TY - JOUR
T1 - Exploring synthesis techniques for an imidazole-based one-component epoxy latent curing agent
T2 - Chemical capping and mechano-chemical capsuling
AU - Jang, Han Gyeol
AU - Lim, Deok Jae
AU - An, Sohyun
AU - Park, Jong Hyuk
AU - Park, Min
AU - Park, Jinwoo
AU - Park, Hyungbum
AU - Kim, Byeong Su
AU - Lee, Doh C.
AU - Kim, Jaewoo
N1 - Publisher Copyright:
© 2024 The Authors
PY - 2024/11/15
Y1 - 2024/11/15
N2 - The increasing demand for one-component epoxy is driven by its eco-friendliness, convenience, and cost-effectiveness, underscoring the importance of developing latent curing agents that trigger reactions under specific conditions. This study introduces an imidazole-based latent curing agent (ICM-SU) characterized by superior storage stability and low-temperature curing capabilities, achieved through dual protections of chemical capping and mechano-chemical capsuling. The process commences with the synthesis of isophorone diisocyanate capped 2-methylimidazole (ICM), wherein the reactivity of 2-methylimidazole (2MI) is controlled via the inductive effect of isophorone diisocyanate, achieved through chemical capping. Subsequently, ICM-SU is produced by uniformly coating it with silica nanoparticles and a urea shell through mechano-fusion system's dry processing for mechano-chemical capsuling, effectively isolating it from contact with epoxy. The curing mechanism and chemical structure of ICM-SU are identified in four stages: de-capping, de-shelling, formation of epoxy-imidazole adducts, and chain growth. Notably, the melting point of the urea shell (122 °C) closely matches the curing onset temperature, suggesting that the exposure of epoxy to restored 2MI initiates the curing process. As a result, ICM-SU demonstrates significantly enhances storage stability at 20 °C for over 42 days, a stark improvement over 2MI, which solidifies within 8 h. Moreover, specimens cured with ICM-SU exhibits a 32 % increase in tensile strength and a 25 % improvement in Young's modulus compared to those cured with 2MI, attributed to the reinforcing filler effect of silica nanoparticles.
AB - The increasing demand for one-component epoxy is driven by its eco-friendliness, convenience, and cost-effectiveness, underscoring the importance of developing latent curing agents that trigger reactions under specific conditions. This study introduces an imidazole-based latent curing agent (ICM-SU) characterized by superior storage stability and low-temperature curing capabilities, achieved through dual protections of chemical capping and mechano-chemical capsuling. The process commences with the synthesis of isophorone diisocyanate capped 2-methylimidazole (ICM), wherein the reactivity of 2-methylimidazole (2MI) is controlled via the inductive effect of isophorone diisocyanate, achieved through chemical capping. Subsequently, ICM-SU is produced by uniformly coating it with silica nanoparticles and a urea shell through mechano-fusion system's dry processing for mechano-chemical capsuling, effectively isolating it from contact with epoxy. The curing mechanism and chemical structure of ICM-SU are identified in four stages: de-capping, de-shelling, formation of epoxy-imidazole adducts, and chain growth. Notably, the melting point of the urea shell (122 °C) closely matches the curing onset temperature, suggesting that the exposure of epoxy to restored 2MI initiates the curing process. As a result, ICM-SU demonstrates significantly enhances storage stability at 20 °C for over 42 days, a stark improvement over 2MI, which solidifies within 8 h. Moreover, specimens cured with ICM-SU exhibits a 32 % increase in tensile strength and a 25 % improvement in Young's modulus compared to those cured with 2MI, attributed to the reinforcing filler effect of silica nanoparticles.
KW - Chemical capping
KW - Latent curing agent
KW - Mechano-chemical capsuling
KW - One-component epoxy
KW - Storage stability
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U2 - 10.1016/j.cej.2024.157368
DO - 10.1016/j.cej.2024.157368
M3 - Article
AN - SCOPUS:85208052229
SN - 1385-8947
VL - 500
JO - Chemical Engineering Journal
JF - Chemical Engineering Journal
M1 - 157368
ER -