Fully Automated Multi-Step Synthesis of Block Copolymers

Abstract

An automated synthesis protocol is developed for the synthesis of block copolymers in a multi-step approach in a fully automated manner. For this purpose, an automated dialysis setup is combined with robot-based synthesis protocols. Consequently, several block copolymerizations are executed completely automated and compared to the respective manual synthesis. As a result, this study opens up the field of autonomous multi-step reactions without any human interactions.

Application of Digital Methods in Polymer Science and Engineering

“…In addition, a corresponding approach could also be linked to monitoring using online NMR spectroscopy, which enabled the investigation of kinetics [ 77 ] and the influence of polymers on the purification rate, [ 78 ] but also the fully automated synthesis of block copolymers with incomplete conversion during the reactions. [ 79 ] First, a polymer was produced using RAFT polymerization in the synthesis robot, purified, and then converted into the block copolymer in the synthesis robot. Ultimately, this even enables the fully automatic synthesis of a pentablock copolymer.…”

A user-guide for polymer purification using dialysis

“…Prior to this study, we developed a semi-automated dialysis system 25 and investigated the best performance parameters via in situ NMR spectroscopy in regard to solvent flow, volume, and starting concentration for the purification of poly(methyl methacrylate) (PMMA) in tetrahydrofuran (THF). 13 Furthermore, we also tested the new setup in fully automated operation mode 26 and for nanoparticle purification successfully. 14…”

“…16,23,24 Prior to this study, we developed a semi-automated dialysis system 25 and investigated the best performance parameters via in situ NMR spectroscopy in regard to solvent flow, volume, and starting concentration for the purification of poly(methyl methacrylate) (PMMA) in tetrahydrofuran (THF). 13 Furthermore, we also tested the new setup in fully automated operation mode 26 and for nanoparticle purification successfully. 14 In the present study, we investigate in detail a variation of the polymer chemistry and the respective monomer type, the polymer molar mass, the dialysis tubing molar mass cut-off limit, and the solvent.…”

A modular low-cost automated synthesis machine demonstrated by ring-opening metathesis polymerization

“…Current research has focused on developing automated methods for synthesizing and characterizing libraries of compounds. [2][3][4] This has significantly accelerated the discovery of new materials for various applications, including energy storage and conversion, [5][6][7][8] polymers, [9][10][11][12][13][14][15] catalysis, [16][17][18][19][20] and drug discovery. [21][22][23][24] Several of these discoveries have relied on advanced statistical methods for experimental design e.g.…”