This README_Supplementary_Data.txt file was generated on 2025-03-04 by Kathrin Marina Eckert (kathrin.eckert@tuhh) ------------------- GENERAL INFORMATION ------------------- Name: Kathrin Marina Eckert (ORCID: 0000-0002-8454-4886) Role/Function: Data Collector, Data Curator (main contact person) Institution: Institute of Thermal Separation Processes, Hamburg University of Technology Address: Eißendorfer Straße 38, 21073 Hamburg, Germany Email: kathrin.eckert@tuhh.de Name: Jelisa Christin Bonsen Role/Function: Data Collector Institution: Institute of Thermal Separation Processes, Hamburg University of Technology Address: Eißendorfer Straße 38, 21073 Hamburg, Germany Name: Anja Hajnal (ORCID: 0000-0002-9010-7877) Role/Function: Data Collector Institution: Institute of Thermal Separation Processes, Hamburg University of Technology Address: Eißendorfer Straße 38, 21073 Hamburg, Germany Name: Johannes Gmeiner Role/Function: Contributing Researcher Institution: Institute for Technical and Macromolecular Chemistry, University of Hamburg Address: Bundesstrasse 45, 20146 Hamburg, Germany Name: Jonah Hasse Role/Function: Contributing Researcher Institution: Institute for Technical and Macromolecular Chemistry, University of Hamburg Address: Bundesstrasse 45, 20146 Hamburg, Germany Name: Muhammad Adrian (ORCID: 0009-0008-3634-9518) Role/Function: Data collector Institution: Institute for Process Imaging, University of Hamburg Address: Denickestraße 17, 21073 Hamburg, Germany Name: Julian Karsten (ORCID: 0000-0002-8243-4114) Role/Function: Data collector Institution: Institute of Chemical Reaction Engineering, Hamburg University of Technology Address: Eißendorfer Strafe 38, 21073 Hamburg, Germany Name: Patrick A. Kißling (ORCID: 0000-0001-5596-9976) Role/Function: Data Collector Institution: Institute of Chemical Reaction Engineering, Hamburg University of Technology Address: Eißendorfer Strafe 38, 21073 Hamburg, Germany Name: Alexander Penn (ORCID: 0000-0001-5596-6310) Role/Function: Principal Investigator Institution: Institute for Process Imaging, University of Hamburg Address: Denickestraße 17, 21073 Hamburg, Germany Name: Bodo Fiedler (ORCID: 0000-0002-2734-1353) Role/Function: Principal Investigator Institution: Institute of Polymers and Composites, University of Hamburg Address: Denickestraße 15, 21073 Hamburg, Germany Name: Gerrit A. Luinstra (ORCID: 0000-0003-4602-8319) Role/Function: Principal Investigator Institution: Institute for Technical and Macromolecular Chemistry, University of Hamburg Address: Bundesstrasse 45, 20146 Hamburg, Germany Name: Irina Smirnova (ORCID: 0000-0003-4503-4039) Role/Function: Principal Investigator (alternative contact person) Institution: Institute of Thermal Separation Processes, Hamburg University of Technology Address: Eißendorfer Straße 38, 21073 Hamburg, Germany Email: irina.smirnova@tuhh.de Name: Alena Sophie Steinbach Role/Function: Data Collector Institution: Institute of Thermal Separation Processes, Hamburg University of Technology Address: Eißendorfer Straße 38, 21073 Hamburg, Germany Date of data collection: November 2022 - March 2025 Location of data collection: Institute of Thermal Separation Processes, Hamburg University of Technology, Hamburg, Germany Funding: This project is funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) – SFB 1615 – 503850735. --------------------------- SHARING/ACCESS INFORMATION --------------------------- Title of data set: "Dataset on Swelling Behavior and Kinetics of pNIPAM Lyogels with Varying Polymer Formulations and Solvents" DOI of data set: https://doi.org/10.15480/882.15062 Handle: https://hdl.handle.net/11420/55308 Keywords: swelling kinetics, polymer, semi-IPN, solvent-induced, stimuli-responsive gels, smart reactors --------------------- DATA & FILE OVERVIEW --------------------- ### 1. Chemicals.csv (creation date: 01.03.2025, version: 01) - **Description:** List of chemicals used in the study. - **Columns:** - Chemical: Name of the chemical used - Purity: Purity of the chemical used - Supplier: Supplier of the chemical used - CAS-Nr.: CAS-Nr. of the chemical used ### 2. Formulation.csv (creation date: 01.03.2025, version: 01) - **Description:** List of chemicals used in the study. - **Columns:** - Network type: Differentiation between Semi-IPN (semi-interpenetrating network) and homopolymers. - Formulation: Name of formulation. - MBA:NIPAM [gMBA/gNIPAM]: Ratio of crosslinker to monomer (MBA to NIPAM). - NIPAM:PVA [gNIPAM/gPVA]: Ratio of monomer to polymer (NIPAM to PVA). ### 3. Degree_of_swelling.csv (creation date: 01.03.2025, version: 01) - **Description:** Degree of swelling (DoS) of pNIPAM lyogels in pure organic solvents. - **Columns:** - Formulation: The name of the gel formulation used in the analysis. - Freeze-thaw cycle: The number of performed freeze-thaw cycles before the analysis. - Degree of swelling [g/g]: Degree of swelling measured after equilibration. - Solvent: Organic solvent in which the gel is immersed. ### 4. Relaxation_time.csv (creation date: 01.03.2025, version: 01) - **Description:** The transverse relaxation time t_2 determined from NMR relaxometry for varying formulations and postmodification using freeze-thaw cycles. - **Columns:** - Formulation: The name of the gel formulation used in the analysis. - Freeze-thaw cycle: The number of performed freeze-thaw cycles before the analysis. - Transverse relaxation time T2 [s]: The transverse relaxation time determined from NMR relaxometry using monoexponential fitting. ### 5. Youngs_Modulus.csv (creation date: 01.03.2025, version: 01) - **Description:** Mechanical analysis of varying hydrogel formulations (compressive Young´s Moduli). - **Columns:** - Formulation: The name of the gel formulation used in the analysis. - Freeze-thaw cycle: The number of performed freeze-thaw cycles before the analysis. - Young’s Modulus: The Young´s Modulus obtained from uniaxial compression tests [kPa] ### 6. Kinetic_homopolymers_varying_crosslinker_absolute.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM homopolymers (pNIPAM-1, pNIPAM-2, pNIPAM-5) during solvent exchange from ethanol to ethyl acetate in absolute numbers for crosslinker concentrations (diameter d5). The time is for the same for all data series, the single data series (pNIPAM-1, pNIPAM-2, pNIPAM-5) contain of normalized volume and standard deviation and are separated by an empty column. - **Columns:** - time t: Time of the experiment in h (hours). - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1. - Std Dev: Standard deviation of the volume over time of pNIPAM-1. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-2. - Std Dev: Standard deviation of the volume over time of pNIPAM-2. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-5. - Std Dev: Standard deviation of the volume over time of pNIPAM-5. ### 7. Kinetic_homopolymers_varying_crosslinker_dimensionless.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM homopolymers (pNIPAM-1, pNIPAM-2, pNIPAM-5) during solvent exchange from ethanol to ethyl acetate in dimensionless numbers for crosslinker concentrations (diameter d5). The single data series (pNIPAM-1, pNIPAM-2, pNIPAM-5) contain of dimensionless time, normalized volume and standard deviation and are separated by an empty column. - **Columns:** - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-1. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1. - Std Dev: Standard deviation of the volume over time of pNIPAM-1. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-2. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-2. - Std Dev: Standard deviation of the volume over time of pNIPAM-2. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-5. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-5. - Std Dev: Standard deviation of the volume over time of pNIPAM-5. ### 8. Kinetic_homopolymers_varying_diameters_absolute.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM homopolymer (pNIPAM-1) during solvent exchange from ethanol to ethyl acetate in absolute numbers for varying diameters (d3, d5, d10). The time is for the same for all data series, the single data series (pNIPAM-1, d3; pNIPAM-1, d5; pNIPAM-1, d10) contain of normalized volume and standard deviation and are separated by an empty column. - **Columns:** - time t: Time of experiment in h (hours). - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1, d3. - Std Dev: Standard deviation of the volume over time of pNIPAM-1, d3. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1, d5. - Std Dev: Standard deviation of the volume over time of pNIPAM-1, d5. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1, d10. - Std Dev: Standard deviation of the volume over time of pNIPAM-1, d10. ### 9. Kinetic_homopolymers_varying_diameters_dimensionless.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM homopolymer (pNIPAM-1) during solvent exchange from ethanol to ethyl acetate in dimensionless numbers for varying diameters (d3, d5, d10). The single data series (pNIPAM-1, d3; pNIPAM-1, d5; pNIPAM-1, d10) contain of dimensionless time, normalized volume and standard deviation and are separated by an empty column. - **Columns:** - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-1, d3. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1, d3. - Std Dev: Standard deviation of the volume over time of pNIPAM-1, d3. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-1, d5. