A novel continuous flow system for automated high‐throughput screening, autonomous optimization, and enhanced process control of polymerizations was developed. The computer‐controlled platform comprises a flow reactor coupled to size exclusion chromatography (SEC). Molecular weight distributions are measured online and used by a machine‐learning algorithm to self‐optimize reactions towards a programmed molecular weight by dynamically varying reaction parameters (i.e. residence time, monomer concentration, and control agent/initiator concentration). The autonomous platform allows targeting of molecular weights in a reproducible manner with unprecedented accuracy (<2.5 % deviation from pre‐selected goal) for both thermal and light‐induced reactions. For the first time, polymers with predefined molecular weights can be custom made under optimal reaction conditions in an automated, high‐throughput flow synthesis approach with outstanding reproducibility.

High-resolution FlowNMR was coupled to a continuous flow reactor to monitor polymer molecular weight evolution online by diffusion ordered NMR spectroscopy.

Dialkyl muconates are synthesized from biobased muconic acid. These monomers are shown to be readily polymerized in radical polymerizations, and may serve as alternatives to classical acrylates.

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