Infrared thermography analysis of the thermally latent polymerization of 3‐ethyl‐3‐phenoxymethyloxetane

Abstract

Infrared thermography was employed to analyze multiple batches of the thermally latent polymerization of 3‐ethyl‐3‐phenoxymethyloxetane at once. The temperature changes in the polymerization depended on the polymerization rates. That is, a fast polymerization was exothermic, increasing the temporal temperature of the polymerization by approximately 130 °C within a few minutes. Infrared thermography, which can analyze multiple samples instantaneously, proved effective as a screening method for thermally latent curing systems. Exothermicity in the crosslinking polymerization of 1,4‐bis(3‐ethyloxetanylmethoxy)benzene was also analyzed by infrared thermography. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 5519–5524, 2006

Infrared Thermography as a High-Throughput Tool in Catalysis Research

“…36 With the help of IRT, phase transitions could be studied during the cationic ring-opening polymerization of multiple batches of 3-ethyl-3-phenoxymethyloxetane. 37 Even enantioselective catalysis has been investigated using IRT. Reetz 38 In 2002, the parallel screening for the enantioselective substrate specificity of candida antarctica lipase in the liquid phase was reported.…”

Novel analytical method for the crosslinking process: Infrared thermographic analysis of the thermally latent cationic polymerization of a spiroorthoester and a bifunctional oxetane for the construction of a low‐shrinkage curing system

“…This result agrees with the homopolymerization of EPOX using these initiators, in which the polymerization initiated with BPMS consumed EPOX faster than that initiated with BTHT. 8 In the copolymerization using BPMS, EPOX was consumed faster than PSOE [ Fig. 1(a)].…”

“…[1][2][3][4] The very low shrinkage or no shrinkage in double ring-opening polymerizations has been explained by the release of the compact structures to freely mobile linear chains. Typical double ring-opening monomers are spiroorthoester (SOE) derivatives, [5][6][7][8] having wide variations in their structures because of their simple preparation method through the addition of lactones and epoxides. Whereas single ring-opening polymerizations of SOE derivatives shrink the volume significantly, the double ring-opening polymerizations shrink the volume negligibly.…”

“…From this point of view, we have preliminarily investigated (co)polymerizations of SOE and oxetane monomers with thermally latent sulfonium salts. 8,9 The SOE monomer was proved to reduce the shrinkage during polymerization. Furthermore, direct temperature monitoring by infrared (IR) thermography revealed that the SOE monomer reduced the exothermicity, probably because of the mild propagation through a stable carbenium cation.…”

“…9 Encouraged by these results, we have preliminarily demonstrated a crosslinking polymerization of a bifunctional oxetane that also shows exothermicity. 8 Accordingly, we extended the IR thermographic analysis to a crosslinking copolymerization system comprising the SOE monomer and a bifunctional oxetane. We also investigated the effect of the initiator on the copolymerization and the thermal behaviors and estimated the origin of the exothermicity by computational calculation.…”