Testing

32-Tube parallel Fixed Bed Reactor unit

The efficient generation of catalytic data is of paramount importance; the objective is to extract the most information possible without compromising quality. High Throughput Evaluation is an enabling technology that allows for the rapid and parallel evaluation of numerous catalyst formulations and/or varying reactor conditions. The technology relies on the miniaturization of conventional micro-reactors and the application of rapid, automated analysis and data interpretation techniques. Fixed bed reactors (FBR) and in particular multi tube parallel FBR units can provide an efficient way to rapidly screen large numbers of small catalyst samples (mg quantities) in a short timeframe. With years of experience in syngas transformations, a high level of technical understanding (in both experimental design and data handling) and state of the art custom designed fixed bed reactor systems, developed in association with our long term collaborators Integrated Lab Solutions GmbH (ILS) we can help you to efficiently generate knowledge. The main unit has been designed to allow both the quick screening of catalysts and the ability to carry out extended runs (160 days). Due to the design of the unit these modes of operation can be achieved simultaneously using the four independent reaction blocks. The flexibility of the unit also allows a variety of conditions to be accessed including the co-feeding of reaction inhibitors and water. The unit consists of 32 reactor tubes and is split into two independent sections each containing 2×8 reactors. Each of the 4 blocks of 8 reactors has its own Ar, CO, H₂ and spare Mass Flow Controllers (MFC). Water (or other liquids) co-feeding is possible via high pressure syringe pumps. Pressure rating 50bar; Temperature rating 470°C; Tube ID=2.4 mm; Typical sample load ~50-200 mg.

4-Tube parallel Fixed Bed Reactor unit

Whilst High throughput methodologies are often used to quickly screen a large number of catalysts using small sample loadings in order to identify promising candidates, further optimisation of the most promising catalysts often requires more flexible operating conditions. This is made possible by the use of our 4-tube FBR unit also from ILS. The flexibility and high accuracy of this unit stems from the fact that each tube operates totally independently, having its own set of mass flow controllers (MFC) and temperature control via a thermocouple inside the catalyst bed. The individual MFCs allow catalysts with different activities to be tested at the same conversions which is often critical for accurate selectivity comparisons. Results obtained on this unit have been used in several patent applications over the years where small differences in activity and/or selectivity provided evidence of novel catalyst properties. Pressure rating 50 bar; Temperature rating 470 °C; Tube ID=6.3 mm; Typical sample load ~400-800 mg.

1 Litre Slurry Reactor

Heterogeneous catalysis can also be conducted in continuous stirred tank reactors, CSTRs: Our laboratory has two 1L slurry reactors. These reactors are custom designed to provide optimal gas, liquid and solid (catalyst) reaction hydrodynamics and allow continuous product removal. Two product knock out pots (hot pot and cold pot) allow for continuous operation for extended periods of time. This is critical for the study of catalyst lifetime and to explore the rate of catalyst deactivation with time online.

Multi-purpose fixed bed reactor

We have a fixed bed reactor supplied by Cambridge Reactor Design suitable for a wide range of applications. It operates at temperatures up to 550 °C and pressures to 20 bar. Gases, liquids or a combination of the two can be used as feeds. A syringe pump enables accurate liquid flow delivery down to very low rates, ca. 10 µL/min, such that small amounts of catalyst can be tested at realistic liquid space velocities. Reaction products are collected in a trap, cooled to sub-ambient temperatures if required, or analysed by on-line GC. In the case of the latter, a heated transfer line, (temperatures up to 120 °C), prevents condensation of moderately volatile species. Computer control facilitates long term experiments where unattended operation is necessary.

Fixed bed reactor for refinery catalysis

We have a purpose-built FBR which is currently configured for the testing of refinery catalysts under industrially relevant conditions. The flexibility of the unit also allows a wide range of other applications. The reactor system has the following specifications:

• Dimension of tubular reactor: ID from 1/4 -3/8 inch for catalyst loading of 0.1 10 g
• Design pressure: 1 60 bar
• Design temperature: up to 550 °C
• Flow rate of gas feed: 0-50 mL/min controlled by Brooks SLA5850C MFC
• Flow rate of liquid or liquefied gas: 0.01 to 10.00 mL/min at a pressure of 0 to 2500 psi delivered by LabAlliance Series I pump

This highly flexible reactor has been successfully used for numerous catalytic evaluations of metal/metal oxides and solid acid catalysts for olefin transformations, alcohol dehydration and CO2/CO hydrogenation reactions under industrial conditions. Equipped with state-of-art safety systems, continuous unattended experiments up to 100 h have been carried out for catalyst life time studies. Detailed on-line and offline product analysis can be used to obtain mass balances for complex multi-phase reactions.

The laboratory is equipped with a purpose-built gas delivery system, including scrubbing trains, capable of supplying ethene, propene, 1-butene, hydrogen, Ar/N2 and vacuum, to each of 7 autoclaves of varying specification. An eighth autoclave is equipped to additionally receive CO2. The MFC system is capable of doping ppm levels of additive/poison gases concomitant with primary feed gas and is routinely used. All the autoclaves are equipped with gas-entraining stirring, internal cooling, electronic temperature and pressure monitoring, and with the exception of the glass units, external fluidised heating-cooling jackets. A purpose-built solvent system, allows 5 solvents to be purified, de-gassed and pumped directly into any vessel, at any pressure. The uptake of substrate gases is monitored via Coriolis flow meters and logged by PC, along with vessel pressure. All autoclaves are coupled directly to gas inlet GC-FID and have liquid phase FID-GC and GC-MS available. We have demonstrated expertise in the acquisition and analysis of kinetic data leading to detailed models suitable for use at commercial scale. All data comes with detailed statistical analysis to determine experimental uncertainty and thus confer confidence in the significance of the data. The equipment is also suited towards toll production for batch sizes up to 1 kg. A number of high pressure 50mL batch autoclaves are also available.

The laboratory is also equipped with: Radleys 6-well (250 mL) parallel reactor, Schlenk lines for catalyst preparation; a GPR-1200 oxygen detector capable of measuring percentage down to ppb levels of oxygen in a range of gas streams; an Ametek 3050-OLV gaseous moisture meter; and a gas detection/alarm system