Tampere

Jukka Konttinen

Chao He

Susanna Maanoja

Contact persons

Operating Catlab

Research groups

Circular Economy Innovation

Energy and Biorefining

Bio and Circular Economy research groups

The fluidized bed reactor

Publications

Recent publications

CATLAB is a combined bench-top microreactor and mass spectrometer (MS) system for rapid and reproducible catalysis studies and thermal analysis.

The module 1 of this system is a bench-top microreactor used for fixed bed catalytic thermochemical reactions, which mainly contains microreactor with accurate temperature and various gas inlets controlling. The module 2 of this system is a mass spectrometer for fast response real-time gas analysis. The Hiden Analytical CATLAB could exactly provide its unique microreactor and mass spectrometer system with completely integrated control- and software for MS-acquisition, temperature and gas control and pulsing in single software package. It also features an integrated analysis software for catalysis and TPD measurements.

<h2>Technical details</h2>

<ul>
	<li>Reactor bypass channel for gas flow setup and mixture preparation independent of the protected sample environment.</li>
	<li>Linear, vertical quartz reactor tube with independent cartridge-style sample holder for fast sample changeover with positive relocation.</li>
	<li>Integrated dual-function pulsing valve with user-changeable sample loop volumes for single or multiple pulsing of the absorbate gas and for fast primary gas stream switchover.</li>
	<li>Fully pre-programmable and automated analysis cycles to control ramp rates, temperature range, temperature dwell periods, gas flows, pulse switching and mass spectrometer parameters.</li>
	<li>“In-bed” thermocouple mounted directly within the sample for the most accurate determination of sample temperature.</li>
	<li>Close coupled gas sampling line with the mass spectrometer gas takeoff just 1 cm downstream from the sample for synchronous measurement of desorbing gases with temperature.</li>
	<li>Choice of different reactor sizes (4mm, 7mm and 12 mm ID).</li>
	<li>2m heated (controllable up to 200°C) quartz lined capillary sampling line length. Mass spectrometer can be easily detached for use off-line. User exchangeable inlet liner for easy maintenance.</li>
	<li>Mass spectrometer range between 0-200 amu, and with dual detector (faraday cup and SEM)</li>
	<li>Mass spectrometer sampling rates up to 650 measurements per second.</li>
	<li>&lt; 500 ms response time to changes in gas concentrations.</li>
	<li>APSI-MS Soft ionisation mode to minimise fragmentation of complex molecules for spectral simplification and interpretation. Controllable down to &lt;10 eV and up to 80 eV at 0.2 eV increments, and in same scans.</li>
	<li>Source emission settable between 1 µA to 500 µA.</li>
</ul>

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2022-02/catlab-reactor-schematic.jpg?itok=TqfLe5-d" alt="Schematic presentation of the Catlab reactor" ><figcaption>Schematic presentation of the Catlab reactor. Image by CEI research group.</figcaption></figure>

CATLAB microreactor

The fluidized bed reactor&nbsp; is a complete reactor system consisting of a high-temperature furnace (max. 1000 ºC) and accurate mass flow controllers (incl. N2, CO2, and air). The reactor part and exhaust system will increase its capability to measure yields and compositions of tar and gas, which can be applied for comprehensive reaction studies in thermochemical conversion processes, i.e., pyrolysis, gasification, combustion, and chemical-looping gasification/combustion.

<h2>Technical details</h2>

<ul>
	<li>Withstand high-oxidizing environments (reactor material: stainless steel grade 253MA)</li>
	<li>Feeding can be manually batch or continuous system by using a conveyor belt system</li>
	<li>Gas cleaning system, including gas washing bottles, a packed bed of silica gel, and quartz cotton, is used to separate tar from product gas</li>
	<li>Flow rate of clean fuel gas is measured by a digital mass flow controller</li>
	<li>Gas composition is measured by an online micro-GC.</li>
</ul>

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2022-02/fbr-system.jpg?itok=mHdnkO-h" alt="Schematic presentation of the fluidized bed reactor" ><figcaption>Schematic presentation of the fluidized bed reactor. Image by CEI research group.</figcaption></figure>

Fluidized bed reactor

The Parr reactor is a high temperature and pressure system that can be used in many branches of chemical and energy technology. Catalytic hydrothermal processing and hydrogenation with its associated catalyst development and testing is certainly one of the principal applications of the reactor. The Parr reactor is being extensively used&nbsp; in hydrometallurgical and hydrothermal conversion of waste streams into valuable products.

<h2>Technical details</h2>

<ul>
	<li>Bench top reactor system</li>
	<li>Alloy600 material magnetic drive</li>
	<li>Max. 500°C, 3000 psi pressure gage &amp; rupture disc</li>
	<li>0-600 rpm, motor control module with RPM set point control, includes tach display</li>
	<li>Flexible graphite sealing</li>
</ul>

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2022-02/parr-reactor-diagram.jpg?itok=sP6bxeaT" alt="Schematic presentation of the Parr reactor" ><figcaption>Schematic presentation of the Parr reactor. Image by CEI research group.</figcaption></figure>

Parr reactor

The Linseis Thermogravimetric analyzer (TGA) is used for testing the thermal and thermochemical conversion of solid samples. In contains an externally heated oven, where the solid samples are placed on a sample holder. Then because of elevated temperature and reactions with feed gases, the weight of the sample changes. The weight is monitored and registered as function of time or temperature. The weight loss data and from that the phenomenon taking place may be used to analyze can be studied, as well as kinetic parameters can be determined for thermochemical reactions.

