reactions.
The general equation for ATR is:
Yet, this reaction is strongly endothermic and must be
conducted at high temperatures (800–900 °C), whereas the CH4 + 1/2 xO2 + yCO2 + (1 − x − y)H2O ↔ (y + 1)CO
CH4/CO2 ratio in biogas (generally closer to 1.5 than to 1) is not + (3 − x − y)H2 (5)
suitable for complete methane conversion. Methane can also be
converted into syngas by steam reforming (SR, eqn (2)): in which the O2/CH4 ratio has to be adjusted to reach the
thermal balance between exothermic and endothermic reac-
CH4 + H2O ↔ CO + 3H2 ΔH = + 206.2 kJ mol−1 (2) tions. According to thermodynamic calculations (HSC chem-
istry software), formation of CO and H2 by steam and dry
SR is also an endothermic reaction but yields more hydro- reforming is favored at temperatures above ca. 630 °C.
gen than DR. SR limits carbon deposition and steam is gener- Catalytic reforming of methane has been widely studied
ally introduced in excess in order to shift the water-gas shift and carried out using different catalysts. Few studies have
equilibrium (eqn (3)) towards more H2 and less CO produc- focused on biogas. The most commonly used catalysts are
tion at the reactor outlet. nickel- and noble metal-based catalysts (Ru, Rh, Pd, Ir, and
Water-gas shift (WGS): Pt).3,4 Nickel-based catalysts are often used because those
combine low cost and acceptable catalytic activity. The main
CO + H2O ↔ CO2 + H2 ΔH = − 41.2 kJ mol−1 (3) issues with nickel are the deactivation caused by deposition
of carbon and/or sintering of metal particles.5,6 Noble metals,
notably Pt and Ir, are more active than Ni.7 Noble metals
Université Lyon 1, Institut de Recherches sur la Catalyse et l'Environnement de
Lyon IRCELYON, UMR5256 CNRS, 2 avenue Albert Einstein, F-69626,
present better performance since they are less prone to oxida-
Villeurbanne Cedex, France. E-mail: Nolven.Guilhaume@ircelyon.univ-lyon1.fr; tion, coking and sintering,8 but are more expensive and
Tel: +33 472 445 389 hence not the preferred option. Furthermore, the nature of

This journal is © The Royal Society of Chemistry 2015 Catal. Sci. Technol.
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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

Catal. Sci. Technol. This journal is © The Royal Society of Chemistry 2015
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Catalysis Science & Technology Paper

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
Published on 22 June 2015. Downloaded by Université Claude Bernard Lyon on 07/07/2015 16:04:13.

by the capillaries was much more important than that cre-


a Bruker D5005 diffractometer with CuKα radiation at λ =
ated by the catalyst bed. Measurement of the individual flows
1.5418 Å.
through the reactor showed deviations of ±4 mL min−1 for a
Elementary analysis of the fresh catalysts was performed
flow of 80 mL min−1 per reactor. A 6-port automatic selection
by ICP-AES using a Jobin Yvon Activa Spectrometer D ICP-
valve placed at the reactor exit allowed selection of the efflu-
OES to determine the Ni loading.
ent of one specific reactor to be sent to a mass spectrometer
Specific surface areas (SSA) were measured by nitrogen
for gaseous product analysis. The selection valve was auto-
adsorption on catalysts at −196 °C on a BELSORP-Mini (Bel-
matically switched every five minutes in order to measure
Japan).
sequentially the performance of each reactor using an online
Thermal analyses (DTA-TGA) were performed in air with a
mass spectrometer. Pressure transducers placed upstream
SETARAM analyser equipped with a mass spectrometer for
and downstream the reactors also measured the pressure
online gas analysis. The samples were placed in a Pt crucible
drop in each reactor being analysed, to check for a possible
and heated at 10 °C min−1 under a flow of synthetic air (50
increase in the pressure due to extensive coke deposition.
mL min−1).

