The challenge in this project was to design a parallel slurry-testing system with independent heating and cooling of each of 4 reactors. Gas uptake is measured in each reactor via two mass-flow controllers, which cover both the high-flow reactant region (at the start of reaction) and the low-flow regime (the last 20% of reaction conversion. This approach gives the user the complete gas-uptake curve and allows one to perform accurate kinetic analysis of 3 phase systems.

Note that this client also requested an ability to easily be able to separate all 4 reactors and use them completely independently in 4 different locations. For this reason a special process-control cabinet was constructed, which allows for 4 separate process-control modules to be separated and transported with the reactors. This flexible, modular approach offered this client the highest-possible flexibility at an attractive price.

This client is interested in studying the intrinsic kinetics of liquid-phase adsorption on zeolitic materials. The experiments are performed at extremely high pressures (250 bar) and elevated temperature 450degC. In order to significantly enhance the client’s experimental throughput, we designed a system in close collaboration with the client, which can simultaneously pretreat 10 catalysts with activation gases and perform 10 adsorption experiments in serial. The unit is completely automated.

One of the greatest challenges of this system was to design a flexible software interface, which allows the client to operate in 5 different liquid sampling modes. These modes allow the client to rapidly collect samples in septum-sealed GC-vials and simultaneously perform on-line analysis of the liquid using a Thermo-Trace fast GC. Injection in the GC can be performed either via a Valco injection valve or via a special in-situ cell, combined with a CTC liquid handler, for rapid injection directly to the FID. The latter provides particularly reproducible chromatograms with extremely sharp, base-resolved peaks.

The unit is plumed with low-dead-volume components allowing for a delta change in concentration to be applied with the ability to view the system response on-line. GC data is automatically imported after the completion of each chromatogram and immediately combined with the system process data in a single .csv file. These files can then be easily viewed using a variety of commercially-available software tools.

This client specializes in the custom-synthesis of fine chemicals for the pharmaceuticals market. Assymetric hydrogenations reactions make up one of the key processes, which they use for creating novel ligands for pharmaceutical clients. The primary challenge in this project was to design a low-cost, manually-operated system, capable of performing multiple experiments in parallel where the reaction medium never comes in contact with air or moisture. The latter criteria is essential in able to be able to obtain reproducible results and ee values when working with homogeneous Ruthenium and Rhodium complexes, which are extremely susceptible to oxidation by water and/or air.

ILS worked together with the client to develop a 48-parallel hydrogenation system, which is separated into 4 different pressure zones. The system allows for reactors to be purged with inert gas and reacted at 4-different pressures simultaneously. Septum-sealed glass liners are used, which minimizes contamination problems and completely eliminates the need to inertize the reactors between reactions. This allows the clients to obtain a significantly higher throughput since there is virtually no downtime required for inertizing reactors.

This client required a system capable of performing parallel, slurry-phase polyolefins synthesis. The system had to be capable of testing 24 polyolefins catalysts without exposing the reaction contents to air or moisture. This is critical because the polyolefin catalysts being tested are extremely air and moisture-sensitive.

ILS worked with the client to design a flexible workstation, capable of reacting 24 samples in parallel. A special reactor design was chosen, which allows for reactors of different volumes to be exchanged. Typical volumes used are approximately 50ml.

Septum-sealed glass liners are used, which minimizes contamination problems and completely eliminates the need to inertize the reactors between reactions. This allows the clients to obtain a significantly higher throughput since there is virtually no downtime required for inertizing reactors.

The system is completely automated and has allowed the client to significantly increase catalyst-screening throughput.

The ability to convert synthesis gas to high-value added fuels is a rapidly growing area. ILS has worked with a number of clients in different areas of Gas-To-Liquids (GTL), converting synthesis gas mixtures to different products.

In this project, the client required a high-pressure system, capable of performing parallel fixed-bed reactions with a sufficiently high data quality to be able to perform kinetic studies and differentiate subtle differences in catalyst performance between catalyst exhibiting similar performance data.

The final product is a 16-parallel fixed-bed reaction system with independent-control of temperature and gas flows capable of calcining, reducing and performing GTL reactions on heterogeneous catalysts in a completely automated fashion. All valves and tubing is mounted in a custom-oven, which can be heated to 200oC to prevent product hardening and/or condensation in downstream lines. Micro-GC’s are used for rapid on-line analysis and liquid-phase products are condensed out.

The system is designed in a modular fashion, with gas and liquid dosing sections, a reaction section and a downstream workup section.

The system is completely automated and includes a recipe-software, which allows the client to design multistep experiments and then execute the experiments in a completely-automated fashion. Data is also automatically imported from the GC’s and combined with process data including all relevant user data and physical property data for the catalyst properties. All data is combined and exported into .csv files, which may be easily exported into commercially-available visualization tools.

ILS has recently designed and constructed a fully-automated micropilot unit
for a client interested in benchmarking commercially-available
extrudate-type catalysts for Fischer-Tropsch synthesis.
    
ILS delivered a system, which was especially designed to deal with the
exceptionally high reaction heats of this reaction. The unit also includes a
CO-carbonyl decomposition reactor, which removes iron and nickel-carbonyls
from the synthesis gas feed, which would otherwise lead to false results
(iron and nickel are excellent water-gas-shift catalysts).

The unit includes on-line micro-GC analysis of the permanent gases
collected after both a high- and low-temperature separation step. The unit
also has completely-automated liquid sampling of both the high- and
low-temperature liquid separators.

The micro-pilot unit represents a significant step in the ability to
scale-up GTL reactions for ILS, a rapidly growing technology sector.

ILS has designed and constructed a number of parallel fixed-bed reactors for
studying the following reactions:

• Gas-to-liquids
• Partial oxidation reactions
• Oxidehydrogenations
• Hydrotreating
• Aldol conversions
• Metathesis
• Isomerization reactions

Our units are designed to operate truly isothermally and have ideal or
near-ideal plug flow. We typically include on-line and/or off-line analytics
such as fast-GC, FTIR and various liquid handlers.

The reactors can be modified to allow for the incorporation or removal of
catalysts without exposing the catalysts to air, thus allowing extremely
accurate pre- or post-reaction analysis of catalyst properties such as
oxidation state, surface area and crystallanity.

A rapidly-growing technology sector is supercritical H2O and CO2 oxidation. Supercritical oxidation using benign oxidants such was water and carbon-dioxide represents an environmentally-benign alternative to many homogeneously-catalyzed systems, which require the use of highly-toxic solvents and/or catalysts.

ILS has worked closely with a number of clients to design systems capable of allowing for the efficient and safe execution of experiments under supercritical conditions.

One system includes a 24-parallel high-throughput testing system capable of screening heterogeneous-catalysts for supercritical oxidation reactions. Each reactor has an individual bursting disc and is independently isolated from all other reactors.

An additional system includes a high-temperature (200oC), high-pressure (200 bar) autoclave with a corrosion-resistant viewing window for observing when the reaction conditions are truly supercritical (disappearance of phase-boundary).

An additional system includes a 10-parallel reactor for the synthesis of novel heterogeneous catalysts under supercritical conditions.

The last system includes a fixed-bed microreactor for testing heterogeneous catalysts under supercritical conditions.

The use of thermostated isco-pumps, allows for the pulsation-free dosing of highly-compressible supercritical CO2. The system is completely automated, allowing for unattended operation.