Dergiler / Pamukkale Üniversitesi Mühendislik Bilimleri Dergisi / 2026 / Cilt: 32 Sayı: 5

"Aşılama" yöntemi kullanılarak RAFT kütle polimerizasyonuyla yıldız-fırça kopolimerinin sentezi ve karakterizasyonu

Synthesis and characterization of star-brush copolymer by RAFT bulk polymerization using "grafting from" method

Melahat Göktaş(VAN YUZUNCU YIL UNIVERSITY)
Ümran Aslan(VAN YUZUNCU YIL UNIVERSITY)
Cengiz Aykaç(VAN YUZUNCU YIL UNIVERSITY)
Sayfa
1114–1120
Yayın Tarihi
2026-09-13
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⚡ TL;DR(1 Cümlede Hızlı Çıkarım)

Ürünler, proton nükleer manyetik rezonans spektroskopisi, infrared spektroskopisi, jel geçirgenlik kromatografisi, termo gravimetrik analiz ve diferansiyel taramalı kalorimetri gibi cihazlar kullanılarak karakterize edildi.

📌 3 Maddede Bu Makale

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Amaç & Hipotez:Bu çalışmada, poli(ɛ-kaprolakton) (PCL) bazlı çok fonksiyonlu makro-RAFT ajanı varlığında, "aşılama" yöntemi kullanılarak tersinir katılmalı/ayrışmalı zincir transfer (RAFT) kütle polimerizasyonu ile yıldız-fırça kopolimeri hazırlandı.
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Temel Bulgular & Veri:Bu polimerizasyon, polimerizasyon süresi değiştirilerek 80 oC’de gerçekleştirildi ve hem polimerizasyon süresinin hem de polimerizasyon sıcaklığının molekül ağırlığı, monomer dönüşümü ve dispersite üzerindeki etkileri incelendi.
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Sonuç & Katkı:Ürünler, proton nükleer manyetik rezonans spektroskopisi, infrared spektroskopisi, jel geçirgenlik kromatografisi, termo gravimetrik analiz ve diferansiyel taramalı kalorimetri gibi cihazlar kullanılarak karakterize edildi.
🔬Tür:Araştırma Makalesi
📍Kapsam:Genişletilmiş Akademik Örneklem
⚙️Değişkenler:Çok fonksiyonlu RAFT ajanı · Brom/klor uçlu poli(ԑ-kaprolakton) · "Aşılama" yöntemi

Özet

Bu çalışmada, poli(ɛ-kaprolakton) (PCL) bazlı çok fonksiyonlu makro-RAFT ajanı varlığında, "aşılama" yöntemi kullanılarak tersinir katılmalı/ayrışmalı zincir transfer (RAFT) kütle polimerizasyonu ile yıldız-fırça kopolimeri hazırlandı. Bu amaç için, brom/klor uçlu poli(ɛ-kaprolakton) (PCL-Br/Cl) ve potasyum etil ksantat tuzunun reaksiyonundan PCL bazlı çok fonksiyonlu makro-RAFT ajanı sentezlendi. Daha sonra, PCL bazlı çok fonksiyonlu makro-RAFT ajanı kullanılarak RAFT kütle polimerizasyonu ile poli(ɛ-kaprolakton-g-stiren) [(PCL-g-PSt)] yıldız-fırça kopolimeri sentezlendi. Bu polimerizasyon, polimerizasyon süresi değiştirilerek 80 oC’de gerçekleştirildi ve hem polimerizasyon süresinin hem de polimerizasyon sıcaklığının molekül ağırlığı, monomer dönüşümü ve dispersite üzerindeki etkileri incelendi. Bu polimerizasyon sonucunda, düşük dispersiteye sahip, çok yüksek molekül ağırlıklı kopolimer elde edildi. Ürünler, proton nükleer manyetik rezonans spektroskopisi, infrared spektroskopisi, jel geçirgenlik kromatografisi, termo gravimetrik analiz ve diferansiyel taramalı kalorimetri gibi cihazlar kullanılarak karakterize edildi.

Abstract

In this study, the star-brush copolymer was prepared by reversible addition/fragmentation chain transfer (RAFT) bulk polymerization in the presence of multifunctional macro-RAFT agent based on poly(ɛ-caprolactone) (PCL) using the "grafting from" method. For this purpose, multifunctional macro-RAFT agent based on PCL was synthesized from the reaction of the brominated/chlorine-terminated poly(ɛ-caprolactone) (PCL-Br/Cl) and ethylxanthic acid potassium salt. Then, the poly(ԑ-caprolactone-g-styrene) [(PCL-g-PSt)] star-brush copolymer was synthesized via RAFT bulk polymerization using multifunctional macro-RAFT agent based on PCL. This polymerization was carried out at 80 oC by changing the polymerization time and, both the polymerization time and the polymerization temperature were investigated on the molecular weight, monomer conversion and dispersity. As a result of this polymerization, very high molecular weight copolymer with low dispersity was obtained. The products were characterized by using multi-instruments such as proton nuclear magnetic resonance spectroscopy, Infrared spectroscopy, gel permeation chromatography, thermo gravimetric analysis and differential scanning calorimetry.

