Polimerik Linoleik Asit İçeren Graft Kopolimerlerin Atom Transfer Radikal Polimerizasyonu ve Kondenzasyon Reaksiyonu ile Sentezi ve Karakterizasyonu

Year 2021, Volume: 9 Issue: 5, 1860 - 1874, 31.10.2021

Sema Allı

https://doi.org/10.29130/dubited.927837

Abstract

Bu çalışmada, NPLina1-g-PCL-g-PSt üç bloklu graft kopolimerler Atom Transfer Radikal Polimerizasyonu (ATRP) ve kondenzasyon reaksiyonu kullanılarak bir basamakta tek kap (one-pot) yöntemiyle sentezlendi. Polimerik linoleik asit dietanolaminle reaksiyona sokularak hidroksillenmiş linoleik asit polimerleri (NPLina1, NPLina2 ve NPLina3) elde edilmiştir. ε-Kaprolakton'nun (ε-CL) kalay (II) 2-etilheksanoat katalizörü varlığında 110 °C'de halka açılma polimerizasyonuyla poli(ε-kaprolakton) (PCL) sentezlenip, ardından 2-bromopropiyonil bromür ile esterleşmesi sonucu bromlanmış poli(ε-kaprolakton) (PCL-Br) makro başlatıcısı hazırlandı. Tek kap yöntemiyle, stiren (St) monomerinin PCL-Br makro başlatıcısıyla CuCl/PMDETA sistemi varlığında [I]:[CuCl]:[PMDETA] = 1:1:3 mol oranları kullanılarak, 110 °C’de toluen içinde ATRP'si ile NPLina1’nın kondenzasyon reaksiyonu aynı anda gerçekleştirildi. Böylece, kontrollü molekül ağırlıklarına ve orta derecede dar polidispersitelere sahip graft kopolimerler elde edildi. Tek basamakta gerçekleşen polimerizasyon üzerine monomer konsantrasyonu, başlatıcı konsantrasyonu ve polimerizasyon süresi gibi temel parametreler incelendi. Elde edilen polimerler, proton nükleer manyetik rezonans (1H NMR), fourier dönüşümlü kızılötesi spektroskopisi (FTIR) ve jel geçirgenlik kromatografısi (GPC) teknikleri kullanılarak karakterize edildi.

Keywords

Linoleik asit, Otooksidasyon, Hidroksilasyon, Kondenzasyon reaksiyonu, Atom transfer radikal polimerizasyonu

Supporting Institution

Düzce Üniversitesi

Project Number

2019.07.06.1021

Thanks

Bu çalışma Düzce Üniversitesi Bilimsel Araştırma Projeleri tarafından desteklenmiştir.

Synthesis and Characterization of Graft Copolymers Containing Polymeric Linoleic Acid by Atom Transfer Radical Polymerization and Condensation Reaction

Abstract

In this study, NPLina1-g-PCL-g-PSt tri-block graft copolymers were synthesized by one-pot method using Atom Transfer Radical Polymerization (ATRP) and condensation reaction in one step. Hydroxylated polymers of linoleic acid (NPLina1, NPLina2 ve NPLina3) were obtained by reacting polymeric linoleic acid synthesized with amine diethanolamine. Bromine ended poly(ε-caprolactone) (PCL-Br) as macroinitiator was prepared via ROP of ε-caprolactone (ε-CL) in the existence of tin(II) 2 ethylhexanoate at 110 °C followed by esterification with 2-bromopropionyl bromide. With the one-pot method, the simultaneously ATRP of Styrene (St) and as condensation polymerization of NPLina1 was performed out by using the PCL-Br macroinitiator and CuCl/PMDETA system in the existence in toluene at 110 °C with [I]:[CuCl]:[PMDETA]=1:1:3. Thus, the graft copolymers with controlled molecular weights and moderately narrow polydispersities were obtained. The impacts of the main parameters were investigated on one-step polymerization such as monomer concentration, initiator concentration, and polymerization time. Polymers obtained were characterized using proton nuclear magnetic resonance (1H NMR), fourier-transform infrared spectroscopy (FTIR), and gel permeation chromatography, (GPC) techniques.

Keywords

Linoleic acid, Autooxidation, Hydroxylation, Atom transfer radical polymerization, Condensation reaction

Project Number

2019.07.06.1021

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