0575488 - ÚMCH 2024 RIV US eng J - Journal Article
Beneš, Hynek - Konefal, Magdalena - Bujok, Sonia - Mrózek, Ondřej - Pavlova, Ewa - Smržová, Darina - Ecorchard, Petra
Intercalation of ionic liquids into LDH structures for microwave-accelerated polymerizations.
Inorganic Chemistry. Roč. 62, č. 36 (2023), s. 14694-14703. ISSN 0020-1669. E-ISSN 1520-510X
R&D Projects: GA ČR(CZ) GA22-05244S; GA MŠMT(CZ) LM2023066
Institutional support: RVO:61389013 ; RVO:61388980
Keywords : ionic liquid * intercalation * layered double hydroxide
OECD category: Polymer science; Inorganic and nuclear chemistry (UACH-T)
Impact factor: 4.3, year: 2023 ; AIS: 0.692, rok: 2023
Method of publishing: Open access
Result website:
https://pubs.acs.org/doi/10.1021/acs.inorgchem.3c02021DOI: https://doi.org/10.1021/acs.inorgchem.3c02021

Microwave-accelerated ring-opening polymerization (ROP) of cyclic esters catalyzed by ionic liquid (IL) anions, intercalated into layered double hydroxides (LDHs), has been recently described as a fast and environmentally friendly synthetic way to prepare biodegradable polyester/LDH nanocomposites. However, to observe this synergistic catalytic effect between microwaves and IL anions and to achieve a homogeneous structure of the final polymer nanocomposite, the IL anions must be efficiently intercalated inside the LDH structure. Herein, we investigate the effects of various metal compositions of M2+/Al3+ LDHs (M = Mg, Co, and Ca) and different LDH synthetic routes (one-step direct coprecipitation, two-step coprecipitation/anion exchange, and two-step urea/anion exchange) on the intercalation efficiency of trihexyltetradecylphosphonium bis(2,4,4-trimethylpentyl)phosphinate IL. The most effective IL anion intercalation was observed for Ca2+/Al3+ LDH prepared using the two-step method consisting of coprecipitation and subsequent anion exchange. After optimization, this synthetic pathway led to the production of LDHs with intercalated IL anions and a reduced amount of intercalated water (<0.6 wt %). The catalytic ability of thus optimized LDH particles was demonstrated on the microwave-assisted ROP of ε-caprolactone, showing rapid progress of polymerization. Within minutes, the polycaprolactones with an average molecular mass in the range of 20 000–50 000 g/mol containing fully delaminated and exfoliated LDH nanoparticles were obtained.
Permanent Link: https://hdl.handle.net/11104/0345368