Closing the 1–5 µm size gap: Temperature-programmed, fed-batch synthesis of µm-sized microgels

Ksiazkiewicz, Agnieszka; Jung, Falco; Wolter, Nadja; Viell, Jörn; Mitsos, Alexander; Pich, Andrij

doi:10.1016/j.cej.2019.122293

Cited by 12 publications

(17 citation statements)

References 30 publications

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“…The hydrodynamic microgel diameter was measured for various fractions of fed initiator and cross-linker. The agreement between the experimental data and model simulation was good . The model shows that microgel diameter increases continuously with an increase in the fraction of fed initiator and cross-linker.…”

Section: Sensitivity Of Microgel Size On Synthesis Conditionssupporting

confidence: 55%

“…We described the synthesis of microgels in the μm size range via a fed-batch synthesis with temperature ramp . The employed reactor was a Mettler Toledo RC1e calorimeter with RTcal option.…”

Section: Experimental Setup and Used Reactantsmentioning

confidence: 99%

“…Microgels are functional colloidal polymer networks that respond to environmental stimuli like temperature, pH, light, or pressure with a change in size. , This functionality makes microgels applicable in diverse fields such as engineering, agriculture, and medicine . The diverse applications require microgels with different hydrodynamic diameters . For example, hydrodynamic diameters in the nm range are applicable for drug delivery or wound healing, , while hydrodynamic diameters in the μm range are applicable for microlensing or crystallization studies. , The hydrodynamic diameter largely is determined by the conditions of the microgel synthesis, as microgels are products by process .…”

Section: Introductionmentioning

confidence: 99%

“…Microgels in the nm range have been synthesized with various monomers, functional properties, and cross-linkers. ,,, The common synthesis recipe for microgels in the nm range is a batch reaction carried out at a medium temperature of about 70 °C . Only recently, we established a recipe for the synthesis of N -vinylcaprolactam (VCL)-based microgels in the μm range . We used a fed-batch reaction with a temperature ramp approach and validated respective experimental results using model-based experimental analysis.…”

Section: Introductionmentioning

confidence: 99%

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Model-Based Optimization of Microgel Synthesis in the μm Size Range

Jung

Ksiazkiewicz

Mhamdi

et al. 2020

Ind. Eng. Chem. Res.

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Microgels are functional polymer colloids with diverse applications, for example, in medicine, engineering, or agriculture. Some applications require large microgels in the size range of μm, which could previously only be synthesized using microfluidics or a synthesis procedure involving a fed-batch reaction with a temperature ramp. We use dynamic optimization to determine a simpler synthesis recipe that allows us to synthesize microgels in the μm range using a batch procedure. First, a sensitivity analysis shows that the microgel size is sensitive to the initial concentration of initiator and the reactor temperature. Second, the dynamic optimization yields a batch recipe that provides microgels of the desired μm size range. The recipe uses a low initial initiator concentration and a low reactor temperature. The respective recipe is validated experimentally; model simulation results and experimental measurements of the hydrodynamic diameter show good agreement.

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Section: Sensitivity Of Microgel Size On Synthesis Conditionssupporting

confidence: 55%

Section: Experimental Setup and Used Reactantsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Model-Based Optimization of Microgel Synthesis in the μm Size Range

Jung

Ksiazkiewicz

Mhamdi

et al. 2020

Ind. Eng. Chem. Res.

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“…Microgels are soft polymeric colloids that are well-studied and easily tunable. Fabricated by precipitation polymerization, microgels offer diameters ranging from less than 100 nm 10 up to 11 . Microgels are tunable to respond to an external stimulus like temperature, pH, ionic strength, or pressure by changing their size or charge 12 .…”

Section: Introductionmentioning

confidence: 99%

Unravelling colloid filter cake motions in membrane cleaning procedures

Lüken

Linkhorst

Fröhlingsdorf

et al. 2020

Sci Rep

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The filtration performance of soft colloid suspensions suffers from the agglomeration of the colloids on the membrane surface as filter cakes. Backflushing of fluid through the membrane and cross-flow flushing across the membrane are widely used methods to temporally remove the filter cake and restore the flux through the membrane. However, the phenomena occurring during the recovery of the filtration performance are not yet fully described. In this study, we filtrate poly(N-isopropylacrylamide) microgels and analyze the filter cake in terms of its composition and its dynamic mobility during removal using on-line laser scanning confocal microscopy. First, we observe uniform cake build-up that displays highly ordered and amorphous regions in the cake layer. Second, backflushing removes the cake in coherent pieces and their sizes depend on the previous cake build-up. And third, cross-flow flushing along the cake induces a pattern of longitudinal ridges on the cake surface, which depends on the cross-flow velocity and accelerates cake removal. These observations give insight into soft colloid filter cake arrangement and reveal the cake’s unique behaviour exposed to shear-stress.

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Anisotropic Microgels by Supramolecular Assembly and Precipitation Polymerization of Pyrazole‐Modified Monomers

et al. 2022

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Soft colloidal macromolecular structures with programmable chemical functionalities, size, and shape are important building blocks for the fabrication of catalyst systems and adaptive biomaterials for tissue engineering. However, the development of the easy upscalable and template-free synthesis methods to obtain such colloids lack in understanding of molecular interactions that occur in the formation mechanisms of polymer colloids. Herein, a computer simulation-driven experimental synthesis approach based on the supramolecular self-assembly followed by polymerization of tailored pyrazole-modified monomers is developed. Simulations for a series of pyrazole-modified monomers with different numbers of pyrazole groups, different length and polarity of spacers between pyrazole groups and the polymerizable group are first performed. Based on simulations, monomers able to undergo 𝝅-𝝅 stacking and guide the formation of supramolecular bonds between polymer segments are synthesized and these are used in precipitation polymerization to synthesize anisotropic microgels. This study demonstrates that microgel morphologies can be tuned from spherical, raspberry-like to dumbbell-like by the increase of the pyrazole-modified monomer loading, which is concentrated at periphery of growing microgels. Combining experimental and simulation results, this work provides a quantitative and predictive approach for guiding microgel design that can be further extended to a diversity of colloidal systems and soft materials with superior properties.

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Closing the 1–5 µm size gap: Temperature-programmed, fed-batch synthesis of µm-sized microgels

Cited by 12 publications

References 30 publications

Model-Based Optimization of Microgel Synthesis in the μm Size Range

Model-Based Optimization of Microgel Synthesis in the μm Size Range

Unravelling colloid filter cake motions in membrane cleaning procedures

Anisotropic Microgels by Supramolecular Assembly and Precipitation Polymerization of Pyrazole‐Modified Monomers

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Closing the 1–5 µm size gap: Temperature-programmed, fed-batch synthesis of µm-sized microgels

Cited by 12 publications

References 30 publications

Model-Based Optimization of Microgel Synthesis in the μm Size Range

Model-Based Optimization of Microgel Synthesis in the μm Size Range

Unravelling colloid filter cake motions in membrane cleaning procedures

Anisotropic Microgels by Supramolecular Assembly and Precipitation Polymerization of Pyrazole‐Modified Monomers

Contact Info

Product

Resources

About

Closing the 1–5 µm size gap: Temperature-programmed, fed-batch synthesis of µm-sized microgels