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1, d5. - Std Dev: Standard deviation of the volume over time of pNIPAM-1, d5. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-1, d10. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-1, d10. - Std Dev: Standard deviation of the volume over time of pNIPAM-1, d10. ### 10. Kinetic_homopolymers_varying_solvents.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM homopolymers (pNIPAM-2) for varying solvents in dimensionless numbers (d10).The single data series (acetic acid to butyl acetate; acetic acid to methyl acetate; 1-butanol to butyl acetate; methanol to methyl acetate) contain of dimensionless time, normalized volume and standard deviation and are separated by an empty column. - **Columns:** - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-2, d10 during solvent exchange from acetic acid to butyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-2, d10 iduring solvent exchange from acetic acid to butyl acetate. - Std Dev: Standard deviation of the volume over time of pNIPAM-2, d10 during solvent exchange from acetic acid to butyl acetate. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-2, d10 during solvent exchange from acetic acid to methyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-2, d10 during solvent exchange from acetic acid to methyl acetate. - Std Dev: Standard deviation of the volume over time of pNIPAM-2, d10 during solvent exchange from acetic acid to methyl acetate. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-2, d10 during solvent exchange from 1-butanol to butyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-2, d10 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of pNIPAM-2, d10 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of pNIPAM-2, d10 during solvent exchange from methanol to methyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of pNIPAM-2, d10 during solvent exchange from methanol to methyl acetate. - Std Dev: Standard deviation of the volume over time of pNIPAM-2, d10 during solvent exchange from methanol to methyl acetate. ### 11. Kinetic_semi-IPN_absolute.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM-PVA semi-IPNs during solvent exchange from 1-butanol to butyl acetate in absolute numbers. The time is for the same for all data series, the single data series (pNIPAM-2 / PVA-0, d5; PVA-1, d5; PVA-2, d5; PVA-3, d5) contain of normalized volume and standard deviation and are separated by an empty column. - **Columns:** - time t: Time of the experiment in h (hours). - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-0 / pNIPAM-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-0 / pNIPAM-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-1, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-1, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-3, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-3, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) ### 12. Kinetic_semi-IPN_dimensionless.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM-PVA semi-IPNs during solvent exchange from butanol to butyl acetate in dimensionless numbers. The single data series (PVA-0 / pNIPAM-2, d5; PVA-1, d5; PVA-2, d5; PVA-3, d5) contain of dimensionless time, normalized volume and standard deviation and are separated by an empty column. - **Columns:** - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of PVA-0 / pNIPAM-2, d5 during solvent exchange from 1-butanol to butyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-0 / pNIPAM-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-0 / pNIPAM-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of PVA-1, d5 during solvent exchange from 1-butanol to butyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-1, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-1, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of PVA-3, d5 during solvent exchange from 1-butanol to butyl acetate. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-3, d5 during solvent exchange from 1-butanol to butyl acetate. - Std Dev: Standard deviation of the volume over time of PVA-3, d5during solvent exchange from 1-butanol to butyl acetate. - Separation column (empty) ### 13. Kinetic_semi-IPN_FTcycles_absolute.