Catalytic activity and stability measurements Catalytic tests


A proprietary automated six-parallel reactor technology was Tests were performed at 700 °C and at a pressure of 1.6 bar.
implemented (Fig. 1) to perform high-throughput long-term Prior to testing, the catalyst samples were pelletized, crushed
testing of the catalysts. The liquid water flow rate was con- and sieved to obtain a particle size fraction between 100 and
trolled by a HPLC pump (Shimadzu LC 20-AD) and vaporized 200 microns. Catalyst beds were composed of 20 mg of cata-
in a custom-made evaporator at 200 °C, before mixing with lyst and diluted with quartz powder (100–200 microns), to
the gaseous reactants whose flow rate was controlled by obtain a similar bed length of 8 mm whatever the catalyst
mass-flow controllers. All gas lines and valves were heated at density. The catalysts were reduced in situ with a H2–argon
160 °C to prevent steam condensation. Six tubular quartz mixture (4 : 1, vol : vol) for 3 hours at 700 °C. The reaction
reactors (length 180 mm, 4 mm ID) were placed in a tubular mixture consisted of 42% steam, 14% CH4, 9% CO2, 7% O2
furnace with six positions. The temperature in each reactor in an argon balance. This composition represents a model
was measured under inert gas flow and at 700 °C, differences biogas containing 60% CH4 and 40% CO2, which is reacted
of ±8 °C between the 6 reactors were found. Taking an activa- with a mixture of O2 and H2O under the conditions O2/CH4 =
tion energy of 110 kJ mol−1 for the steam reforming of meth- 0.5 and H2O/CH4 = 3. If oxygen were supplied as air, the bal-
ane,24 this will lead to a ±10% variation in the reaction rate ance gas would be nitrogen. Argon was substituted for nitro-
gen because N2 would forbid analyzing CO by mass spectrom-
etry (same molecular ion), and Ar was also used as internal
standard for quantification of products. The total flow rate of
the reactant gases was 380 mL min−1 resulting in a gas hourly
space velocity (GHSV) in each reactor of 38 000 m3 m−3 h−1
and a weight hourly space velocity (WHSV) of 190 L (h gcat)−1.
Online analysis of the reactors' exit streams was performed
with a mass spectrometer (MS) monitoring m/z fragments 2
(H2), 4 (He), 15 (CH4, this fragment was chosen rather than
the molecular ion because it is nearly as intense (90%) as
mass 16 in the methane fragmentation spectrum, whereas O2
significantly contributes to mass 16, and also CO, CO2 and
H2O to a lesser extent), 18 (H2O), 28 (CO, corrected for the
contribution of CO2 to this fragment), 32 (O2), 40 (Ar), and 44
(CO2). Quantitative analysis was performed by calibrating the
MS response using different partial pressures of all relevant
compounds diluted in argon. The Ar signal was used as an
Fig. 1 Set-up for the reactors' inlet and outlet. internal standard and the other ion current intensities were

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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
Published on 22 June 2015. Downloaded by Université Claude Bernard Lyon on 07/07/2015 16:04:13.

a high surface area, a basic character in the case of MgAl2O4,


Catalyst characterization whereas Mg2+ and Zn2+ ions occupy the crystallographic posi-
The nickel loading and surface areas of the tested catalysts tions where Ni2+ ions migrate in the alumina structure.
are reported in Table 1. A similar amount of Ni, around 5 Therefore, these supports should prevent, or at least limit,
wt%, was generally deposited on the catalysts, with the excep- the migration of nickel in the support.
tion of sample NRL, which exhibited a lower loading (3.9
wt%), and sample LN (LaNiO3 perovskite) for which the bulk
nickel concentration was 26 wt%. Four catalysts (NC, NS, NA, Six-parallel reactor set-up validation with a commercial
CC) with higher Ni loadings (10–20%) and two catalysts catalyst
doped with a small amount of Rh (NRL and NRM) were also In order to obtain reliable information about the catalyst per-
included in the screening. The catalysts exhibited substantial formance and to assess the repeatability of the results, the
variations in specific surface areas. It was generally high for set-up was validated by testing the same mass of commercial
spinel and hydrotalcite-type catalysts, with NM presenting Ni-based catalyst in the 6 reactors (Fig. 2).
the highest value (158 m2 g−1). The perovskites had lower sur- Methane was fully converted at t = 0 in all the reactors,
face areas, ranging from 2.7 to 15 m2 g−1. The specific surface but declined steadily. The production of hydrogen and of car-
areas of mixed oxides catalysts were 57 and 119 m2 g−1 for bon monoxide was similar in each reactor at full conversion
NCA and NZA, respectively. and decreased with decreasing methane conversion. At t = 0,
The selection of catalysts and support for the screening the production of H2 was of about 1 μmol min−1 and that of
was based on general trends found in the literature related to CO about 0.3 μmol min−1. The H2/CO ratio remained around
steam and dry reforming of methane over Ni-based catalysts: four until the sharp drop in the methane conversion. The
basic supports are preferred over acidic supports, which are deactivation profiles were similar: a slow deactivation was
prone to coking due to cracking reactions taking place on the observed followed by an abrupt loss of the activity although
acid sites. The basic character enhances steam activation as scattered over a range of about 5 h. As the methane
hydroxyl groups, which react with the coke and improve its
gasification. Ceria combines the basic character with oxygen
mobility properties and has also been shown to improve the
gasification of coke in dry reforming reactions.
The Mg–Al–Ni hydrotalcite-type catalyst (HT) has also a
basic character and a high surface area. Ni ions are initially
incorporated in a mixed hydroxy-carbonate structure, then
extracted upon reduction as metallic Ni, which should lead
to the formation of well-dispersed Ni particles. The LaNiO3

