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Reversed Synthesis Workflow: Powder Dispensing of Carrier to Impregnation Solution

IP.com Disclosure Number: IPCOM000127009D
Publication Date: 2005-Aug-17
Document File: 2 page(s) / 37K

Publishing Venue

The IP.com Prior Art Database

Abstract

One known synthesis workflow for the high throughput preparation of supported metal catalysts consists of first slurrying or powder dispensing a carrier to vials followed by liquid dispensing of a premixed impregnation solution from a microtiter plate to the carrier in the vials that are mounted on vortexers, vibrators, orbital shakers etc. and thoroughly agitating or fluidizing while dispensing the liquid to ensure uniform metal distributions over the carrier particles. A new workflow with reversed order of addition is proposed and already practiced for the preparation of supported catalysts consisting of premixing the impregnation solution in the library or even reactor vials (skipping the transfer step from the microtiter plate) followed by powder dispensing the carrier into the solution.

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Reversed Synthesis Workflow: Powder Dispensing of Carrier to Impregnation Solution

One known synthesis workflow for the high throughput preparation of supported metal catalysts consists of first slurrying or powder dispensing a carrier to vials followed by liquid dispensing of a premixed impregnation solution from a microtiter plate to the carrier in the vials that are mounted on vortexers, vibrators, orbital shakers etc. and thoroughly agitating or fluidizing while dispensing the liquid to ensure uniform metal distributions over the carrier particles. A new workflow with reversed order of addition is proposed and already practiced for the preparation of supported catalysts consisting of premixing the impregnation solution in the library or even reactor vials (skipping the transfer step from the microtiter plate) followed by powder dispensing the carrier into the solution.

The usual or common synthesis workflow consists of premixing metal stock solutions in a microtiter plate to form the final multi-component impregnation solution followed by transfer of aliquots of the impregnation solution from the microtiter plate to the library or reactor vials containing the carrier to accomplish the carrier impregnation. While dispensing the liquid, the carrier particles are thoroughly agitated or fluidized (by mounting the rack of vials on vortexers, orbital shakers, vertical vibrators etc.) to make sure all the carrier particles are uniformly wetted and metal gradients across the fixed bed due to chromatographic effects are excluded. However, the high mechanical stress imparted by the agitation to the carrier particles results in attrition, undesirable particle break up into smaller particles and production of fines that might clog the sieves downstream the reactor and lead to increased and unequal pressure drop across the fixed beds.

The proposed reversed workflow consists of premixing the impregnation solution first by robotic or manual dispensing from metal stock solutions directly into the library or reactor vials (thus skipping the microtiter plate transfer step) followed by powder dispensing the carrier into the impregnation liquid (i.e. let the carrier drop into the liquid by gravity) thus avoiding any mechanical stress on the carrier particles, accomplishing very short mixing times of less than a second and immediate contact of carrier with liquid (i.e. much shorter mixing times than can be achieved by dispensing liquid to the carrier), avoiding metal gradients and chromatography effects due to the instantaneous carrier-liquid contact, avoiding the ‘snowball’ effect (particles start sticking together, stop fluidizing and sediment to the bottom of vial when...