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Synthesis of novel metal-containing epoxy polymers and their structural characterization by means of FT-IR and coupled TG/MS measurements

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Abstract

Novel copper containing epoxy polymers have been synthesized using copper(II) formamidine complex [Cu(ampf)Cl2], ampf = N,N′-bis(4-acetyl-5-methylpyrazole-3-yl)formamidine, as curing agent for diglycidyl ether of bisphenol A-based epoxy resins (Araldite and its oligomer consisting of 3–4 monomer units). The curing reaction was performed at room temperature without catalyst. In order to prove the polymerization reaction, differential scanning calorimetry (DSC) was applied. Highly exothermic peaks around 150 °C refer to the polymerization, and according to DSC results, the epoxy resins above 200 °C were almost completely converted to the corresponding metal-containing polymer. The proposed structure of the hybrid polymers was confirmed by FT-IR analysis. Gel permeation chromatography analysis shows that the average molar masses of the polymers are in the range from 3,000 to 50,000 g mol−1. The low conductivities of the hybrid materials in tetrahydrofuran confirm the non-ionic structure of the new polymers in solution. The thermal stability and the decomposition mechanism of the components of the reaction mixture and the new polymers were studied by coupled TG/DTA-MS measurements. The thermal data were analysed also with the aim to obtain additional information about the composition of the synthesized materials.

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Acknowledgements

This paper was supported by the Ministry of Education, Science and Technological Development, Republic of Serbia; contract Grant numbers: III 45022 and ON 172014. B. Barta Holló acknowledges a Domus Hungarica Fellowship. I. M. Szilágyi acknowledges a János Bolyai Research Fellowship of the Hungarian Academy of Sciences, and an OTKA-PD-109129 Grant.

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Authors and Affiliations

  1. Faculty of Technology, University of Novi Sad, Bulevar cara Lazara 1, 21000, Novi Sad, Serbia

    Ivan S. Ristić & Jaroslava Budinski-Simendić

  2. Faculty of Science, University of Novi Sad, Novi Sad, Serbia

    Berta Barta Holló & Katalin Mészáros Szécsényi

  3. Faculty of Technology, University of Nis, Leskovac, Serbia

    Suzana Cakić

  4. MTA-BME Technical Analytical Chemistry Research Group, Szent Gellért tér 4., Budapest, 1111, Hungary

    Imre Miklós Szilágyi

  5. Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szent Gellért tér 4., Budapest, 1111, Hungary

    Imre Miklós Szilágyi & György Pokol

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  1. Ivan S. Ristić
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  2. Berta Barta Holló
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  3. Jaroslava Budinski-Simendić
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  6. Imre Miklós Szilágyi
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  7. György Pokol
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Correspondence to Ivan S. Ristić.

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Ristić, I.S., Barta Holló, B., Budinski-Simendić, J. et al. Synthesis of novel metal-containing epoxy polymers and their structural characterization by means of FT-IR and coupled TG/MS measurements. J Therm Anal Calorim 119, 1011–1021 (2015). https://doi.org/10.1007/s10973-014-4242-0

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  • DOI: https://doi.org/10.1007/s10973-014-4242-0

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