Kinetics of Resorcinol-Formaldehyde Condensation-Comparison of Common Experimental Techniques

Porous carbons, originated from resorcinol-formaldehyde (RF) gels, show high application potential. However, the kinetics and mechanism of RF condensation are still not well described. In this work, different methods (dynamic light scattering-DLS, Fourier transform infrared spectroscopy-FTIR, low field H-1 nuclear magnetic resonance relaxometry-H-1-NMR, and differential scanning calorimetry-DSC) were used to follow the isothermal RF condensation of mixtures varying in catalyst content (Na2CO3) and reactant concentration. The applicability and results obtained by the methods used differ significantly. The changes in functional groups can be followed by FTIR only at very early stages of the reaction. DLS enables the estimate of the growth of particles in reaction solution, but only before the solution becomes more viscous. Following the relaxation of H-1 nuclei in water during RF condensation brings a different view on the system-this technique follows the properties of the present water that is gradually captured in polymeric gel. From this side, the process behaves similarly to the nucleation reaction, which is in contradiction to the n-order mechanism confirmed by other techniques. The widest range of applicability was found for DSC measurement of the freezing/melting behavior of the reaction mixture, which is possible to use without any limitations until full solidification. Furthermore, this approach enables us to follow the gradual formation and development of the gel through the intermediate undergoing glass transition.

Automated summary

Different methods were used to study the kinetics and mechanism of resorcinol-formaldehyde (RF) condensation, yielding significantly different results and applicability. Fourier transform infrared spectroscopy (FTIR) can only track the changes in functional groups at the early stages of the reaction. Dynamic light scattering (DLS) can estimate the growth of particles in the reaction solution before it becomes more viscous. H-1 nuclear magnetic resonance relaxometry (H-1-NMR) provides insights into the properties of water present in the polymeric gel during RF condensation. Differential scanning calorimetry (DSC) measurement of the freezing/melting behavior of the reaction mixture has the widest range of applicability. These findings can enhance our understanding of the mechanism of RF condensation.