Reactir 45m

FTIR analysis was performed in situ, during the epoxidation reaction of the monomers, as well as on the final synthesized monomers; in all instances, the background was subtracted.
For the in situ monitoring, FTIR probe Dicomp AgX, 9.5 mm × 2 m Fiber Silver Halide (Mettler Toledo), was connected to a React IR 45 m (Mettler Toledo, Greifensee, Switzerland) with an inbuilt LN2 NCT detector. The resolution of the FTIR detector was set to 8 cm⁻¹ in the iC IR 4.3 software, and 50 scans were taken for each spectrum. The analysis started when the 2-propanol was poured into the reactor and ended when the reaction was completed.
For the final epoxy monomers, FTIR spectra were recorded on a Spectrum Two FTIR (PerkinElmer, Waltham, MA, USA), equipped with a UATR Two detector (PerkinElmer, Waltham, MA, USA). The resolution was set to 8 cm⁻¹, and 64 scans were collected per FTIR spectrum.

Nuclear magnetic resonance (¹H NMR and ¹³C{¹H} NMR) measurements were recorded on a Bruker AVANCE III-400 Hz instrument in CDCl₃ at room temperature. DOSY measurements were recorded on a Bruker AVANCE III-600 Hz instrument in CDCl₃ at room temperature. SEC measurements were performed at 35 °C with THF as an eluent at a flow rate of 1.0 mL min⁻¹, with a Viscotek GPC_max VE2001 System, and PSS columns (Styragel HR 3, 4, and 5). The molecular weight distributions (M_w/M_n, Ð) were determined by conventional SEC analysis using a calibration curve from polystyrene standards. MALDI-ToF mass measurements were recorded in linear mode, using 2,5-dihydroxybenzoic acid as the matrix in THF (sample/matrix: 1/50). In situ FTIR study was conducted using a ReactIR 45m (Mettler Toledo). The samples were collected every 1 min, and each spectrum was scanned 256 times. DSC measurements were performed at a heating rate of 10 °C min⁻¹ on a Mettler Toledo DSC1/TC100 system under a nitrogen atmosphere. The curve of the second heating scan was adopted to determine the T_g. NMR titration experiments were performed in Young’s NMR tubes using anhydrous toluene-d₈ solvent under argon.