Parallel high-throughput reactor

Today parallel reactor systems for rapid catalyst testing under real process conditions are state-of-the-art. An example of an integrated system is the 48-parallel high-throughput reactor, which can be apphed to discover and to optimize new heterogeneous catalysts. It provides continuous flow of the reactants through separate... 

Solid-phase chemistry can readily be automated, and is therefore well suited to parallel, high-throughput compound production. Programmable synthesizers with hundreds of reactors for solid-phase synthesis have become commercially available these enable the production of large arrays of compounds (one different compound per reactor). This is usually achieved by performing the same synthesis in each reactor, but using different reagents. 

Decane hydroisomerization experiments were performed using a high-throughput reactor with 16 parallel reactor tubes [12]. Samples were impregnated with an aqueous [Pt(NH3)4]Cl2 solution to obtain a 0.5 wt.% nobel metal loading and then palletized in size between 125 and 250 pm. 50mg of catalyst was loaded in the reactors and activated in-situ at 400°C for Ih in O2, N2 and H2. A fixed contact time of 1656 kg s/mol was used along with a temperature step of 10°C. The reaction was performed at a total pressure of... 

Khmelnitsky and coworkers have also examined microwave-assisted parallel Hantzsch pyridine synthesis [28], They have demonstrated the benefits of microwave irradiation in a 96-well plate reactor for high throughput, automated production of a pyridine combinatorial library (Scheme 8.20). 

Figure 11.21 Results of high-throughput screening of catalysts in a 384-parallel single-bead reactor in a partial oxidation reaction, (a) Arrangement of inactive and total oxidation catalysts in the reactor, (b) screening results for the conversion of a hydrocarbon at 400°C, 1 mL/min per bead.

In the last decade methods of combinatorial catalysis and high throughput experimentation has obtained great interest [1-4]. In the field of heterogeneous catalysis most of the efforts are devoted to the investigation of gas phase reactions, where several hundreds catalysts can simultaneously be tested [5,6]. Contrary to that, in high-pressure liquid phase catalytic reactions in a single reactor module only 8-16 parallel experiments can be performed. There are reports to use up to six modules as a parallel setup [7]. 

The basic challenges for parallel test reactor development for high-throughput experimentation are, apart from technological challenges, related to technical demands that arise with the special issues for parallel test reactors, which are identical with the demands for conventional test reactors for gas-phase reactions. The criteria that must be fulfilled to obtain intrinsic catalyst properties from experimental data relate mainly to mass and heat transfer. A sufficient contact between the reactants and the catalyst must be insured to avoid mass transfer limitations inside and outside of the catalyst particles. Isothermal operation under laboratory conditions and avoidance of heat transfer limitations are also crucial. As a general quality check prior to operation intra- and extra-particle limitations should be... 

Although the direct oxidation of ethane to acetic acid is of increasing interest as an alternative route to acetic acid synthesis because of low-cost feedstock, this process has not been commercialized because state-of-the-art catalyst systems do not have sufficient activity and/or selectivity to acetic acid. A two-week high-throughput scoping effort (primary screening only) was run on this chemistry. The workflow for this effort consisted of a wafer-based automated evaporative synthesis station and parallel microfluidic reactor primary screen. If this were to be continued further, secondary scale hardware, an evaporative synthesis workflow as described above and a 48-channel fixed-bed reactor for screening, would be used. 

High-throughput testing was accomplished using a system of 16 continuous fixed-bed parallel microreactors, able to work up to 80 bar. The principal characteristics of this reactor are summarized as ... 

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