Synthesis and Characterization of Resol Type Phenolic Resins

Year 2020, Volume: 20 Issue: 3, 407 - 417, 30.06.2020

Ferda Mindivan , Ahmet Gürses

https://doi.org/10.35414/akufemubid.649241

Abstract

The different pre-polymerization temperatures and various formaldehyde/phenol (F:P) ratios have a critical importance in the synthesis of resol phenolic resin. Understanding the reaction parameters in polymerization reactions is a prerequisite for the production of phenolic resin-based composite materials. X-Ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), Differential scanning calorimetry (DSC) and microhardness analysis were performed to observe the effect of different pre-polymerization temperatures and various F: P ratios. The results of XRD and FTIR analysis provided an understanding of the structural conformation of synthesized resins. It was also found by the DSC and microhardness analysis that the tendency of crystallization increased for the synthesized resin (PFR250) when the pre-polymerization temperature was 50 °C and the F:P ratio was 1,3, especially in parallel with increasing ether bridges.

Keywords

Resol phenolic resin, Pre-polymerization temperature, Formaldehyde / phenol ratio, Thermal analysis, Micro hardness, Structural conformation

Resol Tipi Fenolik Reçinelerin Sentezi ve Karakterizasyonu

Abstract

Farklı ön polimerizasyon sıcaklıkları ve çeşitli formaldehit / fenol (F: P) oranları, resol fenolik reçinenin sentezinde kritik bir öneme sahiptir. Polimerizasyon reaksiyonlarında reaksiyon parametrelerinin anlaşılması, fenolik reçine bazlı kompozit malzemelerin üretimi için ön şarttır. Farklı ön polimerizasyon sıcaklıkları ve çeşitli F:P oranlarının etkisini gözlemlemek için, X-Işını difraksiyonu (XRD), Fourier dönüşümlü infrared spektroskopisi (FTIR), Diferansiyel taramalı kalorimetri (DSC) ve mikro sertlik analizleri yapılmıştır. XRD ve FTIR analizlerinin sonuçları, sentezlenmiş reçinelerin yapısal konformasyonunun anlaşılmasını sağlamıştır. DSC ve mikro sertlik analiz sonuçlarıyla, ön-polimerizasyon sıcaklığı 50 °C ve F:P oranı 1,3 iken sentezlenen reçinenin (PFR250) artan eter köprülerine paralel olarak kristalleşme eğiliminin arttığı tespit edilmiştir.

Keywords

Resol fenolik reçine, Ön polimerizasyon sıcaklığı, Formaldehit/fenol oranı, Termal analiz, Mikro sertlik, Yapısal konformasyon

References

• Referans 1 Aierbe, A., Echeverrı, J.M., Martin, M.D., Etxeberria, A.M., Mondragon I., 2000. Influence of the initial formaldehyde to phenol molar ratio (F/P) on the formation of a phenolic resol resin catalyzed with amine. Polymer, 41, 6797– 6802.
• Referans 2 Cai, X., Riedl, B., Wan, H., Zhang, S.Y., Wang X. M., 2010. A study on the curing and viscoelastic characteristics of melamine–urea–formaldehyde resin in the presence of aluminium silicate nanoclays. Composites: Part A, 41, 604–611.
• Referans 3 Cardona, F., Aravinthan, T., Moscou, C., 2010. Modified PF Resins for Composite Structures with Improved Mechanical Properties. Polymers & Polymer Composites, 18, 6, 297-306.
• Referans 4 Choi, M. H., Chung, I. J., Lee, J. D., 2000. Morphology and curing behaviors of phenolic resin-layered silicate nanocomposites prepared by melt ıntercalation. Chemistry of Materials, 12, 2977-2983.
• Referans 5 Choi, M. H., Byun, H. Y., Chung I. J., 2002. The effect of chain length of flexible diacid on morphology and mechanical property of modified phenolic resin. Polymer, 43, 4437-4444.
• Referans 6 Hirano, K., Asami, M., 2012. Phenolic resins—100 years of progress and their future. Reactive & Functional Polymers, 73, 2, 256-269.
• Referans 7 Huang, J., Xu, M., Ge, Q., Lin, M., Lin, Q., Chen, Y., Chu, J., Dai, L., Zou, Y., 2005. Controlled Synthesis of High-Ortho-Substitution Phenol–Formaldehyde Resins. Journal of Applied Polymer Science, 97, 652–658.
• Referans 8 Hong, Z., Guangsu, H., Pin, G., Chengqun, L., 2007. Preparation of porous/hollow particles of phenolic resin. Polymers for Advanced Technologies, 18, 582–585.
• Referans 9 Manfredi, L. B., De La Osa, O., Fernandez, N., Vazquez, A., 1999. Structure-properties relationship for resols with different formaldehyde/phenol molar ratio. Polymer, 40, 3867-3875.
• Referans 10 Mindivan, F., 2013. fenolik reçine ve modifiye edilmiş kil/reçine kompozitlerinin hazırlanması ve yapısal, termal ve mekanik özelliklerinin incelenmesi. Doktora Tezi, Atatürk Üniversitesi Fen Bilimleri Enstitüsü, Erzurum, 178.
• Referans 11 Pethrick, R. A., 2004. Encyclopedia of Polymer Science and Technology, Characterization of Polymer, Vol.9, John Wiley and Sons, Inc., 170-171.
• Referans 12 Pilato, L., 2010. Phenolic Resins: A Century of Progress, Springer, 43.
• Referans 13 Polijansek, I. Krajnc M., 2005. Characterization of Phenol Formaldehyde Prepolymer Resins by In FT-IR Spectroscopy. Acta Chimica Slovenica, 52, 238-244.
• Referans 14 Saçak, M., 2008. Polimer Kimyası, Gazi Kitapevi, Ankara, 98.
• Referans 15 Tasan, C., Kaynak, C. 2004. Production of Phenolic Resin/Layered Silicate Nanocomposites. International Symposium of Research Students on Material Science and Engineering, India.
• Referans 16 Wang, J., Laborie, M.P.G., Wolcott, M. P., 2005. Comparison of model-free kinetic methods for modeling the cure kinetics of commercial phenol–formaldehyde resins. Thermochimica Acta, 439, 68–73.
• Referans 17 Zhang, X., Shen, L., Xia, X., Wang, H., Du, Q., 2008. Study on the interface of phenolic resin/expanded graphite composites prepared via in situ polymerization. Materials Chemistry and Physics, 111, 368–374.
• Referans 18 Zhou, G., Movva, S., Lee, L. J., 2008. Nanoclay and Long-Fiber-Reinforced Composites Based on Epoxy and Phenolic Resins. Journal of Applied Polymer Science, 108, 3720–3726.