About 80% of hte’s work is still catalyst related but lately this has been broadened to include process formulations such as surface coatings. The company has long-term collaborative research projects with BASF, Chevron, San Ramon, Calif., and Albemarle, Baton Rouge, La. in the field of refinery catalysis. It also recently announced that it is to collaborate with the Shell Group company CRI Catalyst, Houston, Texas, on the discovery and development of new ethylbenzene dehydrogenation catalysts for styrene monomer production.
The hte equipment finds use in stage I and stage II catalyst-screening systems. The micro-scale stage I “single bead reactor” is akin to the combinatorial methods of drug development, in which uniform spherical 1-mm beads of material are sequentially impregnated to create compositional libraries, with up to 625 beads positioned on a reaction plate no bigger than a credit card (Figure 2). The catalysts are screened at ambient pressure and temperatures up to 400ºC.
Figure 2. This microbead reaction plate serves for stage I catalyst screening.
For stage II work — basically optimizing the process efficacies of catalysts that come through the screening process — hte has developed 16- and 48-reactor systems, designed using CFD to ensure that they behave as ideal plug-flow reactors. Systems are available for reaction pressures up to 150 bar and operating temperatures to 700ºC; hte can configure test units to accommodate its clients’ chemistry as required.
Another research company that has recently branched out into selling HT systems is Avantium Technologies, Amsterdam, the Netherlands, which this year opened a branch office in Davenport, Iowa, “to better service our fast expanding customer base in the U.S.,” according to Guus Scheefhals, chief business officer.
“In the past our business was focused on providing high-value-added research services,” notes Tom van Aken, Avantium’s CEO. However, he explains a change was necessary: “While we’ve been successful in growing our services business [Avantium this year entered into a strategic collaboration with BP to apply HT techniques to R&D related to purified terephthalic acid (PTA)], it became clear to us that we couldn’t access part of the market by selling services only.”
Avantium increased in-house HT capabilities at its Delft facility last year with the installation of its “Polyolefin Platform” — an eight-reactor system with integrated handling of catalysts, co-catalysts and additives under inert atmosphere — which has already attracted “three leading polymer companies” to commit to research projects. At the same time, however, it was launching its first HT tool onto the open market — the Crystal16 system and software for crystallization studies. And it has followed this up in 2006 with the Block96 system, designed for HT experiments on a 1- to 2-ml scale in up to 96 parallel high-pressure batch reactors.
Demuth certainly isn’t alone in seeing a surge of interest in high throughput (HT). “In general, the concept of high throughput experimentation is becoming more widely accepted,” agrees van Aken. Likewise, Duncan Akporiaye, chief scientist with independent research foundation SINTEF, Oslo, Norway, and Houston, Texas, echoes the view. “There was a period when it was rather difficult to try and sell the concept [of HT],” he says, “but in the last couple of years the interest has suddenly taken off. Now most of the major companies are involved in some way.”
SINTEF started developing high throughput systems in 1995 and has had a strategic alliance with process technology licensor UOP, Des Plaines, Ill., since 1997. The first result was a more-environmentally-friendly catalysts system for paraffin isomerization, which now is in regular service at Big West Oil’s refinery in Salt Lake City, Utah. “In this study we were able to look at over 500 formulations in five weeks; using traditional means would have required about a year for preparation and two and a half for testing,” notes Jennifer Holmgren, UOP’s director of exploratory and fundamental research.
Figure 3. This 48-array gravimetric unit is designed for parallel processing applications.
Working with SINTEF, UOP has now put together a procedure, called CombiVision, that uses HT at every stage of development — from material synthesis (of zeolites, for example), through material modification (such as metal loading and ion exchange) and characterization, and finally the reaction assay module — based on SINTEF’s CombiChem parallel technology (Figure 3). “Tying it all together,” says Holmgren, “is an informatics system that includes statistical experiment design, automation, data analysis, visualization and modeling tools.”
Developments elsewhere in Europe also testify to the heightened interest. Chemspeed Technologies, Augst, Germany, and Monmouth Junction, N.J., for example, has worked with BASF on the development of “MiniPlant” reactor technology for HT polymerization studies; flow chemistry specialist Syrris. Royston, U.K., last month launched its new Atlas automated lab synthesis system in the U.S. at the American Chemical Society’s exposition in San Francisco.
Meanwhile, the European Union-funded TopCombi project is now in full swing after its launch last year. A €23-million, five-year project, TopCombi — “Towards Optimized Chemical Processes and New Materials by Combinatorial Science” — is a collaboration between 22 industrial and academic partners from 11 European countries, aimed at developing and applying HT techniques to the discovery of more environmentally friendly catalytic processes. Maria Raimondi, who is with one of the TopCombi partners, Insight Faraday, a U.K.-government HT initiative, says one of the priorities of the program is to develop a central library that will provide both academic and commercial HT research labs with easy access to high quality commercial catalyst samples from producers such as Johnson Matthey, London, U.K., and West Chester, Pa.
Another TopCombi partner, InforSense, London, is contributing that all-important aspect of all high throughput techniques, the “informatics” or IT infrastructure required to handle the vast amounts of reaction data generated by the systems, apply statistical techniques to the design of experiments, and provide the level of automated control necessary for parallel experimentation. (Other companies that have informatics tools on the market include Accelrys, San Diego, Calif., which was set up in 2001 from a group of five scientific software companies involved in everything from molecular modeling to the management and mining of experimental data.)
As Dow’s Swogger says: “The amount of information generated off one of these [HT] systems is awesome. What people don’t realize about HT is that it’s not just a bunch of automated equipment that does hundreds of experiments. If you can’t handle the data you’re in trouble. That’s where we look at the benefits. High throughput is expensive, so you always have to make sure the problems you work on are the ones that are going to pay you back.”
HT is viewed as expensive, agrees Mike Fasolka, director of the Combinatorial Methods Center at the National Institute of Standards and Technology, Washington, D.C. “Many companies believe that getting into HT is too costly for them and, depending on how they go about it, this could be true,” he says. “At NIST our aim is to develop HT techniques which don’t require an expensive laboratory infrastructure.”
Expensive or not, high throughput experimentation certainly looks well placed to boost R&D productivity across the chemical industry.