Application 1054 Palladium-containing liquid in a beaker

Palladium catalyst recovery using scavenger resin

Catalyst recovery is an important step in downstream processing. Using an appropriate scavenger resin and a rotating bed reactor to deploy it, the recovery is straightforward and effective.

“Transition metals, and in particular palladium, have been of importance for the development of reactions for the formation of carbon-carbon bonds.” - The Royal Swedish Academy Of Sciences, Palladium-Catalyzed Cross Couplings in Organic Synthesis

Many reactions involving the formation of carbon-carbon bonds, for instance the Wacker process, or the Heck, Sonogashira or Suzuki cross-coupling reactions, utilize transition metals as catalysts. With a heterogeneous catalyst, the separation is straightforward (especially when using a rotating bed reactor), but in the case of homogeneous catalysis, the metal remains in the product after the reaction. The catalyst contaminates the product, and also remains a value worth recovering. Both are valid reasons why recovery of the metal is desirable.

Palladium catalysts can be removed from a liquid using scavenger resins, which are conveniently deployed in a rotating bed reactor. In this application note, we remove from an organic solvent Pd(OAc)₂, or palladium acetate, which is a commonly used catalyst. Initially the liquid has a dark red colour, indicating the presence of the catalyst, and after the scavenging it becomes colourless, signifying that the metal has been scavenged onto the resin.

Dark liquid in a bottle before treatment using a scavenger resin, and clear liquid in the bottle after treatment.

We used 2 mL of the scavenger PhosphonicS SPM32 (200-500 µm) in a rotating bed reactor. 105 mg of Pd(OAc)₂ was dissolved in acetonitrile (50 mL), and the rotating bed reactor was rotated at 1000 RPM. The concentration was determined by spectrophotometry at 400 nm.

98.7% was removed in the first 2 hours, and more than 99.5% was removed in 20 hours.

Bar graph showing the concentration of Palladium before and after remediation using a scavenger resin in a rotating bed reactor.

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