SELÜLOZ ÜZERİNDE AŞILAMA ÇALIŞMALARI

Abstract

Bu çalışmada N-(4-nitrofenil)akrilamit (4NFAA) ve N-siklohekzilakrilamit (SHAA) monomeri sentezlenip IR, 1H ve 13C NMR teknikleriyle karakterize edildi. Ayrıca toz selüloz, bu monomerler ve bazı vinil monomerleriyle serbest radikal polimerizasyonu ve atom transfer radikal polimerizasyonu (ATRP) yöntemiyle aşılandı.Birinci yöntemde, önce toz selülozdaki primer OH grupları metakriloil klorürle estere dönüştürülerek selüloz metakrilat elde edildi. Selüloz metakrilat, sentezlenen monomerlerle ve metil metakrilat (MMA), 4-vinilpiridin (4VP), diallilamin (DA), akrilamit (AM), metakrilamit (MAM), diasetonakrilamit (DAAM) monomerleriyle 2,2'-azobis(isobutironitril) (AIBN) başlatıcısı yanında asetonitril çözücüsünde aşılandı.İkinci yöntemde ise, ATRP ile toz selülozun primer OH grupları önce klorasetilklorürle reaksiyona girerek selülozklorasetat elde edildi. Selülozklorasetat makrobaşlatıcı olarak kullanılıp bakır(I)klorür ve ligand olarak 2,2'-bipiridin varlığında 130oC'de N,N-Dimetilformamit ortamında; sentezlenen monomerler ile ve 4-vinilpiridin (4VP), diallilamin (DA), akrilamit (AM), diasetonakrilamit (DAAM) monomerleriyle aşılandı.Poli[Sel-g-(4NFAA-ko-MMA)] ve Poli[Sel-g-(SHAA-ko-MMA)]'ın CuCl/2,2'-bipiridin varlığında aşı kopolimerleri hazırlandı. Aşı kopolimerizasyonunda monomer reaktivite oranları Kelen-Tudos (KT), Extended Kelen-Tudos (EKT), Finemann-Ross (FR), Inverted Finemann-Ross (IFR), Yezrielev-Brokhina-Roskin (YBR) yöntemiyle hesaplandı.Aşı kopolimerleri; Element Analiz, IR, TGA ve AAS yöntemleri kullanılarak karakterize edildi.Ayrıca selülozdan elde edilen aşı kopolimerlerin su ve metal iyonu tutma özellikleri ve elektriksel iletkenlik özellikleri belirlendi ve sonuçlar tartışıldı.Anahtar Kelimeler: Selüloz, N-(4-nitrofenil)akrilamit, N-siklohekzilakrilamit, Aşı Kopolimer, Atom Transfer Radikal Polimerizasyonu

In this study, N-(4-nitrophenyl)acrylamide (4NPA) and N-cyclohexylacrylamide (NCHA) monomers were synthesized and characterization by IR, 1H and 13C NMR techniques. In addition, powder cellulose, and some of these monomers were grafted by using two different methods, with some vinyl monomers, through free radical graft copolymerization and atom transfer radical polymerization (ATRP).In the first of these methods, primary OH groups in powder cellulose were first transformed to ester groups with methacryloylchloride and cellulose methacrylate was obtained. This cellulose methacrylate was grafted with the synthesized monomer and 4-vinylpyridine (4VP), acrylamide (AM), methacrylamide (MAM), diacetone acrylamide (DAAM), methylmethacrylate (MMA), diallylamine (DA) monomers, in presence of 2,2'-azobis(isobutyronitrile) AIBN in acetonitrile as solvent. In the second method, with the atom transfer radical graft copolymerization, primary OH groups of powder cellulose was first reacted with chloroacetylchloride and cellulose chloroacetate was obtained. Used cellulose chloroacetate as macro initiator was grafted with synthesized the monomer and AM, DAAM and DA monomers in the presence copper (I) chloride and as ligands 2,2'-bipyridine at 130°C in the N,N-Dimethylformamide. Some graft copolymers of Poly[Sel-g-(4NFAA-co-MMA)] and Poly[Sel-g-(SHAA-co-MMA)] were prepared in the presence of CuCI/2,2'-bipyridine. The monomer reactivity ratios of graft copolymerization were calculated by using Kelen-Tudos (KT), Finemann-Ross (FR), and Inverted Finemann-Ross (IFR), Yezrielev-Brokhina-Roskin (YBR), and Extended Kelen-Tudos (EKT) methods.The graft copolymers were characterized by elemental analysis, IR, TGA and AAS techniques.In addition, water and metal ion uptake properties and electrical conductivity of the graft obtained from cellulose were determined and the results were discussed.Keywords: Cellulose, N-(4-nitrophenyl)acrylamide, N-cyclohexylacrylamide, Graft Copolymer, Atom Transfer Radical Polymerization