Infrared spectroscopy as an effective tool in ring-opening metathesis polymerization: monitoring the polymerization kinetics of norbornene with amine-based Ru catalysts in real time

Tomazett, Vinicius K.; Santos, Willy G.; Neto, Benedito dos Santos Lima

doi:10.1007/s11144-017-1147-5

Cited by 15 publications

(9 citation statements)

References 23 publications

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“…As it can be seen in Figure 11, the absorption band at 1,650 cm -1 for the metathesis products is significantly bigger than in the reference material. This band is characteristic of the alkenes produced during polymerization (Shchapin et al, 2007;Tomazett et al, 2017;Zedler et al, 2014;Sengupta et al, 2007;Guadagno et al, 2014) and it is assigned to the stretching vibration of the double bond which is formed during ROMP polymerization (Schaubroeck et al, 2006;Shchapin et al, 2007).…”

Section: Ilss Behaviormentioning

confidence: 98%

Mechanical behavior of aeronautical composites containing self-healing microcapsules

Polydoropoulou

Katsiropoulos

Loukopoulos

et al. 2018

IJSI

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Purpose Over the last decades, self-healing materials based on polymers are attracting increasing interest due to their potential for detecting and “autonomically” healing damage. The use of embedded self-healing microcapsules represents one of the most popular self-healing concepts. Yet, extensive investigations are still needed to convince on the efficiency of the above concept. The paper aims to discuss these issues. Design/methodology/approach In the present work, the effect of embedded self-healing microcapsules on the ILSS behavior of carbon fiber reinforced composite materials has been studied. Moreover, the self-healing efficiency has been assessed. The results of the mechanical tests were discussed supported by scanning electron microscope (SEM) as well as by Attenuated Total Reflection–Fourier-transform infrared spectroscopy (ATR–FTIR) analyses. Findings The results indicate a general trend of a degraded mechanical behavior of the enhanced materials, as the microcapsules exhibit a non-uniform dispersion and form agglomerations which act as internal defects. A remarkable value of the self-healing efficiency has been found for materials with limited damage, e.g. matrix micro-cracks. However, for significant damage, in terms of large matrix cracks and delaminations as well as fiber breakages, the self-healing efficiency is limited. Originality/value The results obtained by SEM analysis as well as by ATR–FTIR spectroscopy constitute a strong indication that the self-healing mechanism has been activated. However, further investigation should be conducted in order to provide definite evidence.

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Section: Ilss Behaviormentioning

confidence: 98%

Mechanical behavior of aeronautical composites containing self-healing microcapsules

Polydoropoulou

Katsiropoulos

Loukopoulos

et al. 2018

IJSI

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“…However, the phosphine–amine complexes produced higher yields. It was demonstrated by calculation and kinetic studies via FT‐IR that the phosphine–amine complexes react first with EDA, losing the phosphine ligands, followed by the reaction with monomer . As these phosphine–amine complexes are 16‐electron species, they undergo efficient substitution processes.…”

Section: Resultsmentioning

confidence: 99%

Dual catalytic performance of arene‐ruthenium amine complexes for norbornene ring‐opening metathesis and methyl methacrylate atom‐transfer radical polymerizations

Cruz

Silva

Oliveira

et al. 2020

Applied Organom Chemis

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Arene ruthenium(II) complexes bearing the cyclic amines RuCl2(η6‐p‐cymene)(pyrrolidine)] (1), [RuCl2(η6‐p‐cymene)(piperidine)] (2), and [RuCl2(η6‐p‐cymene)(peridroazepine)] (3) were successfully synthesized. Complexes 1–3 were fully characterized by means of Fourier transform infrared, UV–visible, and NMR spectroscopy, elemental analysis, cyclic voltammetry, computational methods, and one of the complexes was further studied by single crystal X‐ray crystallography. These compounds were evaluated as catalytic precursors for ring‐opening metathesis polymerization (ROMP) of norbornene (NBE) and atom‐transfer radical polymerization (ATRP) of methyl methacrylate (MMA). NBE polymerization via ROMP was evaluated using complexes 1–3 as precatalysts in the presence of ethyl diazoacetate (EDA) under different [NBE]/[EDA]/[Ru] ratios, temperatures (25 and 50°C), and reaction times (5–60 min). The highest yields of polyNBE were obtained with [NBE]/[EDA]/[Ru] = 5000/28/1 for 60 min at 50°C. MMA polymerization via ATRP was conducted using 1–3 as catalysts in the presence of ethyl‐α‐bromoisobutyrate (EBiB) as initiator. The catalytic tests were evaluated as a function of the reaction time using the initial molar ratio of [MMA]/[EBiB]/[Ru] = 1000/2/1 at 95°C. The increase in molecular weight as function of time indicates that complexes 1–3 were able to mediate the MMA polymerization with an acceptable rate and some level of control. Differences in the rate of polymerization were observed in the order 3 > 2 > 1 for the ROMP and ATRP.

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“…O objetivo é estudar processos de polimerização que envolva compostos com propriedades luminescentes. Inglez [38] e Tomazett [60] , alunos do grupo, sintetizaram e estudaram metalopolímeros com propriedades luminescentes, a partir da síntese de ligantes-monômeros.…”

Section: Proposta De Trabalhounclassified

“…Recentemente obteve-se o ligante-monômero etilenodiamina-(bisnorborneno) (en(NBE2)), ilustrado na Figura 6 [60] . Assim, planejou-se reagir este ligante-monômero com [RuCl2(L)2], e em seguida o monômero seria copolimerizado com monômeros de NBE.…”

Section: Proposta De Trabalhounclassified

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Desenvolvimento de complexos de rutênio com diiminas funcionalizadas com norborneno e suas polimerizações via metátese

Alves¹

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Infrared spectroscopy as an effective tool in ring-opening metathesis polymerization: monitoring the polymerization kinetics of norbornene with amine-based Ru catalysts in real time

Cited by 15 publications

References 23 publications

Mechanical behavior of aeronautical composites containing self-healing microcapsules

Mechanical behavior of aeronautical composites containing self-healing microcapsules

Dual catalytic performance of arene‐ruthenium amine complexes for norbornene ring‐opening metathesis and methyl methacrylate atom‐transfer radical polymerizations

Desenvolvimento de complexos de rutênio com diiminas funcionalizadas com norborneno e suas polimerizações via metátese

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