Table 1 Ni loading and specific surface area of prepared catalysts

Ni loading BET surface area


Catalysts Code (%) (m2 g−1)
5 wt% Ni/MgAl2O4 NM 5.1 158
5–0.05 wt% NiRh/MgAl2O4 NRM 5.1 118
5 wt% Ni/ZnAl2O4 NZ 4.5 99
5 wt% Ni/LaAlO3 NL 4.5 15
5–0.05 wt% NiRh/LaAlO3 NRL 3.9 7.8
LaNiO3 LN 26 2.7
5 wt% Ni/CeO2–Al2O3 NCA 5 57
5 wt% Ni/ZrO2–Al2O3 NZA 5 119
Hydrotalcite-type precursor HT 4.3 116
NiO/CaAl12O19 NC 14 10
20 wt% Ni/SiO2 NS 20 40 Fig. 2 Autothermal reforming of model biogas (60%–40%; CH4–CO2)
20 wt% Ni/Al2O3 NA 20 123
at T = 700 °C with S/C = 3, O/C = 0.5. a) Methane conversion (%), b)
Commercial catalyst CC 10 16
H2 and CO production, and c) H2/CO ratio over time.

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conversion fell to zero, the hydrogen and monoxide produc-


tions were simultaneously suppressed.
Fig. 3 shows the composition (on a dry basis, i.e. not tak-
ing the steam into account) of reactor 6 exit stream. With an
S/C ratio of 3, the steam is in large excess and is only partly
consumed during the reaction. H2 and CO molar fractions
reach about 40% and 10%, respectively, at full methane con-
version. Complete conversion of methane and oxygen is
Published on 22 June 2015. Downloaded by Université Claude Bernard Lyon on 07/07/2015 16:04:13.

