Kaliksarenler kullanılarak sulu çözeltilerden bazı organik kirleticilerin uzaklaştırılması
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Dosyalar
Tarih
2014-03-26
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Selçuk Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu çalışma, polimerik yapıdaki bir kaliks[4]aren türevinin hazırlanarak önemli organik kirleticilerden olan p-nitro fenolün (PNF) sulu ortamdan adsorpsiyon çalışmalarında adsorban olarak kullanılmasını içermektedir. Bu amaçla adsorpsiyon çalışmalarında kullanmak için öncelikle monomerik kaliks[4]aren türevleri ile polimerik adsorban hazırlandı ve hazırlanan bileşiklerin yapıları, FTIR, 1H NMR, elementel analiz, TGA, XRD ve SEM gibi yapı analiz teknikleri kullanılarak aydınlatıldı. Sentez çalışmalarında, literatürlerde belirtilen metoda göre 5,11,17,23-tetra-ter-bütil-25,26,27,28-tetrahidroksikaliks[4]aren (1) sentezlendikten sonra, bu bileşik asetonitril içerisinde metil iyodür ile potasyum karbonat varlığında etkileştirildiğinde dimetoksi türevi (2) elde edildi. Dimetoksi türevi ise kuru aseton içerisinde metil bromoasetat ile etkileştirilerek metoksi-ester türevi (3) elde edildi. Bu bileşik, LiAlH4 ile dietileter içerisinde indirgendikten sonra elde edilen metoksi-alkol türevi (4) de p-toluensülfonilklorürle piridinli ortamda -4oC da muamele edilerek metoksi-tosilat türevi (5) elde edildi. Son olarak metoksi-tosilat türevi kuru toluen içerisinde aminopropil slikajel (APS) ile etkileştirilerek polimerik yapıdaki kalik[4]aren türevi (6) elde edildi. Elde edilen kaliksaren temelli APS bağlı polimerle adsorpsiyon çalışmaları yapılarak ilgili önemli parameteler (pH, etkileşim süresi, PNF konsantrasyonu, adsorban miktarı ve sıcaklık) incelendi. Yapılan çalışmalar sonucunda pH 6, temas süresi 1 saat, PNF konsantrasyonu 5.0x10-5 M, adsorban miktarı 0,025 g ve sıcaklık 25oC parametleri en uygun adsorpsiyon şartları olarak belirlendi. Ayrıca farklı konsantrasyon çalışmaları sonucunda Langmuir ve Freundlich izotermleri çizilerek adsorpsiyon mekanizması aydınlatılmaya çalışıldı.
This study polymeric structure calix [4] arene derivatives prepared toxic selected p-nitro phenol (PNF) from the aqueous medium includes the use as a sorbent in the adsorption studies. For this purpose the adsorption studies for use in the calix [4] arene based polymeric sorbent was prepared and this compound prepared structure, FTIR and 1H NMR, elemental analysis, TGA, XRD and SEM such as structure analysis techniques were elucidated. In the synthesis part of this study, it was firstly performed the synthesis of 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrahydrxycalix[4]arene (1) and then it was reacted with methyl iodide in dry acetonitrile in the presence of potassium carbonate to give its dimethoxy derivative (2). After that methoxy-ester derivative (3) was obtained by reacting of 2 with methylbromoacetate in dry acetone. After last compound (3) was reduced to alcohol derivative (4) by LiAlH4 in diethyl ether, 4 was converted into tosylate derivative (5) by reacting of 4 with p-toluenesulfonyl chloride in pyridine at -4oC. Finally methoxy-tosylate derivative in dry toluene aminopropil slikajel (APS) (6) was obtained. Calixarene-based polymer 6 was used in the adsorption studies of PNP and it was examined some parameters such as pH, contact time, initial concentration, and temperature of the sorbent dosage. The results showed that pH 6, contact time 1 hour, the concentration of 5.0x10-5 M PNP, 0.025 g of sorbent dosage and 25oC of temperature was found as optimum parameters of PNP adsorption with 6. Also Langmuir and Freundlich isotherms were drawn to clarify the adsorption mechanism.
This study polymeric structure calix [4] arene derivatives prepared toxic selected p-nitro phenol (PNF) from the aqueous medium includes the use as a sorbent in the adsorption studies. For this purpose the adsorption studies for use in the calix [4] arene based polymeric sorbent was prepared and this compound prepared structure, FTIR and 1H NMR, elemental analysis, TGA, XRD and SEM such as structure analysis techniques were elucidated. In the synthesis part of this study, it was firstly performed the synthesis of 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrahydrxycalix[4]arene (1) and then it was reacted with methyl iodide in dry acetonitrile in the presence of potassium carbonate to give its dimethoxy derivative (2). After that methoxy-ester derivative (3) was obtained by reacting of 2 with methylbromoacetate in dry acetone. After last compound (3) was reduced to alcohol derivative (4) by LiAlH4 in diethyl ether, 4 was converted into tosylate derivative (5) by reacting of 4 with p-toluenesulfonyl chloride in pyridine at -4oC. Finally methoxy-tosylate derivative in dry toluene aminopropil slikajel (APS) (6) was obtained. Calixarene-based polymer 6 was used in the adsorption studies of PNP and it was examined some parameters such as pH, contact time, initial concentration, and temperature of the sorbent dosage. The results showed that pH 6, contact time 1 hour, the concentration of 5.0x10-5 M PNP, 0.025 g of sorbent dosage and 25oC of temperature was found as optimum parameters of PNP adsorption with 6. Also Langmuir and Freundlich isotherms were drawn to clarify the adsorption mechanism.
Açıklama
Anahtar Kelimeler
Aminopropil silika jel (APS), Aminopropyl silica gel (APS), Adsorpsiyon, Adsorption, P-nitro fenol (PNF), P-nitro phenol (PNP), Polimerik kaliksaren, Polymeric calixarene
Kaynak
WoS Q Değeri
Scopus Q Değeri
Cilt
Sayı
Künye
Aladağlı, V. (2014). Kaliksarenler kullanılarak sulu çözeltilerden bazı organik kirleticilerin uzaklaştırılması. Selçuk Üniversitesi, Yayımlanmış yüksek lisans tezi, Konya.
