Thermosensitive poly N-isopropylacrylamide based cryogel: A SAXS study

Abstract

The purpose of this study is to observe the structural changes of the thermosensitive poly N-isopropylacrylamide- N-methacryloyl-L-histidine poly NIPA-MAH monolithic cryogel with changing temperature around lower critical solution temperature LCST of NIPA by Small Angle X-Ray Scattering SAXS . Poly NIPA-MAH cryogel was prepared by free radical cryocopolymerization of NIPA with MAH as functional comonomer and N,N- methylene-bisacrylamide MBAAm as crosslinker directly in a plastic syringe. Polymerization initiated by N,N,N,N- tetramethylene diamine TEMED and ammonium persulfate APS pair at subzero temperature in an ice bath. LCST of poly NIPA-MAH cryogel was found to be 34oC. Poly NIPA-MAH cryogel with 60–100 μm in pore diameter have a specific surface area of 42.6 m2/g polymer. This porous cryogel form provides fast temperature response comparing to conventional gels. The surface morphology and bulk structure of poly NIPA-MAH cryogel revealed with scanning electron microscopy SEM . SAXS allowed the determination of nanoalteration of poly NIPA-MAH cryogel such as pore volume, wall thickness and pore shape with changing temperature. Scattering data were analysed both native form and in water at temperature range of 300C-400C. At two different temperatures 34oC and 35oC a detailed investigation on shape of pores and pore size; which indicating a recordable change, were also carried out.

Keywords

• N-isopropylacrylamide NIPA,thermosensitive,cryogels,Small Angle X-Ray Scattering SAXS

Isıya duyarlı poli N-izopropilakrilamit temelli kriyojellerin SAXS çalışması

Abstract

B u çalışmanın amacı, NIPA’in düşük kritik çözelti sıcaklığı LCST civarındaki sıcaklığın değiştirilmesiyle ısıya duyarlı poli N-izopropilakrilamid-metakriloil-L-histidin , poli NIPA-MAH monolitik kriyojellerinin nano yapısındaki değişimleri küçük açı x-ışını saçılması SAXS yöntemi ile incelemektir. Poli NIPA-MAH kriyojeller, NIPA, MAH fonksiyonel monomeri ve N,N-metilen-bisakrilamit MBAAm çapraz bağlayıcısı kullanılarak plastik şırınga içerisinde serbest radikal kriyopolimerizasyonu ile hazırlanmıştır. Polimerizasyon buz banyosunda sıfır derecenin altında N, N, N, N-tetrametilen diamin TEMED ve amonyum persulfat APS çifti kullanılarak başlatılmıştır. Poli NIPA-MAH kriyojelinin LCST değeri 34 oC olarak bulunmuştur. Poli NIPA-MAH kriyojelleri 60-100 µm gözenek çapına ve 42.6 m2/g polimer spesifik yüzey alanına sahiptir. Sentezlenen gözenekli kriyojeller geleneksel jellerle karşılaştırıldığında sıcaklık değişimine hızlı tepki vermektedir. Poli NIPA-MAH kriyojelinin yığın yapısı ve yüzey morfolojisi taramalı elektron mikroskobu SEM kullanılarak belirlenmiştir. SAXS, poli NIPA-MAH kriyojelinin sıcaklık değişimiyle gözenek hacmi, duvar kalınlığı ve gözenek şekli gibi nano boyuttaki değişimlerin belirlenmesine imkan vermektedir. 30-40oC sıcaklık aralığında doğal form ve su içerisinde saçılma verileri incelenmiştir. Iki farklı sıcaklıkta 34oC ve 35oC gözenek boyutu ve şekli üzerinde kaydedilebilir bir değişikliği gösteren ayrıntılı bir inceleme de gerçekleştirilmiştir

Keywords

• N-izopropilakrilamid NIPA , ısıl duyarlı, kriyojel, Küçük Açı X-ışını Saçılması SAXS

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