Potassium Carbonate as Catalyst for Transesterification of Cellulose in TBAF/DMSO Solvent System Instead of KH2PO4 and Na2HPO4 Salt Mixture

Year 2023, Volume: 23 Issue: 2, 86 - 98, 01.10.2023

Emir Erişir , Esat Gümüşkaya

https://doi.org/10.17475/kastorman.1367919

Abstract

Aim of study: This study's goal is to evaluate potassium carbonate as a catalyst for the transesterification of cellulose dissolved in TBAF/DMSO and to identify the optimal reaction conditions.
Material and methods: First, a solvent system consisting of 33 g TBAF and 165 g DMSO was prepared for 10 g dissolving pulp in this solvent system for one hour, then the cellulose solution was generated. The catalysts were added to the solution. At reaction temperature, vinyl acetate was added to the solution and the 70-h transesterification process was started. The product was precipitated in ethyl alcohol and washed with water on a sieve, and then dried at room temperature. The effects of changes in catalyst ratio and temperature on bond acetyl groups were investigated by heterogeneous saponification method, FTIR, XRD, DSC, viscosity and solubility test.
Main results: The samples' DS values ranged from 1.39 to 2.37 and using phosphate salt mixture catalyst and increasing the ratio of catalyst increased the DS. FTIR and XRD data revealed that acetylation was effective. DSC thermograms showed a minor endotherm at 283.3-291.2°C, and it was identified as the melting point. With potassium carbonate, the viscosity and the solubility of the products increased.
Highlights: Cellulose in TBAF/DMSO could be acetylated using potassium carbonate as the catalyst. Potassium carbonate's catalyst activity was weak on DS.

Keywords

Cellulose, TBAF/DMSO, Potassium Carbonate, Transesterification, FTIR, XRD, DSC

Selülozun TBAF/DMSO Çözücü Sisteminde KH2PO4 ve Na2HPO4 Tuz Karışımı Yerine Transesterifikasyonunda Katalizör Olarak Potasyum Karbonat

Abstract

Çalışmanın amacı: Bu çalışmanın amacı TBAF/DMSO içinde çözünmüş selülozun transesterifikasyonunda potasyum karbonatı katalizör olarak değerlendirmek, uygun reaksiyon koşullarını belirlemektir.
Materyal ve yöntem: 33 gram TBAF ve 165 gram sıvı DMSO’dan oluşan çözücü içerisinde mekanik olarak öğütülmüş yüksek saflık oranına sahip 10 gram çözünür hamur oda sıcaklığında 1 saat süreyle bekletilmiş ve selüloz çözeltisi üretilmiştir. Çözünen selüloza katalizör ilave edilmiş ve yönteme uygunsa ortam sıcaklığı arttırılmıştır. Reaksiyon sıcaklığına ulaşıldığında vinil asetat sisteme ilave edilmiş ve 70 saatlik transesterifikasyon reaksiyonu başlatılmıştır. Sürenin sonunda ürün sırasıyla etil alkol içerisinde çöktürülmüş ve su ile elek üzerinde yıkandıktan sonra, oda sıcaklığında kurutulmuştur. Katalizör oranı ve sıcaklığın değişiminin bağ asetil grupları üzerindeki etkileri heterojen sabunlaştırma yöntemi, FTIR, XRD, DSC, viskozite ve çözünürlük testi ile araştırılmıştır.
Sonuçlar: Örneklerin DS değerlerinin 1.39 ile 2.37 arasında değişmiş ve fosfat tuzu karışımı katalizörünün kullanılması ve katalizör oranının arttırılması ile DS artmıştır. FTIR ve XRD verileri asetilasyonun başarılı bir şekilde gerçekleştiğini göstermiştir. DSC termogramlarında 283.3-291.2°C'de küçük bir endoterm mevcuttur ve bu erime noktası olarak tanımlanmıştır. Potasyum karbonat ile, örneklerin viskoziteleri ve ürün çözünürlüğünün arttığı tespit edilmiştir.
Önemli vurgular: TBAF/DMSO içinde selülozun katalizör olarak potasyum karbonat ile asetilasyonu gerçekleştirilebilir. Potasyum karbonatın katalizör etkisinin DS üzerinde daha az etkili olduğu görülmüştür.

Keywords

Selüloz, TBAF/DMSO, Potasyum Karbonat, Transesterifikasyon, FTIR, XRD, DSC

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