Polymerization processes with high reproducibility, traceability, and nontoxic compounds are required for biomedical applications. Here an automated solvent‐free polymerization of hyperbranched polyglycerol has been established on a multiple‐hundred gram scale. Performed is an anionic ring‐opening multibranching (ROMB) polymerization with slow addition of glycidol. The solvent‐free approach avoids commonly used organic solvents during the polymerization and work‐up. Due to the automation of the polymerization process a high reproducibility and traceability is accomplished. The used reactor is equipped with an anchor stirrer and stirrer control, which measures the applied torque. A linear correlation of the increasing torque and the degree of polymerization is observed, which can be used to monitor the molecular weight in situ during the polymerization.
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