OPTIMISATION TOOLS

Our optimisation test units allow researchers to improve the yields, selectivities or reaction conditions of a process established in early development studies. Precise process condition control combined with high quality online or offline data enables in depth studies of the optimum conditions. Finely engineered reactors working in batch or CSTR mode, or as fixed-bed systems, help our customers feel confident they’ve discovered the right process to scale-up.

Fixed Bed Units and Case Studies

6-parallel Multi Reactor Catalyst Testing Unit

This is an example for a Multi Reactor Catalyst Testing unit, which we have designed for Repsol as multipurpose tool for catalyst and feedstock evaluation for hydroprocessing reactions (e.g. hydrodesulfurization and hydrocracking). The greatest challenge in this project was to design a unit that fulfils all budget, space and safety requirements while providing a large flexibility in operating conditions (T, P, F,X) as well as the capability to handle a large variety of feedstocks and products. Also unit robustness was key element as catalytic studies up to multiple months need to be executed.

Reactors can be individually operated as well as sets of two (3×2). Therefore ILS chose to design the unit in a modular fashion to reduce engineering and cabling work as well as minimizing footprint while providing good user access. The hard- and software was designed according to the standards of Repsol, which allows future expansions and also makes operation and service much easier.

High-temperature, high pressure diaphragm pumps in combination with high-temperature coriolis flow meters have been selected to dose different feedstocks independently of their properties. Optimized Reactors in multi-zone split shell ovens give enough space for larger catalyst amounts while ensuring plug-flow conditions, avoiding wall effects and axial dispersion. The pressure control and gas/liquid separation and striping section was designed to handle huge variations in pressures and flows by using novel 2-phase membrane pressure controllers. An integrated online GC, as well as exit gas flow meters and automatic liquid product recovery and sampling has been used to provide a tight mass balance.

Altogether this gives Repsol a powerful tool with high flexibility to support the refineries and productions sites much quicker. Also catalyst evaluation capacity and data quality could be improved without the need to hire more operators.

4-Parallel Fixed-Bed Bitumen Hydrotreater

The H&R Refinery in Germany is a world-class refiner specialized in hydrocracking and hydrotreating particularly difficult, heavy feedstocks.

ILS designed a unique, 4-parallel fixed-bed testing unit for H&R capable of reliably, continuously treating even the heaviest of feeds like asphaltene-rich bitument feedstocks. The unique feed design enables high-pressure dosing of liquid bitumen at extremely low flowrates resulting from the low LHSV’s at which these catalsts operate.

The unit was designed to not be susceptible to problems such as ammonium bisulphite formation and blockage in downstream tubing. The use of large, convection ovens instead of more traditional heat-tracing and insulation combined with a unique quick closure system makes the unit very user friendly.

Both hot and cold liquid fractions are continuously collected and an on-line GC provides continuous analysis of all vapor-products formed as well as calculating the volume change during reaction via measurement of an additional internal standard.

4-Parallel deNOx SCAT Synthetic Gas Automotive Catalyst Testing Unit

This automotive testing unit represented our 5th-generation testing unit, where the client can both test catalyts as well as use the unit to evaluate the performance of different automotive emmissions sensors such as Nox and Lamda sensors under extremely well-controlled conditions. The fully-automated unit has been specifically designed to allow for seamless integration of a variety of different sensors from different suppliers with maximum flexibilty needed for sensor evaluation studies. 5Hz rich/lean switching and an ever increasing dynamic oven (50°C/s) represented yet another step-change improvement for ILS NOx testing units.

In this 4-parallel dynamic synthetic test bench we combined the strength of parallel reactor testing with the ability to do rich/lean switching as well as have increased heating and cooling capability in order to better-simulate new European Driving cycles. The on-line analytics are fully-integrated and the easy-to-use Integrated Workflow Manager from ILS makes the programming of multistep driving cycles extremely simple and reproducible.

CSTR Units and Case Studies

4-Parallel Slurry Fischer-Tropsch Testing Unit

ILS was approached by one of its oldest clients to develop a unique, 4-parallel slurry Fischer-Tropsch testing system. This client is one of the worlds major Fischer-Tropsch wax manufacturers. ILS was chosen both for it’s excellent track record with this client as well as because of the large number of both fixed-bed and slurry Fischer Tropsch units that ILS had already made. Issues around reactor hydrodynamics and heat removal were well known to us at the time.