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Bu Makaleye Atıf Yap

Göktaş, M., Aslan, Ü., Aykaç, C. (2026). "Aşılama" yöntemi kullanılarak RAFT kütle polimerizasyonuyla yıldız-fırça kopolimerinin sentezi ve karakterizasyonu. Pamukkale Üniversitesi Mühendislik Bilimleri Dergisi, Cilt: 32 Sayı: 5, 1114–1120. https://doi.org/10.65206/pajes.30277

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Kaynakça (32)

  1. Shanmugam S, Cuthbert J, Kowalewski T, Boyer C, Matyjaszewski K. “Catalyst-free selective photoactivation of RAFT polymerization: a facile route for preparation of comblike and bottlebrush polymers”. Macromolecules, 51(19), 7776-7784, 2018.
  2. Tanaka J, Hakkinen S, Boeck PT, Cong Y, Perrier S, Sheiko SS, You W. “Orthogonal cationic and radical RAFT polymerizations to prepare bottlebrush polymers”. Angewandte Chemie International Edition, 59(18), 7203-7208, 2020.
  3. Altay E, Rzayev J. “Synthesis of star-brush polymer architectures from end-reactive molecular bottlebrushes”. Polymer, 98, 487-494, 2016.
  4. Klemm B, Picchioni F, Mastrigt F van, Raffa P. “ Starlike Branched Polyacrylamides by RAFT Polymerization Part I: Synthesis and Characterization”. ACS Omega, 3, 18762-18770, 2018.
  5. Göktaş M, Aykaç C, Hazer B and A Richard D. “Synthesis of Poly(styrene)-g-Poly(oleic acid) graft copolymers via reversible addition/fragmentation transfer (RAFT) polymerization using a poly oleic acid Macro-RAFT agent”. Journal of polymers and Environment, 32, 2629-2643, 2024.
  6. Kaneyoshi H, Matyjaszewski K. “Synthesis of a linear polyethylene macromonomer and preparation of polystyrene-graft-polyethylene copolymers via grafting-through atom transfer radical polymerization”. Journal of Applied Polymer Science, 105, 3-13, 2006.
  7. Göktaş M, Aslan Ü. “Synthesis and characterization of graft copolymer hydrogel by “grafting from” atom transfer radical polymerization using brominated macro monomeric initiator and investigation of hydrogel properties”. Polymer Bulletin, 81, 11127-11143, 2024.
  8. Göktaş M, Aykaç C. “Synthesis of block-brush terpolymer via one-step RAFT-ROP and grafting to "click" chemistry methods”. Polymer Bulletin, 82, 3991-4004, 2025.
  9. Concilio M, Nguyen N, Hall CLS, Huband S, Becer CR. “Synthesis of oxazoline/methacrylate-based graft-copolymers via grafting-through method and evaluation of their self-assembly in water and dodecane”. Macromolecules, 56(19), 7961-7972, 2023.
  10. Huang J, Xiao W, Yang Z, Yan X, Jiang L, Liao S. “Grafting-from” synthesis of polyvinyl ether bottlebrush polymers via a combination of cationic polymerization and ATRP”. Polymer Chemistry, 16(23), 2778-2783, 2025.
  11. Bai J, Wang X, Fu P, Cui Z, Zhao Q, Pang X, Liu M. “From the unimolecuclar template of water-soluble multiarm star brush copolymers to one-dimensional colloidal nanocrystal clusters: facile synthesis via a combination of magnetic assembly with photoinduced cross-linking”.The Journal of Physical Chemistry C, 120, 705-714, 2016.
  12. Chiefari J, Chong Y K, Ercole F, Krstina J, Jeffery J, Le TPT, Mayadunne RTA, Meijs GF, Moad CL, Moad G, Rizzardo E, Thang SH. “Living free-radical polymerization by reversible addition-fragmentation chain transfer. The RAFT process”. Macromolecules, 31(16), 5559-5562, 1998.
  13. Li P, Li Z, Huang J. “Water-Soluble star brush copolymer with four arms composed of Poly(ethylene Oxide) as Backbone and Poly(acrylic Acid) as Side Chains”. Macromolecules, 40, 491-498, 2007.
  14. Thankappan H, Semsarilar M, Li S, Chang Y, Bouyer D, Quemener D. “Synthesis of block copolymer brush by RAFT and click chemistry and its self-assembly as a thin film”. Molecules, 25, 4774, 2020.
  15. Nikzaban S, Abdollahi A. “Self-Assembly of star-shaped block copolymer to halochromic janus nanoparticles for in situ visualization of latent fingerprints and colorimetric/fluorimetric pH sensing”. ACS Applied Materials & Interfaces, 17, 57453-57474, 2025.
