Suda çözünebilen o-karboksimetil kitosan-imine destekli bazı komplekslerin sentezi ve uygulamaları
Yükleniyor...
Dosyalar
Tarih
2015
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Aksaray Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu çalışmada 4 yeni suda çözünebilir O-karboksimetil kitosan Schiff bazı ve onların Cu(II), Pd(II) kompleksleri sentezlendi. Sentezlenen O-karboksimetil kitosan Schiff bazları[OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a], [OCMCS-6a] ve metal komplekslerinin yapıları FTIR, 1H NMR, 13C NMR, 13C CP-MAS NMR, TG/DTG, XRD, SEM-EDAKS, ICP, UV-VIS, elementel analiz, manyetik moment ve molar iletkenlik ölçümleri ile karakterize edilmiştir. [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] ve [OCMCS-6a] bileşiklerinin sübstitüsyon dereceleri (DS) yapılan elementel analiz sonucunda sırası ile 0.36, 0.34, 0.48 ve 0.44 olarak belirlenmiştir. Yapılan çözünürlük testi ile [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] ve [OCMCS-6a] bileşiklerinin oda sıcaklığında saf suda tamamen çözündüğü kaydedilmiştir. Kitosan, O-karboksimetil kitosan Schiff bazları ve komplekslerinin yüzey görüntüleri SEM-EDAKS tekniği ile araştırılmıştır. Sentezlenen bileşiklerin termal davranışları TG/DTG tekniği ile kristaliniteleri ise X-ışını toz kırınım tekniği kullanılarak belirlenmiştir. Elde edilen komplekslerin metal içerikleri ICP-OES cihazı kullanılarak belirlenmiştir. Yapılan analizler sonucunda O-karboksimetil kitosan Schiff bazları ve komplekslerinin kitosana göre termal kararlılıklarında ve kristalinite değerlerinde azalma kaydedilmiştir. Yapılan yüzey incelemesi sonucunda kitosanın yüzey yapısının, elde edilen bileşiklere göre daha düz bir yapıda olduğu da kaydedilmiştir. Ayrıca sentezlenen metal komplekslerinin katalitik aktiviteleri Suzuki çapraz kenetlenme reaksiyonları ile biarillerin sentezinde test edilmiştir. Sentezlenen biarillerin yapıları GC-MS ve 1H NMR teknikleri ile aydınlatılmıştır. Deneyler sonucunda, sentezlenen Pd(II) katalizörleri varlığında, reaksiyonlar yüksek seçicilik göstermiş ve homo kenetlenme yan ürünleri spektrumlarda gözlenmemiştir. Katalizörlerin tekrar kullanılabilirlik testleri sonucunda katalizörlerin birden fazla kez kullanılabildiği belirlenmiştir.
In this study, four new water soluble O-carboxymethyl chitosan Schiff bases and their Cu(II) and Pd(II) complexes were synthesized. These synthesized O-carboxymethyl Schiff bases [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] and [OCMCS-6a] and their metal complexes were characterized by FTIR, 1H NMR, 13C NMR, 13C CP-MAS NMR, TG/DTG, XRD, SEM-EDAX, ICP, UV-VIS, elemental analysis and magnetic moment and molar conductivity measurements. Degree of substitution (DS) of [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] and [OCMCS-6a] compounds were determined by elemental analysis as 0.36, 0.34, 0.48 and 0.44, respectively. It was specified by solubility tests that [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] and [OCMCS-6a] compounds were completely soluble in pure water. Surface images of chitosan, O-carboxymethyl chitosan Schiff bases and their metal complexes were investigated by SEM-EDAX technique. Thermal behaviors and crystallinities of synthesized compounds were determined by TG/DTG and X-ray powder diffraction techniques, respectively. Metal contents of obtained complexes were determined by ICP-OES instrument. As a result of the analyses, it was noted that thermal stabilities and crystallinities of O-carboxymethyl chitosan Schiff bases and their complexes were decreased as compared to chitosan. In consequence of surface screening, it was also noted that surface structure of chitosan was smoother than that of obtained compounds. Furthermore, catalytic activities of synthesized metal complexes were tested by Suzuki cross-coupling reactions in the synthesis of biaryl. Structures of synthesized biaryl were identified by GC-MS and 1H NMR techniques. As a result of the analyses, high selectivity were obtained in the reactions and by-products of homo coupling were not seen in the spectra in the presence of Pd(II) catalysts. It was determined that the catalysts could be used for several times in consequence of reusability tests.
In this study, four new water soluble O-carboxymethyl chitosan Schiff bases and their Cu(II) and Pd(II) complexes were synthesized. These synthesized O-carboxymethyl Schiff bases [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] and [OCMCS-6a] and their metal complexes were characterized by FTIR, 1H NMR, 13C NMR, 13C CP-MAS NMR, TG/DTG, XRD, SEM-EDAX, ICP, UV-VIS, elemental analysis and magnetic moment and molar conductivity measurements. Degree of substitution (DS) of [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] and [OCMCS-6a] compounds were determined by elemental analysis as 0.36, 0.34, 0.48 and 0.44, respectively. It was specified by solubility tests that [OCMCS-3a].2H2O, [OCMCS-4a].2H2O, [OCMCS-5a] and [OCMCS-6a] compounds were completely soluble in pure water. Surface images of chitosan, O-carboxymethyl chitosan Schiff bases and their metal complexes were investigated by SEM-EDAX technique. Thermal behaviors and crystallinities of synthesized compounds were determined by TG/DTG and X-ray powder diffraction techniques, respectively. Metal contents of obtained complexes were determined by ICP-OES instrument. As a result of the analyses, it was noted that thermal stabilities and crystallinities of O-carboxymethyl chitosan Schiff bases and their complexes were decreased as compared to chitosan. In consequence of surface screening, it was also noted that surface structure of chitosan was smoother than that of obtained compounds. Furthermore, catalytic activities of synthesized metal complexes were tested by Suzuki cross-coupling reactions in the synthesis of biaryl. Structures of synthesized biaryl were identified by GC-MS and 1H NMR techniques. As a result of the analyses, high selectivity were obtained in the reactions and by-products of homo coupling were not seen in the spectra in the presence of Pd(II) catalysts. It was determined that the catalysts could be used for several times in consequence of reusability tests.
Açıklama
Anahtar Kelimeler
Suda Çözünür O-karboksimetil Kitosan, Schiff Baz, Suzuki Çapraz Kenetlenme, Biyopolimer, Katalizör, Water Soluble O-carboxymethyl Chitosan, Schiff Base, Suzuki Cross-Coupling, Biopolymers, Catalyts