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM-PVA semi-IPNs (PVA-2, d5) during solvent exchange from butanol to butyl acetate after freeze–thaw treatment in absolute numbers. - **Columns:** - time t: Time of the experiment in h (hours). - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate after freeze–thaw treatment. - Std Dev: Standard deviation of the volume over time of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate after freeze–thaw treatment. ### 14. Kinetic_semi-IPN_FTcycles_dimensionless.txt (creation date: 01.03.2025, version: 01) - **Description:** Swelling kinetics of pNIPAM-PVA semi-IPNs (PVA-2, d5) during solvent exchange from butanol to butyl acetate in dimensionless numbers after freeze–thaw treatment. - **Columns:** - dimensionless time t/t50 [-]: Dimensionless time calculated by the absolute time t devided by the time t50 at which 50 % shrinkage was obtained of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate after freeze–thaw treatment. - norm. Volume V/V0: The normalized gel volume over time (dimensionless: normalized with volume at 0 s experiment run time) of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate after freeze–thaw treatment. - Std Dev: Standard deviation of the volume over time of PVA-2, d5 during solvent exchange from 1-butanol to butyl acetate after freeze–thaw treatment. ### 15. Volumetric_shrinkage_analysis.py (creation date: 01.03.2025, version: 01) - **Description:** Python script to analyze height and diameter of a cylindrical gel over time from an image sequence. This script calculates the relative volume and diameter over time and saves these calculation in an excel file. --------------------------- METHODOLOGICAL INFORMATION --------------------------- The methodolical of the distinct analysis. 1. Gel Synthesis: For the preparation of hydrogels, 2.175 g of N-isopropylacrylamide (NIPAM) and the appropriate amount of N-N-methylenebisacrylamide (MBA) (as outlined in Formulations.csv) were dissolved in 21 g of deionized water and degassed with nitrogen for 30 minutes. Following this, 2.5 mg each of sodium persulfate and ammonium persulfate were dissolved in 1 mL of deionized water and added to the mixture. The hydrogel monoliths were then cast in syringes (inner diameters: d3 = 1 mm, d5 = 1.3 mm, d10 = 1.65 mm, BRAUN) and sealed with PARAFILM (Sigma Aldrich). In formulations containing polyvinyl alcohol (PVA), the 21 g of deionized water was substituted with a PVA-water mixture, as detailed in Table 1. To aid in the analysis of swelling equilibria and kinetics, 0.01 g of fluorescent pigment (Kremer Pigmente, Fluorescent Pigment Magenta Red) was added to all formulations. For the investigation of the impact of freeze-thaw cycles on swelling behavior, gels underwent a freeze-thaw cycle by freezing at -18 °C for 24 hours, followed by thawing at room temperature for 24 hours. 2. Swelling Equilibria: The hydrogel was sliced into cylindrical segments measuring 1–1.5 cm in height and 1.5 cm in diameter; inhomogeneous end pieces were discarded. For the solvent exchange from water to pure solvents or mixtures, the gel monoliths were immersed in the desired solvent or mixture and shaken, followed by two additional solvent exchange steps with fresh solvents each after 24 h. Subsequently, the lyogel was equilibrated for 48 h at 25 °C (± 0.1 °C) in a water bath (Grant OLS200). The required timeframe was determined based on previous experiments. The solvent exchange to pure esters or 1-butanol required an additional solvent exchange to ethanol due to the limited miscibility of the solvents with water. In solvent mixtures, the hydrogel was first immersed in the solvent in which lower swelling behavior of the gel was obtained. Afterwards, the solvent exchange to the requested solvent mixture was performed. The equilibrated lyogels were dried at 40 °C (± 0.1 °C) under vacuum conditions for 48 h to calculate the mass-specific degree of swelling: Dos = m_gel/m_polymer (mass of equilibrated gel / mass of dried polymer). For the investigation of the swelling behavior during an ongoing esterification reaction, solutions of equimolar mixtures of the reactants were prepared with different concentrations of esters. The concentrations of esters in these mixtures were set to be equivalent to specific conversion rates of the reactions. In this work, solvent-polymer interactions were investigated by preparing solvent mixtures based on conversion rates of the esterification reaction, without carrying out the reaction experimentally. This method enabled the investigation of the influence of solvent-polymer interactions in the occurring solvent mixtures during the reaction, separate from the reaction kinetics. The solvent mixtures were prepared water-free to avoid the formation of a second solvent phase. 