Products and Services

Fixed-Bed Reactor Systems

Fixed-bed, tubular reactors are the workhorse reactors of the chemical and petrochemical industry. ILS has designed numerous systems for a variety of applications. ILS recognizes that despite the apparent simplicity of fixed-bed reactors, great attention must be paid to the reactor design in order to insure isothermicity and optimal flow hydrodynamics. We can provide all reagent feeds, downstream workup operations, automated liquid-fraction handling and on-line analytics as needed.

Temperatures to 1000oC
Pressures to 250 Bars
Reactors available in various materials: Stainles-Steel, Hastalloy C276, Iconel, Borosilicate Glass, Quartz, Glass-Coated Steel
Gas-phase reaction fixed-bed reaction systems for partial oxidation reactions and gas-to-liquids have already been produced.
Trickle-phase reaction systems, exhibiting ideal flow hydrodynamics designed for kinetic studies have been provided.
Liquid-phase reaction systems for adsorbent testing studies in dead-volume free microreactors, exhibiting ideal plug-flow have been constructed.
Both single and multiple, parallel fixed-bed reactors for high-throughput catalytic studies can be provided
Inclusion of automated liquid-handling robot for liquid fraction collection and subsequent off-line analysis can be provided
Inclusion of automated liquid-handling systems in combination with rapid GC- and/or HPLC-analytics can be provided for rapid, on-line liquid analysis.
On-line analysis of gas-phase products with GC, micro-GC, IR and FTIR have been performed on numerous systems.
Process automation allowing for the execution of multistep experiments has been designed.
Our Analytical-import tool enables the automatic import of analytical data, which is immediately combined with process-data into a single .csv-table, which can be efficiently mined or imported into virtually any commercially-available visualization program.

High-Throughput Zeolite Adsorption Screening

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.

Micro-Pilot Fischer-Tropsch Synthesis Unit

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.

High-Throughput parallel fixed-bed Reactors

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.

Batch-Reactor Systems

The extreme flexibility of batch reaction systems makes them one of the most widely-used reactor types in the chemical and pharmaceutical industries. ILS has worked with a number of clients in both areas to develop both single and parallel-reactor systems capable of efficiently performing extremely demanding reactions. In particular, we can deliver reactors capable of operating at isothermal or near-isothermal conditions even with very rapid reaction kinetics. Our parallel screening systems allow the testing of air- and moisture-sensitive systems, where large numbers of novel ligands for asymmetric hydrogenations or batch-polymerizations can be rapidly and reproducibly performed.

Semibatch, CSTR-Reactors continuous in either gas- or liquid-phase or both have been provided. Reflux condensers and multiphase-backpressure regulators can be included for a broad range of temperatures and pressures.
Parallel Reactor Systems-10 to 96-parallel systems have already been supplied to customers. The primary areas of interest are for hydrogenation, GTL and polymerization applications. These systems are designed either for primary-screening applications, where large numbers of catalysts may rapidly be screened or for process-improvement applications, where higher-quality data is required.
Internal Recycle Reactors-ILS has worked together with Premex to design two novel types of internal recycle reactors for performing gas, liquid and multiphase kinetic studies. The Turbo-reactor is a unique reactor system capable of achieving extremely high internal-recycle rates even at low pressures, where traditional internal recycle reactors do not perform well. The reactor can be operated at up to 500oC and 200 Bars and is ideal for studying automotive exhaust catalysts, monolith catalysts or gas-phase gas-to-liquid applications.
Maximum pressure-800 bars
Maximum temperature-600oC
Large variety of materials of construction-1.4435, 1.4980, HC22, HC276, Zirconium
Variety of different standard stirrers are available and custom-stirrers can be provided.

High-Throughput Polyolefins Screening Unit

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.

High-Throughput Supercritical Reaction Testing Station

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.

