Cross-link in norbornadiene-based polymers from ring-opening metathesis polymerization with pyrrolidine-based Ru complex

Ring-opening metathesis polymerization (ROMP) of norbornadiene (NBD) with [RuCl 2 (PPh 3 ) 2 (pyrrolidine)] as the starting complex was evaluated as a function of reaction time, solvent volume, and atmosphere type at 25 °C. Quantitative yields of polyNBD were obtained either under inert argon atmosp...

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Bibliographic Details
Published in:Polymer bulletin (Berlin, Germany) Germany), 2018-08, Vol.75 (8), p.3705-3721
Main Authors: Fonseca, Larissa R., Silva Sá, José L., Carvalho, Valdemiro P., Lima-Neto, Benedito S.
Format: Article
Language:English
Subjects:
Argon
Characterization and Evaluation of Materials
Chemistry
Chemistry and Materials Science
Chloroform
Complex Fluids and Microfluidics
Copolymerization
Copolymers
Crosslinking
Decomposition reactions
Ligands
Metathesis
NMR
Nuclear magnetic resonance
Organic Chemistry
Original Paper
Photomicrographs
Physical Chemistry
Piperidine
Polymer Sciences
Polymerization
Polymers
Porous materials
Ring opening
Ruthenium compounds
Soft and Granular Matter
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Summary:Ring-opening metathesis polymerization (ROMP) of norbornadiene (NBD) with [RuCl 2 (PPh 3 ) 2 (pyrrolidine)] as the starting complex was evaluated as a function of reaction time, solvent volume, and atmosphere type at 25 °C. Quantitative yields of polyNBD were obtained either under inert argon atmosphere or in air, with 2 mL of CHCl 3 , for 30 min. Copolymerization of NBD with norbornene (NBE) resulted in 100–70% yield under argon, depending on the NBE/NBD molar ratio, and in 70% yield in air, with 2 mL, for 120 min. TGA, DSC, and DMA measurements and swelling tests supported the occurrence of cross-linking in homopolyNBD and in the copolymers isolated from polymers. SEM micrographs showed porous polymeric NBD materials with pores that decreased in size when increasing the amount of NBD in the starting reaction composition. Results from amine parent complexes when the amine was piperidine or perhydroazepine are also discussed, with high cross-linking degree from reaction with the pyrrolidine complex.
ISSN:0170-0839
1436-2449
DOI:10.1007/s00289-017-2236-3