Automated Polymer Synthesis Platform for Integrated Conversion Targeting Based on Inline Benchtop NMR.

An automated polymer synthesis platform based on an inline low-field nuclear magnetic resonance spectrometer is developed. Flow chemistry and automated inline analyses are an excellent combination for automated kinetic screening and for self-optimizing reactions with programmable conversion targeting. By monitoring monomer conversion over a continuous range of reactor residence times, the platform is able to construct kinetic profiles of polymerizations in an accurate and efficient way. The machine-assisted self-optimization routine allows the reaction to be stopped at any given preselected conversion, giving rise to unprecedented reproducibility in polymer synthesis.

[1]  S. Perrier,et al.  In Situ NMR Monitoring of Living Radical Polymerization , 2003 .

[2]  M. Eberlin,et al.  Probing the mechanism of the Baylis-Hillman reaction by electrospray ionization mass and tandem mass spectrometry. , 2004, Angewandte Chemie.

[3]  A. deMello,et al.  Intelligent routes to the controlled synthesis of nanoparticles. , 2007, Lab on a chip.

[4]  Gisela Guthausen,et al.  Online Low-Field 1H NMR Spectroscopy: Monitoring of Emulsion Polymerization of Butyl Acrylate , 2010 .

[5]  Klavs F Jensen,et al.  An integrated microreactor system for self-optimization of a Heck reaction: from micro- to mesoscale flow systems. , 2010, Angewandte Chemie.

[6]  Steven V. Ley,et al.  A breakthrough method for the accurate addition of reagents in multi-step segmented flow processing† , 2011 .

[7]  Martyn Poliakoff,et al.  Self-optimizing continuous reactions in supercritical carbon dioxide. , 2011, Angewandte Chemie.

[8]  Holger Löwe,et al.  Microflow Technology in Polymer Synthesis , 2012 .

[9]  M. Fey,et al.  NMR flow tube for online NMR reaction monitoring. , 2014, Analytical chemistry.

[10]  Fan Yang,et al.  Real-time monitoring of living cationic ring-opening polymerization of THF and direct prediction of equilibrium molecular weight of polyTHF , 2014, Chinese Journal of Polymer Science.

[11]  Tanja Junkers,et al.  Photoinduced Sequence-Controlled Copper-Mediated Polymerization: Synthesis of Decablock Copolymers. , 2014, ACS macro letters.

[12]  Richard J Ingham,et al.  Organic synthesis: march of the machines. , 2015, Angewandte Chemie.

[13]  H. Frey,et al.  Copolymerization Kinetics of Glycidol and Ethylene Oxide, Propylene Oxide, and 1,2-Butylene Oxide: From Hyperbranched to Multiarm Star Topology , 2016 .

[14]  M. Maiwald,et al.  Quantitative Online NMR Spectroscopy in a Nutshell , 2016 .

[15]  Joris J. Haven,et al.  Online Monitoring of Polymerizations: Current Status , 2017 .

[16]  Joris J. Haven,et al.  The Kinetics of n-Butyl Acrylate Radical Polymerization Revealed in a Single Experiment by Real Time On-line Mass Spectrometry Monitoring , 2017 .

[17]  C. Hawker,et al.  Rapid Visible Light-Mediated Controlled Aqueous Polymerization with In Situ Monitoring. , 2017, ACS macro letters.

[18]  P. Seeberger,et al.  The Hitchhiker's Guide to Flow Chemistry ∥. , 2017, Chemical reviews.

[19]  Tanja Junkers Precise Macromolecular Engineering via Continuous-Flow Synthesis Techniques , 2017, Journal of Flow Chemistry.

[20]  Geoffrey R Akien,et al.  Enhanced process development using automated continuous reactors by self-optimisation algorithms and statistical empirical modelling , 2018, Tetrahedron.

[21]  M. Rubens,et al.  Precise Polymer Synthesis by Autonomous Self-Optimizing Flow Reactors. , 2019, Angewandte Chemie.

[22]  F. Casanova,et al.  Progress in low-field benchtop NMR spectroscopy in chemical and biochemical analysis. , 2019, Analytica chimica acta.