The client wished to have 3L reactors, which could be operated fully independently and operated 24/7 in a fully-automated way. ILS designed a novel low-flow dosing system for feeding mg/min quantitites of water and alpha-olefins to the reactors for kinetic testing. The ability to do sulphur poisoning studies was also included. Inclusion of carbonyl capture reactors to the feed section insured that no nickel or iron carbonyls formed in the CO storage bottles would deposit on the catalyst surface potentially falsifying data. The unique combined ILS liquid-level control and slurries separaiton system insures that the wax level is exactly regulated and that the outlet lines to not block even when operating with very high solids contents of extremely fine FT-Slurries. Inclusion of on-line gas-phase GC-analytics as well as fully automated wax and water/alcohol collection mean that only a limited staff is required to operate the unit.

The unit was successfully delivered to our client and it has been in operation for 8 years now and continues to produce valuable data for this client. This represents yet another of the many GTL systems that ILS has had the pleasure of making over the last 14 years.

4-Parallel Heavy Oil Hydrotreater

Low crude prices mean that refineries today are turning out record amounts of product and attractive margins. The ability to convert bottom-of-the-barrel products to valuable fuels presents an excellent opportunity for refiners to generate significant revenue out of an otherwise low-value-added product. Additionally the ability to convert non-conventional hydrocarbon sources like tar-sands to fuels and(/or chemicals is an attractive option given the right macro-economic environment.

An existing ILS client initially approached ILS for help in getting an existing laboratory set-up that had been made by an ILS competitor running. ILS collaborated closely with the client on this project to help them solve the problems with their existing unit. It was this flexibility and in-depth engineering knowledge as well as a proven track-record that resulted in this client coming back to ILS to acquire a new laboratory test unit for heavy oil upgrading.

The unit consists of 4 parallel batch reactors plus a separate pre-sulphiding reactor, which was used for catalyst pre-sulphiding. One of the major challenges of this unit was the high reaction temperature and issues around reactor fouling. Feedstocks containing significant amounts of asphaltenes are prone to fouling. ILS desinged the unit in such a way that products were not stripped off, which would otherwise result in asphaltene precipitation and subsequent coke formation. Special high-temperature autoclaves, with long operating lifetimes were successfully made. Implementation of a custom oven as opposed to cumbursome heat-tracing and insulation meant that a design could be made where all parts were easily accessible and maintained. This was particularly important to make possible the measuring of both hot- and cold-product fractions, which had been formed in small amounts. This, combined with the implementation of a powerful on-line micro-GC meant that excellent mass-balances could be obtained with this set-up.

Last-but-not-least the unit was co-developed with the safety and automation group of our client. This company has extremely high standards in both areas. As a result of this, the unit could quickly be approved, commissioned and operated. The project was done on -time and to the complete satisfaction of this client.

4-Parallel Polyolefins Process-Optimization Unit

The world demand for polyolefins is rapidly growing. This, combined with the record low prices of olefin monomer feedstocks is resulting in a real rennaisance in polyolefins catalysis R&D.

ILS was chosen by Evonik due to our proven track-record of having designed and delivered multiple, high-throughput polyolefins testing systems. This was the first major project ILS did with Evonik. An additional reason for chosing ILS for this project was the high-degree of customization, which Evonik required. ILS worked hand-in-hand with Evonik process, automation and safety engineers to design a custom-tailored unit that met or exceeded Evonik’s expectations.

The unit had to be designed to fit into an extremely small laboratory space. An inert glovebox had to be seamlessly incorporated with the 4 batch reactors to insure that the air and moisture sensitive catalysts and co-catalysts were never oxidized. ILS made highly-customized reactors, requiring minimum space with special stirrers and an automated pneumatic-lift system to make the unit as compact and yet ergonomically attractive as possible. Having the reactors outside of the glovebox as opposed to inside makes cleaning and maintenance much easier.

Low flows of liquid-gas monomers could be quantitatively dosed using novel mini-coriolis mass-flow technology. Fully-automated, high-pressure catalyst and co-catalyst injection maximizes reproducibility.

2-Parallel Residual Hydrotreater

The ability to upgrade heavy residual products can significantly improve refiners margins. For this reason, there is a great deal of interest in this topic at the moment. ILS was charged with designing, constructing and chemically validating a 2-parallel x 250ml high-pressure (200 Bar) high-temperature (550°C) heavy-oil hydrocracker. The unit is unique in its ability to do high-pressure liquid sampling during reaction.

Seamless integration of a high-temperature on-line GC makes continuous analysis of up to C10 products possible. The same GC has an exchangeable liquid-autosampler, which can be used for more detailed liquid analysis of products formed via SimDist or a more-detailed liquid PIANO analysis.

The unit is fully-automated and was chemically validated using real chemicals in the ILS laboratory prior to delivery.