GPT - Thermo-Chemical Processes Group Instituto Universitario de Investigación en Ingeniería de Aragón. Universidad de Zaragoza
Facilities
Microscale catalytic fixed bed test rig
The microscale catalytic fixed bed test rig, operated at atmospheric pressure, was designed and constructed by Process Integral Development Eng.&Tech. (Microactivity Reference v3.0.) for the GPT in 2005. This setup enables to do catalytic tests at a microscale, hence needing very small amounts of catalyst and thus facilitating the screening of catalysts at varying operating conditions. The catalytic reactor consists of a fixed bed tubular quartz reactor, but the rig could be adapted to other types of reactors with minor modifications, being just limited by the dimensions of the electric furnace.
 
The unit has a liquid feeding system consisting of a HPLC metering pump which allows the feeding of various liquid feedstocks including biomass pyrolysis liquids (bio-oils), crude glycerol solutions, cheese whey, etc. The liquid fed in flows through 316 stainless steel tubing of 1/16 in. o.d. that can be preheated inside a heating system that can reach up to 180 ºC, thus allowing (if needed) a preliminary evaporation of the feed. The setup also has 3 mass flow controllers for gases, 2 of them for N2 (MFC01 and MFC02) and one for H2 (MFC03). Nitrogen is used as a carrier entraining the liquid in the form of sprayed small droplets, as a sweeping gas after reaction, and as an internal standard for the quantitative analysis of the product gases. Hydrogen is used for preliminary in-situ activation of the catalysts. Nevertheless, the gas lines could be easily adapted to other gases if necessary.
 
The liquid fed in is entrained together with N2 coming from MFC01, flowing through 316 stainless steel tubing of 1/8 in. o.d. and fed directly into the upper part of the reactor, placed inside an electric furnace that is also sheltered inside the cabin that hosts the pre-heating system. The temperature is controlled by two K-type thermocouples, one placed inside the reactor directly measuring the temperature of the bed, and the other measuring the temperature inside the cabin.
 
The setup has a condensing system to collect liquid products downstream the reactor and the gas fraction is quantitatively analysed on line by means of a micro gas cromatograph which analyses product gas samples online every 2-3 min.
 

Tech. Spec.

Liquid inlet: Gilson 307 HPLC metering pump equipped with a 5SC head, flow rate capacity: 0.010 – 5.000 mL/min.
- Gas inlet: 3 Bronkhorst HI-TEC EL-FLOW® Metal Sealed F-201C mass flow controllers: maximum capacity of 500 N mL/min (MFC01, for N2), 300 N mL/min (MFC02, for N2) and 100 N mL/min (MFC03, for H2).
- Watlow electric furnace, with a maximum temperature limit of 900 ºC, controlled by means of a TOHO TT-005 PID controller and a K-type thermocouple directly in contact with the catalytic bed inside the reactor. Dimensions: Heated zone: 25 cm high, 5 cm inner diameter. Insulated by means of quartz wool.
- Pre-heating system with a maximum temperature limit of 180 ºC, controlled by means of a TOHO TT-005 PID controller and a K-type thermocouple.
- Fixed bed, tubular quartz reactor. Dimensions: 12 mm o.d., 9 mm i.d. and 32.5 cm long. The bed is fixed at ca. 12.5 cm from the bottom by means of a quarz wool plug.
- Rig constructing materials: AISI 316 stainless steel
- Maximum allowable reactor volume: 0.5 L approx.
- Maximum allowed pressure: 0.5 bar-g
- Control loop
- Gas analysis: Agilent G2801A Micro GC equipped with 2 analysis modules using TCD detectors. Modules: Plot U (with Plot Q pre-column), He carrier, and MolSieve 5A, Ar carrier. Possibility of analysing H2S and up to C3 hydrocarbons.
- Computerized data acquisition system
 

Research projects

  • Producción de hidrógeno mediante reformado de líquidos de pirólisis de biomasa (CTQ2004-06279) – (Hydrogen production by steam reforming of biomass pyrolysis liquids).
    • Funded by the Spanish Ministerio de Educación y Ciencia (Spanish Research Council).
    • Period: 2005-2008.
    • Research leader: Dr. Jesús Arauzo.
    • Total budget: 209,600.00 €
  • Producción de gas de síntesis a partir de bio-oil generado de residuos agroforestales (CTPP02/09)
  • Funded by the Comunidad de Trabajo de los Pirineos.
  • Period: 2009-2011.
  • Research leader: Dr. Lucía García.
  • Total budget: 150,000.00 €
  • Participants: Universidad Zaragoza (Spain), Ikerlan (Spain), CIRAD (France)
 
 

Publications

Bimbela, F., Oliva, M., Ruiz, J., García, L., Arauzo. J.: “Hydrogen production by catalytic steam reforming of acetic acid, a model compound of biomass pyrolysis liquids.”, Journal of Analytical and Applied Pyrolysis 79 (2007) 112-120.
 
Bimbela, F., Oliva, M., Ruiz, J., García, L., Arauzo. J.: “Catalytic steam reforming of model compounds of biomass pyrolysis liquids in fixed bed: acetol and n-butanol.”, Journal of Analytical and Applied Pyrolysis 85 (2009) 204-213.
 
Bimbela, F., Oliva, M., Ruiz, J., García, L., Arauzo. J.: “Steam Reforming of Bio-Oil Aqueous Fractions for Syngas Production and Energy.” Environmental and Engineering Science 28 (2011) 757-763.
 
Bimbela, F., Chen, D., Ruiz, J., García, L., Arauzo. J.: “Ni/Al coprecipitated catalysts modified with magnesium and copper for the catalytic steam reforming of model compounds from biomass pyrolysis liquids.” Applied Catalysis B: Environmental, under revision.
 
Bimbela, F., Ruiz, J., García, L., Arauzo. J.: “Ni/Al coprecipitated catalysts for the catalytic steam reforming of the aqueous fraction of bio-oil.” In preparation.
 
European Comission Brisk
The Thermochemical Processes Group (GPT) is partly funded by the EU's European Social Fund and by the Gobierno de Aragón (Aragonese government)
EU's European Social Fund Gobierno de Aragón