Dialysis Diffusion Kinetics in Polymer Purification

Schuett, Timo; Geitner, Robert; Zechel, Stefan; Schubert, Ulrich S.

doi:10.1021/acs.macromol.1c01241

Cited by 12 publications

(24 citation statements)

References 40 publications

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“…Prior to this study, we investigated that there is no solvent exchange required to reach the detection limit of the NMR-spectrometer regarding the monomer contaminations when starting with 20 mL of a 0.5 M solution of PMMA and methyl methacrylate (MMA) in THF and 250 mL of surrounding solvent in the dialysis system. 13 Consequently, we continued this study by utilizing the same parameters, but varying the polymer chemistry and monomer type, the dialysis tubing, and the solvent. Specifically, we investigated three common polymer types, PMMA ( P1 and P2 ), polystyrene (PS) ( P3 and P4 ) and poly(poly(ethylene glycol) methyl ether methacrylate) (Poly(PEGMEMA)) ( P5 and P6 ) featuring two different molar masses with 10 000 g mol −1 ( P1 , P3 and P5 ) and 30 000 g mol −1 ( P2 , P4 and P6 ) for each polymer.…”

Section: Resultsmentioning

confidence: 99%

“…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…”

Section: Introductionmentioning

confidence: 99%

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A user-guide for polymer purification using dialysis

et al. 2023

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

A user-guide for polymer purification using dialysis

et al. 2023

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“…Prior to this study, we developed an automated continuous dialysis process, which is compatible to the automated synthesizer [35]. The system was investigated utilizing tetrahydrofuran (THF) as a solvent, which is commonly used in polymer purification [36][37][38][39] and resulted in a monomer removal up to the detection limit of the NMR-spectrometer in less than 48 h [39].…”

Section: Introductionmentioning

confidence: 99%

Fully Automated Multi-Step Synthesis of Block Copolymers

et al. 2022

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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.

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“…For a long time, size exclusion chromatography (SEC) − and nanoporous membrane-based dialysis , are two widely used approaches for the purification of polymers. The SEC method is based on the rule that the polymer fraction with a smaller size elutes later.…”

Section: Introductionmentioning

confidence: 99%

Exploring the Feasibility of Utilizing Nanopore-Based Ultrafiltration for the Purification of Graft-Onto Polymerization Products

Zhou

Yang

et al. 2022

Macromolecules

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Exploring an efficient way to purify the graft-onto polymerization products is an important but challenging problem. This work explores the feasibility of utilizing nanopore-based ultrafiltration for this purpose. First, a library of PPA Nd b -g-PS Nd g -σ graft-onto products with polystyrene (PS) sidechain and poly(propargyl acrylate) (PPA) backbone has been prepared, and the effect of molecular parameters, including contour length (l c ), sidechain radius (R sidechain ), and persistence length (l p ), on the flowassisted translocation and cutoff performance of PPA Nd b -g-PS Nd g -σ through nanopores with diameter D = 20 nm has been studied. At a low macroscopic flow rate Q = 0.2 mL/ h, it is found that for PPA Nd b -g-PS Nd g -σ chains with R sidechain > 1/2D, they are completely retained due to the size-sieving effect. More generally, it is found that the decrease of l c from ∼500 to ∼50 nm and R sidechain from 18.0 to 3.9 nm facilitates the diffusive passage of chains through nanopores; surprisingly, the increase of l p from 5.4 to 22.2 nm also facilitates the process, which actually signifies the possibility of enhanced chain orientation. At a high macroscopic flow rate Q > 0.2 mL/h, the increase in l c and R sidechain results in a larger critical macroscopic flow rate (Q c ) for chains to squeeze into the nanopores. When R sidechain > 1/2D, no l c -dependence is observed for the cutoff performance. Furthermore, it is found that the separation efficiency can be efficiently enhanced by increasing the solution concentration in the regime of C < C* with C* being the overlap concentration, which is demonstrated by one example of the practical purification process of the PPA 780 -g-PS 41 -60% model sample.

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Dialysis Diffusion Kinetics in Polymer Purification

Cited by 12 publications

References 40 publications

A user-guide for polymer purification using dialysis

A user-guide for polymer purification using dialysis

Fully Automated Multi-Step Synthesis of Block Copolymers

Exploring the Feasibility of Utilizing Nanopore-Based Ultrafiltration for the Purification of Graft-Onto Polymerization Products

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