observed during the first hours. After 15 hours, the methane


molar fraction increases while the oxygen molar fraction
remains zero. When the methane molar fraction reaches 10%
(corresponding to 60% conversion), the oxygen conversion is
no longer complete. Methane and oxygen conversions sud- Fig. 4 Methane conversion (%) during autothermal reforming of
denly drop to zero and hydrogen and carbon monoxide pro- model biogas: a) (60%–40%; CH4–CO2) at T = 700 °C with S/C = 3 and
in the absence of oxygen and b) (60%–40%; CH4–CO2) at T = 700 °C
ductions drop similarly. The catalyst is fully deactivated. Sim- with S/C = 3 and addition of hydrogen.
ilar behavior was observed on all the reactors.
The catalyst stability in the six reactors varied around 40 ±
gaseous oxygen will rapidly oxidize the metallic Ni and deac-
5 hours. This corresponds rather well to the variation of the
tivate the catalyst. These catalysts will not be reactivated
methane steam reforming rate of ±10% which can be attrib-
when O2 is removed from the feed because Ni is fully oxi-
uted to slight differences in the reactor temperatures, catalyst
dized and unable to catalyse the steam reforming reaction. In
loadings and reactant flow rates. The six deactivation pro-
reactors 2 and 5 the catalyst was not completely deactivated
files, however, were sufficiently similar to allow unambiguous
and still produced small amounts of H2 + CO, which suggests
discrimination between fast-deactivating and stable catalysts.
that some metallic Ni was still present, and upon oxygen
The role of oxygen in the catalyst deactivation is evidenced
removal the hydrogen produced by methane steam reforming
by the experiments shown in Fig. 4. After 43 hours, oxygen
was able to reduce again the oxidized Ni. After ca. 47 hours,
was removed from the feed gas, and the catalyst in reactors 2
hydrogen was added to the feed. Methane conversions rang-
and 5 started to convert methane again. Before oxygen
ing from ca. 65 to 70% were observed in all the six reactors.
removal, the O2/CH4 ratio in the feed stream is 0.5, which
Oxidation of Ni appears to play an important part in the
means that 25% of the methane is immediately burnt into
deactivation process.
CO2 at the reactor inlet (the stoichiometry for methane com-
bustion is O2/CH4 = 2). Oxygen is totally converted and Ni is
likely to be oxidized in the CH4 combustion zone, but the Catalyst screening for ATR of model biogas
metallic Ni still present downstream in the reactor ensures The results of catalyst screening in terms of methane conver-
the reaction of the remaining methane with steam, and pos- sion are shown in Fig. 5.
sibly with CO2. As soon as the catalyst is sufficiently The catalyst performance at 700 °C versus time-on-stream
deactivated that some of the oxygen is unconverted (this depended strongly on catalyst composition.
should theoretically happen when the methane conversion Comparing the behaviour of the ≈5 wt% Ni catalysts
falls below ≈25%, but it might also happen before since NiO loaded on different supports, our screening shows that the
is not a very good catalyst for methane combustion),25 the support properties that were shown to be beneficial in meth-
ane steam reforming do not appear as relevant when

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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autothermal reforming of methane is involved: NM, NZ and


NCA exhibited full initial conversion but deactivated within 2
hours, while NZA deactivated almost instantly. HT was found
fully inactive, but the catalyst reduction temperature was
probably too low to reduce and extract Ni from the mixed-
oxide structure, since the Ni reduction in Ni–Mg–Al hydro-
talcite catalysts has been shown to take place between 750
and 900 °C.26 NL catalyst (5% Ni/LaAlO3) deactivated more
Published on 22 June 2015. Downloaded by Université Claude Bernard Lyon on 07/07/2015 16:04:13.

gradually and was fully deactivated after 16 h. Therefore


LaAlO3 appears as an interesting support, despite its low SSA.
Increasing the Ni loading was expected to delay the cata-
lyst deactivation, since more Ni is available in the reactor,
provided that it is dispersed enough and that the support Fig. 6 Hydrogen production (μmol min−1) during autothermal
exhibits the appropriate acid–base properties. This was gener- reforming of model biogas (60%–40%; CH4–CO2) at T = 700 °C with
ally verified since all 5 wt% Ni catalysts except NL deactivated S/C = 3, O/C = 0.5.

