Early-stage catalyst R&D often requires synthesizing and testing as many catalysts in as short a period of time as possible. ILS can provide a number of different units to meet these goals.
Fixed Bed Reactors: 16-, 32- and 48-parallel, fixed-bed reactors provide a quantum leap in catalyst screening capabilitiy. Our attention to proper reactor design insuring true plug-flow, catalyst wetting and isothermicity insure that you get scalable data for your most challenging heterogeneous catayst R&D projects
Batch & CSTR Reactors: 10 to 96-parallel batch reactors have been provided for clients for challenging applications involving the screening of minute amounts of moisture- and air-sensitive reactions.
Units and Case Studies
16-Parallel Trickle flow Reactor
The group of Prof. Marin at the University of Gent approached ILS to provide a 16-parallel trickle flow reactor. This had to be an extremely flexible unit that could be used both for high-temperature gas-phase reactions at up to 700°C as well as lower-temperature trickle-flow reactions at up to 100 Bar.
This unit offers unprecedented flexibility by having the possibility to operate each segment of 4-reactors with different flow rates, gas and liquid compositions and temperatures. This represents a significant deviation from other high-throughput units, which often operate with all reactors at identical conditions of pressure, temperature and composition.
Integration of three on-line gas-chromatographs means that three different gas-phase product analysis can be carried out simultaneously. This significantly accelerates measurement time and adds flexibility. A liquid-fraction collection robot continuously separates gas- and liquid-product, collecting the liquid and passing the gases and vapors to the gas-phase analytics.
32-Parallel Fischer Tropsch Testing Unit
Sasol needed a high-throughput tool to substantially increase their capacity for testing Fischer Tropsch catalysts without increasing their need for more unit operators. It was important to have a system capable of both catalyst screening as well as ageing and kinetics testing, and they needed an increase in reactor channels while keeping catalyst amounts to a minimum.
Our design split the unit into two 16-parallel sections with each one dedicated for the respective catalyst tests – screening and ageing. The fast screening unit was euipped with a fast cold tail-gas analysis allowing to quickly determine potential catalyst candidates and the long-term testing section had a hot tail-gas GC included, which allows to detect up to C10 hydrocarbons and alcohols. A carbonyl purification reactor in the feed section prevents low amounts of iron- or nickel carbonyls from decomposing on the catalyst surface and possibly falsifying data; a particularly large problem for long time-on-stream runs.
The system has operated successfully for more than 7 years and provides Sasol with a powerful tool for catalyst screening and stability testing with 32 channels in total while keeping the operator load to a minimum. The quick sealing system online analysis methods have resulted in higher speed improved carbon balance as well as the ability to derive Flory-Schulz distribution plots directly from the on-line data produced. The possibility to study the kinetics of olefin incorporation and steaming ageing effects or water co-adsorption on the reaction make the system even more versatile and powerful.
Multipurpose 16-Parallel Ultra-high pressure Trickle Flow Unit
For this particularly challenging project, ILS was approached by Evonik interested in having a flexible, High-Throughput reactor unit capable of operating up to 300Barg. The reactors should be designed for speciality-chemicals production in trickle-flow mode with ability to dose liquid gases as well as viscous feedstocks.
For this application, ILS first performed a large series of feasibility tests upfront using their unique feedstock liquids in order to demonstrate the ability to perform reliable single-stage, 2-phase backpressure control and still close the mass-balance. This is often challenging as mist- or aerosol formation can result in significant liquid materials losses. ILS was able to “tweak” the suggested design appropriately and clearly demonstrate to the client an ability to perform the 2-phase, 300-bar backpressure control in single step with neglegible materials losses. Only then did ILS move on to the final design and construction phases of the fully automated unit.
Liquid gases are dosed in the liquid phase and quantitatively measured using mini-coriolis mass-flow-control technology. Viscous feedstocks are stored in weighed, heated and pressurized feed barrels and dosed with high-temperature dosing pumps. The unit has a fully-integrated liquid-fraction collection robot, which can collect samples from all 16 reactors in parallel. The liquid-fraction collection vials are simultaneously the gas-liquid separators. An on-line GC provide analysis of the gaseous products formed.
The unit is for more than 2 years in successful operation and provides Evonik with a powerful multipurpose tool being able to study a variety of trickle flow reactions. The low amount of catalysts and feedstocks required combined with the online analytics, robotics and the ILS quick-loading system decrease the human effort needed and reduce the running costs. Increased number of reactors coupled with high data quality significantly improved the speed for Evonik to develop and improve their catalyst business.
20-Parallel Asymmetric Hydrogenation/Carbonylation Reactor
Syngenta approached us with a request to have a cost-effective, reliable, flexible and easy to operate high throughput system for screening of air- and moisture sensitive homogeneous and heterogeneous catalysts in a corrosive environment. To overcome this challenge we designed them a manually operated 20-parallel screening unit with two temperature blocks with 10 high-pressure reactors in each segment. Each temperature block of 10 reactors was split into 2-rows of 5 reactors operating at separate pressures, designed for 100barg and 200°C in this case.
The reaction media are contained completely within a HPLC-type, septum-sealed glass vials, which are magnetically stirred via a teflon-coated magnetic stirrer. The design used ensures there is no pressure gradient over the glass wall of this vessel meaning that reactions up to high pressure can be tested. There is zero cleaning required after reaction as the reagents are completely contained within the glass vial. The pressures vessels and needles have been manufactured in Hastelloy C for excellent corrosion protection.
The tool was delivered in less than 5 months after the order. Because of the small footprint our unit required no additional infrastructure investment but could be installed in an existing fumehood. The handover & training was successfully finished in one week on-site at Syngenta. The ease of use combined with the fast delivery time quickly improved Syngenta’s screening capacity for very low amounts of moisture- and air-sensitive catalysts. Also the flexibility and extremely low (1-2 weeks) downtime per year make this system a very helpful R&D catalyst screening tool.