3. Swelling Kinetics: The preparation of the monoliths for swelling kinetic analysis followed a procedure similar to that used for swelling equilibrium measurements. The sliced hydrogels were solvent-exchanged with the selected solvents and were then equilibrated. In this study, the hydrogels were exchanged with ethanol, methanol, acetic acid, or 1-butanol. As described for swelling equilibrium analysis, the exchange to 1-butanol was preceded by an initial exchange step with ethanol. The lyogels were held in place with a needle along their height and suspended in a custom-designed wire mesh. Solvent-induced swelling was monitored during the exchange from the pure solvent (alcohol or carboxylic acid) to its corresponding ester derivative. For this, the gels were placed in a 250 mL DURAN beaker containing 200 mL of the ester. Gel dimension changes in response to ester exposure were recorded using a camera (Kurokesu C1 Pro with a 5-50 mm CS lens), capturing an image every minute for 24 to 48 hours, depending on the solvent system. The image sequences were analyzed with a Python script that calculated the gel’s height and diameter by summing pixel counts. Volumetric changes were then determined from this analysis. 4. NMR Relaxometry: All measurements were conducted using a 60 MHz benchtop NMR spectrometer (Spinsolve 60, Magritek, Germany) equipped with a 5 mm diameter NMR tube. Hydrogel samples were characterized using a Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence with an echo time of 300 microseconds, providing insight into the gel’s internal structure and dynamics. The CPMG method enabled the measurement of transverse relaxation times (T2), which reflect molecular mobility and interactions within the gel network. Analysis of T2 relaxation time distributions offered information on the heterogeneous molecular environments present in the gel. In this approach, T2 decay curves were analyzed using mono-exponential fitting. 5. Mechanical Properties: The mechanical properties of the hydrogels were assessed through uniaxial compression tests using a universal testing machine (ZwickRoell GmbH & Co. KG, Universalprüfmaschine Z1474, nominal force: 2.5 kN) under ambient conditions. Before testing, the hydrogels were soaked in deionized (DI) water for at least 48 hours. During the test, the compression stamp (dstamp: 40 mm, unconfined compression test: dstamp > dsample) was initially brought into contact with the gel until an initial force of 0.02 N was registered. The gel was then compressed at a rate of 50 mm/min until either a maximum deformation of 75% or the load cell’s maximum force of 50 N (ZwickRoell GmbH & Co. KG, Xforce HP, nominal force: 50 N) was reached. The force was recorded as a function of the crosshead displacement throughout the test. The elastic modulus (Young’s modulus, EC) was calculated from the elastic region of the compression curve, specifically within the 10-12% deformation range. ----------------- RESEARCH CONTEXT ----------------- This study focuses on modeling and analyzing the swelling behavior of pNIPAM-based lyogels for potential applications in chemical and biochemical reactors. By integrating smart lyogel technology, the research aims to contribute to the development of intelligent reactor systems. This dataset is divided into two parts: the first focuses on characterization techniques, such as NMR relaxometry, swelling degree measurements and mechanical testing; the second examines the swelling kinetics through solvent exchange as a stimulus. ---------------------------------- EXPLANATION OF MEASURED VARIABLES ---------------------------------- Dos: Degree of swelling, describes swelling capacity of gel. T2: transversal relaxation time is measured in with NMR relaxometry. EC: Young's Modulus obtained from uniaxial compression tests describes the elasticity of the network. normalized Volume: The volume changing over time during solvent exchange as trigger (solvent-induced swelling/shrinkage). -------------- ABBREVIATIONS -------------- NIPAM: N-isopropylacrylamide, the monomer of the gel considered in this dataset. pNIPAM: Polymer of N-isopropylacrylamide, forms the gel analyzed in this dataset. MBA: N-N-methylenebisacrylamide, crosslinker added to the polymerisation mixture to form a three-dimensional structure (gel) of the polymer pNIPAM. PVA: Polyvinylalcohol, a polymer included in this dataset in the gel matrix of pNIPAM. NMR: Nuclear magnetic resonance, used to analyze interactions of gel and solvent. d3, d5, d10: Describe varying syringe diameters used in this study to prepare gels with varying diameters. Homopolymer: A polymer composed of one polymerised monomer. Semi-IPN: Semi-Interpenetrating polymer network is a copolymer in which one polymer is chemically crosslinked and the other is a linear polymer physically embedded in the polymer network. pNIPAM-1, pNIPAM-2, pNIPAM-3, pNIPAM-4, pNIPAM-5: Homopolymers of pNIPAM with varying crosslinker concentration from least to highest. PVA-0, PVA-1, PVA-2, PVA-3: Semi-IPN heteropolymers with varying copolymer concentration from least to highest.