Laboratory Scale Plants

Laboratory scale plants (LSP) are low capacity but high flexibility facilities. LSP are used at the first stage of a researching when not a high productiviy capacity is need but a great amount of experimental essays are required. On LSP, any modifications could be done quickly and with a relative low cost, what allow to reach easily the best process configuration and conditions.

Laboratory scale plant for batch hemicellulose extraction

This experimental device is used for the analysis and study of hemicellulose extraction reactions. It is composed by an AISI 304 stainless steel vessel (170 mL), also disposed of an electric heater (275 W) placed around the wall and a magnetic stirrer. Reaction temperature is controlled by a PID controller (ICP, TC21) and a pressure gauge is used to measure the autogenous pressure inside the reactor. Maxima reaction pressure and temperature are 50 bar and 200 ºC. Outline disposes of a cooling system to reduce sample temperature and avoid degradation after the reaction.

Laboratory scale plant for hydrogenation reactions

This experimental apparatus consists into a stainless-steel high pressure reactor with an internal volume of 25 cm3 (Berghof BR-25) with a maxima operation pressure and temperature of 20 MPa and 300 ºC. Reactor disposed also of a magnetic stirrer and PID controlled. Reaction temperature is controlled by a thermostatic oil bath. Nitrogen supply is available to ensure inert atmosphere inside the reactor as safety stage before and after hydrogen feeding. HPLC pump with a maximum flow rate of 10 ml/min is used for organic solution pumping. If it is necessary higher reactor could be used with a total volume of 170 ml. Nitrogen and hydrogen are feed using Bronkhorst mass flow controllers until reacting pressure is reached. Hydrogen – nitrogen mixture or pure hydrogen could be used for hydrogenation.

Laboratory scale plant for catalyst synthesis using supercritical carbón dioxide 

Used for the determination of catalyst activity at high pressure reaction conditions. The chamber, HP HD300 from Eurotechnica GmbH, is built on SS316-Ti and it has an internal volume of 25 ml, supporting 30 MPa and 150 °C as maximum operating conditions. A magnetic driven agitator (12 VDC with transformer 230 VAC) is installed at the top of the reaction chamber in order to ensure a homogeneous medium. The temperature of the vessel is controlled by means of an electrical jacket (230 VAC; 50/60 Hz) connected to a digital display and NiCrNi thermocouple with a ±0.1 °C accuracy. Pressure inside the chamber is measured by a pressure gauge between 0.1 and 40 MPa.  The CO2 is pumped with a dosing pump Milton Roy Dosapro, MILROYAL D (up to 0.6 L/h and 24 MPa).

Laboratory scale plant for aerogel microparticles production by SAS technology with scCO2

The apparatus is used to produce aerogel microparticles by batch supercritical drying. It was designed and supplied by Eurotechnica (Hamburg, Germany).

Both vessels and the gear recirculation pump are placed inside a hot air oven in order to achieve the desired temperature and to keep it constant during all the process. Maxima operation pressure and temperature are 150 bar and 60 ÂşC.

Two buffer vessels with a capacity of 100 mL, an extraction vessel of 85 mL with a magnetic stirrer, and two pumps: an air-driven pump used for loading CO2 into the system, and a gear pump (Micropump 180 Series mod. GAH-T23) used to recirculate CO2 through the system in order to improve the contact between the supercritical fluid and the organic solvent.

Laboratory scale plant for carbon dioxide hydrogenation

Surface plasmon resonance can enhance the light absorbed by copper catalysts to improve the efficiency of the carbon dioxide photocatalytic transformation.

In this plant, carbon dioxide hydrogenation can be performed using light energy to produce methanol, which is considered as a potential fuel and a way to store the light energy. Glass microreactors with 0.5 mm ID are used to perform the reaction, and LEDs will provide the light energy.

The pilot plant allows a precise control of the temperature, pressure and gas mass flows to study their influence in the process, and the outlet gases can be analyzed directly in-line with a micro gas chromatograph. Hydrogen and carbon dioxide are mixed in a 3:1 proportion and heated in an oven together with the glass microreactor. Visual light is supplied by 36 LEDs which provide a nominal power of 9780 W/m2.

The system can control carbon dioxide and hydrogen flows up to 1 ml/min. The system allows to work at temperatures up to 200 ÂşC and pressures up to 70 bar.

 Laboratory scale plant for supercritical drying and functionalization of alcogels with supercritical CO2

The equipment was design and built for supercritical drying of alcogels. The main components of the setup used for the supercritical drying of aerogels are: a 1L CO2 buffer, a 25mL extractor (view chamber) and a recirculation gear pump whose frequency of rotation could be modified thus varying the CO2 flowrate through the view cell. The entire equipment is placed inside a hot air circulating oven that kept the temperature constant during the drying.

After the aging period, the alcogels are placed on a metallic tray in the extractor. Straightaway, the rest of the container is filled up with solvent in order to avoid the formation of cracks in the alcogel while the supercritical conditions are reached. Then, the complete equipment is heated and CO2 is pumped into the circuit. Once the operation conditions are reached (10.5 MPa, 45°C), the recirculation pump is activated and the extraction of the solvent begings.

Laboratory scale plant for batch hydrothermal hydrolisis

This stainless-steel reactor vessel with a total volume of 300 mL (Parker Autoclave Engineers) is able to operate up to 227 bar at 454°C. In its inside, it is equipped with a DispersimaxTM turbine stirrer (whose speed is controlled by MagneDrive® II,) a baffle bar and a cooling coil. The reactor is coupled with a ceramic band heater and a pressure gauge. Inside temperature, furnace temperature and stirring speed are controlled by a IB50 apparatus, which also shows the pressure’s value.

Actually, it is being used for biomass’ hydrolysis. It can be operated in a continuous way, but its current use is semi-continuous: the reactor is heated till the desired temperature, and then the liquid current is inserted. After the time is over, the refrigeration is performed both, inside with the cooling coil, and outside with a cold bath.

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