before CC (10% Ni) and NC (14% Ni) catalysts, which in turn


deactivated before NA (20% Ni). A noticeable exception was
NS (20% Ni/SiO2), which deactivated so rapidly that no meth- combustion of methane (to provide heat) with steam/dry
ane conversion was observed, evidencing that SiO2 is not a reforming of the remaining methane. Since methane com-
good support in this reaction. LN catalyst (26 wt% Ni) bustion is much faster than the reforming reactions and is
revealed peculiar performance, with a moderate but constant strongly exothermic (ΔH = −801 kJ mol−1), it takes place at
methane conversion (≈30%), which gradually dropped to the catalyst bed inlet and leads to the formation of hotspots
zero after 20 h (not shown), probably due to the negative and temperature gradients along the bed.30,35 As shown in
combination of high Ni loading and very low surface area. the case of methane partial oxidation,36 the combination of
Rh doping had a very strong influence on the stability of high temperature and the presence of oxygen in the feed
NM since NRM still fully converted methane after 200 h of stream is likely to oxidize the nickel particles, which no lon-
reaction. In contrast, NRL deactivated before NL, which ger participate in the reforming reactions. The high tempera-
might be attributed to the very low surface area of the cata- ture front will diffuse further down the bed, leaving less
lyst after its second impregnation with Rh. Ni–Rh bimetallic metallic Ni available for the reforming reactions. Once the
catalysts have been shown to exhibit enhanced stability for combustion zone reaches the end of the catalyst bed, the
methane tri-reforming27 and dry-reforming reactions,28 simi- methane conversion will drop to zero.
lar to Ni–Pd29–31 Ni–Pt32 and Ni–Co formulations.33,34 Post-reaction characterization of catalysts showed that
With the exception of LN, the deactivation profiles of all XRD patterns were not significantly modified compared to
the tested catalysts were rather similar to that of the commer- fresh catalysts. Fig. 7 presents the diffractograms of NM cata-
cial catalyst: the methane conversion decreased slowly for a lyst before and after the ATR reaction. Both diffractograms
certain time, then rapidly fell to zero. Hydrogen production exhibited the characteristic lines of the spinel phase
versus time is shown in Fig. 6. The order of deactivation time MgAl2O4, whereas no Ni or NiO lines were evidenced.
NS-HT-NZA < NZ < NCA < NM < NRL < NC < NL < NA < However, the small amount of catalyst in each reactor (20
NRM was observed. mg, mixed with quartz powder) provided only a low-
The hydrogen production profiles matched well the con- resolution diffractogram, which did not allow a thorough
version profiles of methane shown in Fig. 5. In agreement comparison of fresh and used catalyst diffraction patterns.
with the low methane conversion, the reaction on LN pro- TGA-DTA-TPO analysis of the commercial catalyst after reac-
duced much less hydrogen than the other catalysts. tion revealed two small mass losses with maxima at ca. 350
The abrupt changes in the slopes of the deactivation pro- °C (−0.12%, exothermic) and 690 °C (−0.11%, endothermic),
files exhibited by most catalysts suggested different deactiva- associated with CO2 production in sub-ppm amounts. The
tion mechanisms for each stage. For the slow initial deactiva- CO2 production at low temperature might be attributed to
tion: nickel and/or support sintering eventually combined the combustion of very reactive carbon, in direct contact with
with coke deposition may progressively deactivate the cata- Ni. The high temperature CO2 production is endothermic
lysts. Our reaction conditions imply working with an excess and thereby suggests the decomposition of carbonates
of steam IJH2O/CH4 = 3) that can promote the sintering of formed on the basic support. Limited carbon deposition is
oxides and metals, known to be a rather slow process. How- consistent under the reaction conditions in which the
ever, whatever be its origin, such a slow initial deactivation H2O/CH4 ratio of 3 and the high CO2 partial pressure should
cannot account for the subsequent sharp collapse in the cata- prevent extensive coking (carbon can be gasified by steam
lytic activity. The latter might be related to the presence of and by CO2 through the reverse Boudouard reaction37). TEM
oxygen in the feed stream, leading to nickel oxidation. As examination of the deactivated commercial catalyst samples
mentioned previously, the ATR of methane combines the also revealed the presence of a carbon film on some Ni

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for several hours. A six-parallel flow reactor is a powerful tool


to assess the long-term stability of six catalysts simulta-
neously in the ATR of biogas. A screening of catalysts was
performed in a short time demonstrating an order of deacti-
vation time NS-HT-NZA < NZ < NCA < NM < NRL < NC <
NL < NA < NRM. A slow initial deactivation process could be
related to some carbon deposition, but the main fast final
deactivation process is likely associated with nickel oxidation.
Published on 22 June 2015. Downloaded by Université Claude Bernard Lyon on 07/07/2015 16:04:13.

Rh promotes Ni stability and thus 5–0.05 wt% Ni–


Rh/MgAl2O4 was identified as a robust catalyst for
autothermal reforming of model biogas.

Fig. 7 X-ray diffractogram of NM catalyst a) after reduction at 700 °C Acknowledgements


and b) after deactivation.
The research leading to these results has received funding
from the European Community's Seventh Framework
Programme ([FP7/2007–2013] under grant agreement no.
325383 (BioRobur). The authors thank Bernadette Jouguet for
performing timely TGA-DTA analyses.

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