A mixture of feed gases, such as N2, O2, CO2, CO, H2 and H2O can be fed in the thermobalance. The TGA can operate at constant conditions with gradual temperature elevation. A special feature of the balance is the possibility to increase the heating rate temperature over 10 K/s.

The interesting feedstock samples for the balance include different types of waste biomasses, such as agro and forest biomass.

Thermogravimetric analyzer

The drop-tube reactor (DTR) is used to study the thermal conversion of renewable bio- and waste feedstocks. It enables experimental determination of kinetic parameters for selected chemical reactions. The thermochemical conversion processes may include pyrolysis, gasification, and combustion. Conversion of small feedstock particulates can be measured at up to 1000 °C temperature at different gas atmospheres. The temperature of the particles can be increased by adding oxygen to the gas atmosphere. Moreover, particle size distribution as well as their temperature history can be measured and accounted in the kinetic rate parameter determination. The reactor is at full length 65 cm long. The length can be adjusted with a water-cooled probe. The particle feeding system is best suited for 100-200 µm particles. A combination of CFD modeling and measurements are used to determine the temperature environment inside the reactor. This is a crucial factor in ensuring accurate kinetic modeling and reliable kinetic parameter determination.

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2022-06/dtr.jpg?itok=mOrejQfs" alt="Schematic image of DTR" ></figure>

Drop-tube reactor

The gas conversion reactor mimics a regenerative heat exchanger to investigate hydrocarbon thermal decomposition. The reactor tube is filled with spherical ceramic beads with an approximate diameter of 10 mm. The ceramic beads serve as a heat exchange material that stabilize the temperature and gas flow profiles in the reactor tube. In this setup, there is no bed material circulation. The primary part of the experimental setup is the vertically mounted reactor tube made of Kanthal APM iron-chromium-aluminum (FeCrAl) alloy. The reactor tube has the following dimensions: the inner diameter of 73 mm, the outer diameter of 83 mm and the length of 2500 mm. In order to enable opening and closing of the reactor tube, there are flanges at both ends of the tube. During the operation, the joints of the flanges were sealed with copper seals. The middle part of the reactor tube is electrically heated with three circular Fibrothal RAC 200/500 heating modules which were insulated with Fibrothal insulation modules. Each heating module has a heating power of 19.7 kW. The modules are separately controlled with an Eurotherm 7100 A thyristor unit combined with an Eurotherm 3204 temperature controller. The temperature profile inside the reactor tube is measured by using eight measuring points. The experiments can be conducted with a reactor maximum temperature of 1450 K. Various gas mixtures be used as feedstock.

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2022-06/gas-conversion-reactor.jpg?itok=SPHC0Td6" alt="principle of a gas conversion reactor" ></figure>

Gas conversion reactor

The externally heated pyrolysis oven is used for studying biomass and waste pyrolysis. The oven internal consists of a stainless-steel reactor (Length: 31 cm and outer diameter: 22 cm). When testing, the reactor lid is sealed with graphite gasket and dense screw fastening. Pyrolysis is performed by placing 100-1000 g of biomass sample in the reactor. The sample is heated by placing the reactor in the furnace. Additional heating is provided through a steel coil in the reactor using hot air circulation, and an electric coil connected to a trace heater. As results, the char, oil, and pyrolysis gases are separated from each other during pyrolysis and weighed as separate fractions after each batch to obtain a mass balance. The volatiles (oil and gases) released during pyrolysis are passed through a water-cooled condenser. The oil is condensed and collected in glass bottles while the gases were passed through the exhaust, and not analyzed. Char formed during the reaction is removed from the reactor after pyrolysis and weighed. K-type thermocouples are used to measure the temperature inside the reactor.

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2022-06/pyrolysis.png?itok=Z4Gcjchq" alt="Schematic image of a Pyrolysis oven" ></figure>

Pyrolysis oven

Equipment

MSEE labs

Related infrastructures at Tampere University

Research Infrastructures of Materials Science and Environmental Engineering

Facilities of Energy and Biorefining investigates thermal conversion of fuels and feedstocks. These are for example pyrolysis, gasification and combustion, liquefaction, catalytic pyrolysis, chemical looping process, hydrothermal processing and aqueous phase reforming. With these conversion techniques, various biomass and waste materials can be converted into high-refining value energy products.

<figure role="group"><img src="https://content-webapi.tuni.fi/image-style/max_1300x1300/proxy/public/2024-09/he-chao-221121-jr-01.jpg?itok=ET8QpWp6" alt="Mies laboratoriossa " ><figcaption>Parr reactor. Photo: Jonne Renvall / Tampere University.</figcaption>Photo: Jonne Renvall, Tampereen yliopisto</figure>

Energy and biorefining