Robotics

When providing high-throughput reaction systems to our clients, we sometimes find that we end up shifting the bottleneck in the high-throughput experimentation cycle from the screening-stage to the catalyst preparation or analysis stage. In such cases, ILS has worked together with Labman to provide customized laboratory robots capable of providing a wide range of different functionalities.

Catalyst Preparation: Our high-throughput batch-testing system for testing air- and moisture-sensitive catalysts requires that the client fill the reactor liners under inert conditions. A glovebox-enclosed liquids and/or slurries handling robot can be provided for such applications. This allows for the efficient and highly-accurate filling of the reactors without wasting valuable glovebox space with the screening system, which is located outside of the glovebox.
Analysis: ILS has recently constructed with Labman a slurries sampling robot, capable of both preparing reaction mixtures for testing (liquids only with manual powder addition) as well as filtering and sampling liquid from the reactors after reaction. Liquid is extracted via disposable PTFE filters and transported to GC/HPLC vials for off-line liquid testing.

High-Throughput Supercritical Reaction Testing Station

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.

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.

Process-Control Systems

An essential part of all of our hardware systems, is a reliable and easy-to-use process control system. The ILS approach to process control is significantly different than many other hardware suppliers, which offer custom, in-house solutions.
ILS uses time-tested, industry-standard process control systems as the foundation for controlling our hardware systems. Our preferred hardware platform of choice is Eurotherm. Euotherm process controllers in combination with the Eurother In-Touch software suite provides a flexible and robust process-control solution, which we can size according to the level of complexity of the system we are working on.

Custom-Systems: ILS has a number of clients, which have in-house standard hardware and/or software platforms, which they prefer to work with. In these cases our process-control experts team up with an expert from our client company and work together to provide a system, which meets our requirements and fully-complies with the standards required by the client. Typical examples include Siemens and Honeywell process controllers and the implementation of iFIX and DeltaV software tools.
Safety and Reliability: Many other hardware suppliers work with PC-based process control systems. The PC represents the weakest chain in the process-control series and the most susceptible to crashes and other defects. At ILS, we have consciously chosen to always control our systems from a robust, industrial process controller operating with redundant safety processors and sensors. This time-tested approach allows us to offer a level of safety and reliability, characteristic of full-scale plants.

Batch Process Optimization Reaction System

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.

Parallel Fixed-Bed Gas-To-Liquids Testing

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.

Custom Software Tools

ILS uses well-known, industrial process-control systems for controlling our systems.In many cases, however, additional tools are required in order to provide our clients with the degree of flexibility and ease-of-operation, which cannot be met with commercially-available solutions.

Integration of On-Line Analytics: The integration of various analytical techniques into our process-controllers is one of our strong points. We have extensive experience in coupling our PCS with various GC systems from well-known suppliers such as Varian, Agilent and Thermo-Electron. A custom-tailored software interface, automatically triggers the GC and downloads the relevant data (volume %, retention time, component i.d., etc). This data is combined with the process data as well as all of the relevant experimental data for the reactor being sampled at that moment. Our system then generates a simple .csv-file, which the client can then import into any commercially-available visualization program. We also have extensive experience with HPLC and FTIR.
Integration of Liquid-Handling Robotics: In a number of cases, ILS has worked together with clients to integrated, complex, liquid-handling robotics into our reaction systems. This is necessary, when clients which to do on-line liquid sampling. We can either incorporate automated liquid-handlers capable of storing samples for later analysis or we can directly integrate Fast-GC techniques, with integrated liquid handlers for direct, on-line liquid analysis.
Recipe Editor for Setting up Experiments: We have designed a recipe-editor tool, which allows the chemist or engineer to design complicated, multistep experiments, which can then be stored for later use and allow for fully-automated execution of multistep experiments. We offer two variations of this program. The first is a simple .csv-based tool, in which the client specified the states of all of the controlled parameters as well as the transition criteria for switching from one state to the next. The second tool has a more advanced graphical-interface, allowing for experimental workflows to be generated and automatically executed.