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우레탄 결합을 갖는 폴리에틸렌옥사이드와 폴리스티렌 IPN 의 열분해 반응속도 및 열안정성에 관한 연구
김용주,심인철,이치규,성용길 ( Yong Joo Kim,In Chul Sim,Chi Giu Lee,Yong Kiel Sung ) 한국공업화학회 1995 공업화학 Vol.6 No.1
우레탄 본드를 갖는 폴리에틸렌옥사이드와 폴리스티렌의 IPN을 동시중합법에 의하여 합성하고 적외선 분광기, 시차주사열량계 및 전자현미경으로 특성을 측정하였다. 전자현미경사진에서 폴리에틸렌옥사이드의 함량이 6owt%일때 상전이 현상이 일어나며 유리전이온도는 각각의 온도에서 안쪽으로 이동하였다. 열중량분석기를 사용하여 열안정성 및 열분해반응속도 파라메터를 조사하였다. 가교된 폴리에틸렌옥사이드 및 IPN에서의 열분해는 2단계 분해곡선을 나타내는데 첫단계는 우레탄본드의 분해에 기인하며 두번째 단계의 분해거동은 폴리스티렌의 양이 증가할수록 증가하는 열안정성과 관련된다고 생각된다. 열분해의 활성화 에너지는 각 고분자의 상전이 현상에 영향을 받으며 열분해 반응속도 파라메터를 각각 Ozawa, Friedman 및 Kissinger이론에 의하여 구하였다. The IPN of poly(ethylene oxide) with urethane bond and polystyrene were synthesized by a simultaneous method. The IPN were characterized by FT-IR spectrophotometer, differential scanning calorimetry and electron micrography. Electron micrographs showed the separated phases which underwent with the phase inversion at about 60wt% composition of PEO. The IPN showed inwardly shifted two Tg corresponding to the Tg of each networks. The thermal stability of the IPN were also measured using thermogravimetry. The crosslinked PEO and IPN decomposed in two stages; the first stage was caused by the creavage of urethane linkage, and the second stage by thermal stabilities of the IPN increasing with the weight fractions of crosslinked PS. The activation energies for the thermal decomposition of the IPN were affected by phase behaviours of each polymer networks. By using Ozawa, Friedman, and Kissinger, the kinetic parameters of thermal decomposition were evaluated.
양말단에 서로 다른 관능기를 갖는 PEO를 합성하기 위한 Sila-protected Amino Functionality Initiator의 합성
김용주,한애란,성용길 동국대학교 자연과학연구원 1994 자연과학연구 논문집 Vol.14 No.-
A new initiator, potassium N-[2-(2,2,5,5-tetramethyl-1-aza-2,5-disila cylopentyl) ethyl] methyl amide, was synthesized with sila-protected amino functionality for well-defined heterobifunctional PEO. The synthesized initiator was identified by IR, ¹H-NMR, GC-Mass and GC.
Thermal Properties of Aminated Polyetherurethanes
Kim,Yong-Joo,Sung,Yong-Kiel 동국대학교 자연과학연구소 1990 자연과학연구 논문집 Vol.10 No.-
생체 적용 고분자로 사용되어진 Polyetherurethane을 메틸아민, 에틸아민 및 브틸아민으로 처리한 후 FT-IR로 확인하였다. 아민 처리된 Polyetherurethane의 열적성질 및 열분해 속도를 시차주사 열량계와 열무게 분석법으로 수행하였으며 열분해 속도로부터 활성화 에너지를 구하였다. 아민이 처리된 Ployetherurethane이 분해되는 동안에 나온 아민은 FT-IR과 가스크로마토그라피로 확인하였다. Polyetherurethanes are materials that have been used in biomedical applications. The materials were treated with methylamine, ethylamine and buylamine. The aminated polyetherurethnaes were identified by FT-IR. The thermal properties and the kinetic study of thermal decomposition of amine treated materials have been carried out by means of differential scanning calorimetry and thermogravimetry. In the kinetic study of the thermal decomposition, the activation energies were determined. The evolved gas during the decomposition was analyzed by gas chromatography and FT-IP spectrophotometer.
Multiblock Copolymers Heparin-PEO-PDMS-PEO-Heparin. : Ⅰ. Synthesis and Characterization
Sung, Yong Kiel,Kim, Yong Joo 東國大學校 1991 東國論叢 Vol.30 No.-
Amphiphilic block copolymer containing poly(dimethyl siloxane)〔PDMS〕 , poly(ethylene oxide)〔PEO〕, and heparin were prepared by a series of coupling reactions using functionalized prepolymers, diisocyanates and derivatized heparin. PDMS(PEO-NH_2)_2 block copolymers were synthesized by adding diisocyanated PDMS in toluene. Heparin was introduced to PDMS(PEO-NH_2)_2 block copolymers by sodium cyanoborohydride. The block copolymers and the heparinized block copolymers were identified by ^1H-NMR spectrometer and FT-IR spectrophotometer. The compositions of synthesized block copolymers were measured by end group analysis, sulfur elemental analysis, and integration of NMR signal. The water swelling degrees of the block copolymers and the heparinized block copolymers were also determined. The swelling degrees of the block copolymers were increased with increasing the molecular weight of PEO in water. Utilizing contact angle and electron microscopy, the surface of the block copolymers were characterized. Wilhelmy plate contact angle measurements demonstrated the effect of hydrophilic PEO and heparin on the hysteresis of the block copolymers and the heparinized block copolymers. In addition, the decreased hysteresis on the heparinized block copolymers suggests the surface reorientation of the heparin segment into the aqueous phase.
Characterization of Multiblock Copolymer Containing PDMS, PEO and Heparin
Sung, Yong Kiel,Kim, Yong Joo 東國大學校 1992 東國論叢 Vol.31 No.-
Poly(dimethyl siloxane)(PDMS), poly(ethylene oxide)(PEO) 및 헤파린을 포함하는 다블록 공중합체들은 diisocyanate와 헤파린 유도체들과 같은 기능기를 갖는 물질을 사용하여 합성하였다. PEO-PDMS-PEO의 공중합체는 toluene용매에서 isocyanate기가 도입된 PDMS와 diamino기가 도입된 PEO를 반응시켜 합성하였으며, 여기에 sodium cyanoborohydride를 이용하여 헤파린일 포함된 ABCBA형태의 다블록 공중합체를 합성하였다. 합성된 다블록 공중합체들을 핵자기공명법과 적외선분광기를 이용하여 확인하였으며 블록공붕합체내에의 조성은 단말기 분석법, 황 원소분석법 및 핵자기공명 피이크의 면적비에 의하여 구하였다. 또한 벌크상태에서 시차주사열량계와 X선 회절기를 사용하여 다블록 공중합체의 물리적성질을 측정하였는데, 다블록 고웅합체내의 PEO의 분자량이 증가함에 따라 결정도는 증가하였으며, Tm, △Hm 및 △Sm의 값도 변하였다. ABCBA type amphiphilic block copolymere were synthesize and characterized to examine the bulk properties. The block copolymers and the heparinized block copolymers were identified by 1^H-NMR spectrometer, FT-IR spectrophotometer, end group analysis, sulfur elemental analysis, and integration of NMR signal. The block copolymers and the heparinized block copolymers were characterized in bulk by differential scanning calorimetry and X-ray diffractometer. The crystallinity. Tm, △Hm, and △Sm of PEO in block copolymers and the heparinized block copolymers varied according to the molecular weight of PEO.