Synthesis and Characterization of Clay/Organoclay-Chitosan and Clay/Organoclay-Triethyl Chitosan Nanocomposites

Year 2022, Volume: 25 Issue: 3, 1083 - 1090, 01.10.2022

Nuray Çelebi , Nuray Yıldız

https://doi.org/10.2339/politeknik.818665

Abstract

Synthesis and characterization of composites, namely clay-chitosan, organoclay-chitosan, clay-triethyl chitosan and organoclay-triethyl chitosan, were investigated by using montmorillonite (Mt) as clay mineral. Cetyltrimethylammonium bromide (CTAB, long-chained)), tetraethylammonium bromide (TEAB, short-chained)), and benzyltriethylammonium bromide (BTEAB, ringed)) surfactants were employed to modify the clay surfaces to obtain organoclay. Organoclays were labelled as CTAB-O (clay modified with cetyltrimethylammonium bromide), BTEAB-O (clay modified with benzyltriethylammonium bromide) and TEAB-O (clay modified with tetraethylammonium bromide). The structural and thermal properties were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). XRD and TEM results showed that exfoliated structure was formed for clay-chitosan composites and also organoclay-chitosan composites at lower CTAB-O, TEAB-O and BTEAB-O content. However, by increasing the organoclay content, tactoid morphology was obtained for organoclay-chitosan composites. Moreover, exfoliated structure was observed for clay-triethyl chitosan (TEC) and organoclay-triethyl chitosan (TEC) composites containing 2.5%, 5%, 10% clays and organoclays respectively. Thermal degradation temperature for 10% clay-chitosan and some organoclay-chitosan composites (5% and 10% TEAB-O-chitosan; 10% BTEAB-O-chitosan) increased (about 375 °C) with regard to neat chitosan (350 °C) at 50% weight loss. Furthermore, it was observed that thermal degradation temperature of TEC composites (clay-TEC, organoclay-TEC) increased significantly in reference to composites with chitosan (clay-chitosan, organoclay-chitosan). In particular, maximum degradation temperature (965-968 ˚C) was reached for clay-TEC (2.5% and 10%), CTAB-O-TEC (5%) and BTEAB-O-TEC (5% and 10%) at 50% weight loss.

Keywords

Clay, chitosan, montmorillonite, organoclay, triethyl chitosan

Supporting Institution

Ankara University Scientific Research Fund

Project Number

11B4343002

Thanks

Ankara University Scientific Research Fund

Kil/Organokil-Kitosan ve Kil/Organokil-Trietil Kitosan Nanokompozit Sentezi ve Karakterizasyonu

Abstract

Bu çalışmada montmorillonite (Mt) kili kullanılarak kil-kitosan, organokil-kitosan, kil-trietil kitosan ve organokil-trietil kitosan nanokompozitleri sentezlenmiş ve karakterizasyonları yapılmıştır. Organokil elde etmek için kil yüzeyi uzun zincirli (setil trimetil amonyum bromür (CTAB)), kısa zincirli (tetrametil amonyum bromür (TEAB)), ve halkalı (benzil trietil amonyum bromür (BTEAB)) yüzey aktif maddeleri ile modifiye edilmiştir. Organokiller CTAB-O (setil trimetil amonyum bromür ile modifiye edilmiş kil), BTEAB-O (benzil trietil amonyum bromür ile modifiye edilmiş kil) ve TEAB-O (tetrametil amonyum bromür ile modifiye edilmiş kil) olarak gösterilmiştir. Nanokompozitlerin yapısal ve termal özellikleri X ışını kırınım difraktometresi (XRD), transmisyon elektron mikroskobu (TEM) ve termogravimetrik analiz (TGA) ile incelenmiştir. XRD ve TEM sonuçları, kil-kitosan kompozitleri ve düşük miktarda CTAB-O, TEAB-O and BTEAB-O organokili içeren organokil-kitosan kompozitleri için dağılmış tabakalı (exfoliation) yapı elde edildiğini göstermiştir. Trietil kitosan kompozitlerinde (kil-TEC, organokil-TEC) ise bütün kil ve organo kil miktarları (%2.5, %5, %10) trietil kitosan içinde dağılarak, dağılmış tabakalı (exfoliated) kompozit yapı oluşturmuştur. %50 kütle kaybındaki termal bozunma sıcaklığı tek başına kitosan için 350 °C civarında iken, 10% kil-kitosan and bazı organokil-kitosan kompozitleri (5% and 10% TEAB-O-kitosan; 10% BTEAB-O-kitosan) için 375 °C civarına kadar artmıştır. Ayrıca, trietil kitosan kompozitlerinde (kil-TEC, organokil-TEC) termal bozunma sıcaklığı, kitosan kompozitlerine (kil-kitosan, organokil-kitosan) göre önemli ölçüde artmıştır. En yüksek termal bozunma sıcaklığına (965-968 ˚C), %50 kütle kaybında kil-TEC (%2.5 ve %10), CTAB-O-TEC (%5) ve BTEAB-O-TEC (5% ve %10) kompozitleri için ulaşılmıştır. 

Keywords

Kil, kitosan, montmorillonit, organokil, trietil kitosan

Project Number

11B4343002

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