  16. Hazer B, Subramaniyan S, Zhang B. “RAFT polymerization of the novel methacrylated methyl salicylate. Block copolymerization with poly (3-hydroxy butyrate)”. Chemistry Select, 6,12255-12265, 2021.
  17. Chohan P, György C, Mykhaylyk OO, Prentice GM, Filip SV, Payne MJ, Manna G, Armes SP. “RAFT dispersion polymerization of 2‐hydroxyethyl methacrylate in non-polar media”. Macromolecules, 57, 11738-11752, 2024.
  18. Docherty PJ, Derry MJ. and Armes SP. “RAFT dispersion polymerization of glycidyl methacrylate for the synthesis of epoxy-functional block copolymer nanoparticles in mineral oil” Polymer Chemistry, 10(5), 603-611, 2019.
  19. Hazer B, Keleş Ö. “Comparison of the Macro Chain transfer agent and the macro azo ınitiator based on the Poly(3-hydroxy Butyrate) in the Polymerization Kinetics of Methyl Methacrylate”. ACS Omega, 10(7), 6814-6826, 2025.
  20. Barner-Kowollik C, Davis T.P, Stenzel MH. “Synthesis of star polymers using RAFT polymerization: What is Possible?”. Australian Journal of Chemistry, 59, 719-727, 2006.
  21. Hu W, Safari M, Zhou Y, Pérez-Camargo RA, Liu G, Müller AJ, Wang D. “Comonomer ınclusion in single crystals of ısodimorphic random copolymers of butylene succinate and ε‐caprolactone”. Macromolecules, 56(13), 5058-5067, 2023.
  22. Cheechana N, Akkravijitkul N, Khamto N, Rithchumpon P, Junpirom T, Limwanich W, Punyodom W, Tantirungrotechai Y, Nimmanpipug P, Meepowpan P. “Room-Temperature lewis acid organocatalysts for bulk ring-opening polymerization of bis-lithium n-heterocyclic carbenes complexes activated on 𝝐-caprolactone: synthetic, experimental, and density functional theory of mechanistic studies”. Macromolecular Chemistry and Physics, 2300129, 1-8, 2023.
  23. Tuzen M, Elik A, Hazer B, Şimşek S, Altunay N. “Poly(styrene)-co-2-vinylpyridine copolymer as a novel solid-phase adsorbent for determination of manganese and zinc in foods and vegetables by FAAS”. Food Chemistry, 333, 127504, 2020.
  24. Rajendran PB, Raghavachari D. “Synthesis of graft copolymers onto styrenic polymer backbone via “Grafting From’’ RAFT Process”. Journal of Polymer Science. Part A: Polymer Chemistry, 50, 4772-4782, 2012.
  25. Khani MM, Abbas ZM, Benicewicz BC. “Well-Defined polyisoprene-grafted silica nanoparticles via the RAFT process”. Journal of Polymer Science Part A: Polymer Chemistry, 55, 1493-1501, 2017.
  26. Bolton J, Tandem JR. “RAFT-ATRP Synthesis of Polystyrene-Poly(Methyl Methacrylate) bottlebrush block copolymers and their self-assembly into cylindrical nanostructures”. ACS Macro Letter, 1, 15-18, 2012.
  27. Göktaş M. “Synthesis and characterization of various block copolymers using PMMA-Br macroinitiator”. Chemical Papers 73, 2329-2339, 2019.
  28. Öztürk T, Göktaş M, Hazer B. “One-Step synthesis of triarm block copolymers via simultaneous reversible-addition fragmentation chain transfer and ring-opening polymerization”. Journal of Applied Polymer Science, 117, 1638-1645, 2010.
  29. Qin A, Sun Z, Zhang Y, Wang Y. “Electro-Optical properties of polymer dispersed liquid crystal prepared by successively controlled living radical polymerization”. Polymer Composites, 33, 178-184, 2012.
  30. Kilic MS, Korkut S, Hazer B. “Novel enzymatic rhodium modified poly(styrene-g-oleic amide) film electrode for hydrogen peroxide detection”. Electroanalysis, 29, 2377-2384, 2017.
  31. Guan T, Qian S, Guo Y, Cheng F, Zhang W, Chen J. “Star brush block copolymer electrolytes with high ambient-temperature ıonic conductivity for quasi-solid-state lithium batteries”. ACS Materials Letters, 1, 606-612, 2019.
  32. Öztürk T, Çakmak I. “Synthesis of poly(ethylene glycol-b-styrene) block copolymers by reverse atom transfer radical polymerization”. Journal of Polymer Research, 15, 241-247, 2008.