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생체적합성과 생분해성을 갖는 폴리에스테르 중합체의 합성과 특성에 관한 연구(II) : Poly(1, 4-butanediol succinate)의 결정화 및 생분해성
송대경,성정석 대한의용생체공학회 1995 의공학회지 Vol.16 No.1
Biodegradable poly (I ,4-butanediol succinate) (PBS) was synthesized from 1,4-butanediol and succinic anhydride. The glass transition temperature of poly (I, 4-butanediol succinate) was revealed at $73^{\circ}C$. The crystallization and cold crystallization of the polymers were investigated as a function of holding time in melt state, cooling rate. reheating, and molecular weight. Chain scission and/or cmsslinking did not occur in the melt state at var.ious holding times. Slower scanning rate can allow more times for nucleation, rearrangement, and packing of the polymer chain, so the onset temperature of crystallization from the melt was increased. PBS crystallized from the melt was found to have spherulitic structure. The degradation behavior of PBS was studied under basic conditions and with microorganisms using the modified ASTM method. In the basic solution. PBS lost up to 85% of its mass within two days. Based upon visual observation, the crystalline structure of films composed of larger molecular weight polymers retained their crystallinity longer than similar structures in low molecular weight samples.
생분해성 Poly(1,4-butanediol succinate)의 합성과 물성에 관한 연구
송대경,오명식,성용길 동국대학교 대학원 1993 大學院硏究論集-東國大學校 大學院 Vol.23 No.-
A new biodegradable poly(1,4-butanediol succinate) as synthesized from 1,4-butanediol and succinic anhydride by using Krebs cycle acid derivatives. The synthesized poly(1,4-butanediol succinate) was identified by 1^H-NMR spectrometer and FT-IR spectrophotometer. The molecular eights and molecular weight distributions were measured by gel permeation chromatography. The glass transition temperature, crystallization temperature and melting temperature of the polymers ere characterized by differential scanning calorimetry. The crystallization behavior of the polymers ere also studied by DSC analysis in nonisothermal system.
정광보,송대경 한서대학교 산학협력연구원 부설 환경연구소 1999 환경연구소 논문집 Vol.2 No.-
Krebs 회로산인 L-mialic acid를 1,4-butanediol과 기능기의 비를 달리하면서 새로운 가교공중합체 Poly(1,4-butanediol L-malate)(XL-PBM10, XL-PBM12 및 XL-PBM14)를 합성하였다. 합성된 가교공중합체의 유리전이온도는 XL-PMB10은 3.3℃, XL-PBM12는 3.9℃, XL-PBM14는 4.9℃에서 나타났으며, 열분해 온도는 각각 246℃, 280℃, 320℃ 이었다. 곰팡이 Aspergillus niger와 박테리아 pseudomonas fluorescens를 이용하여 가교공중합체를 생분해시킨 결과 전자의 경우에는 7주후에 85%가, 후자의 경우에는 75%가 분해되었다. There kinds of new crosslinked poly(1,4-butanediol L-malate)such as XL-PBM10, XL-PBM12, and XL-PBM14 were synthesized from L-malic and 1,4-butanediol by varying functional group ratios. The glass transition temperatures of the copolymers appeared at 3.3℃ in XL-PBM10, at 3.9℃ in XL-PBM12, and at 4.9℃ in XL-PBM14. Thermal decomposition of copolymer started at 246℃ in XL-PBM10, at 280℃ in XL-PBM12, and at 320℃ in XL-PBM14. The biodegradable behaviors of the cross-linked copolymer were studied using microorganisms such as fungus and bacterium. After seven weeks, the degree of biodegradation was 85% in Aspergillus niger and 75% in Pseudomonas fluorescens.
Poly(glycolic acid)의 결정화에 미치는 온도와 냉각속도의 영향
송대경,오명식,성용길 동국대학교 자연과학연구소 1993 자연과학연구 논문집 Vol.13 No.-
1.4-Butanediol과 stannous octate를 개시제 및 촉매로 사용하여 poly(glycolic acid)를 합성하고 적외선 흡수분광기를 이용하여 확인하였다. 시차주사열량계를 이용하여 25℃에서의 결정화 시간변화, 냉각속도와 결정화 온도등이 PAG의 결정화에 미치는 영향을 조사해본 결과 25℃에서의 결정화 시간이 증감함에 따라 생성되는 결정의 양은 증가하였으며 냉각 속도가 느려질수록 경정화가 더 높은 온도에서 나타나는 경향을 보였다. 25℃까지 냉각시킨 시료를 다시 가열하였을 때 결정생성에 의해 나타나는 발열 피이크가 냉각속도 20℃/min까지만 나타나고 5℃/min이하의 속도로 냉각시켰던 시료에서는 냉결정화만 일어남을 관찰할 수 있었다. 또한 용융된 시료를 등온 결정화 시킨 후 재가열 해본 결과 120℃~140℃에서 등온 결정화 시킨 경우가 100℃나 160℃에서 등온 결정화 시킨 경우보다 결정이 더 잘 생성되었다. Poy(glycolic acid) was synthesized using glycolide with 1, 4-butanediol and stannous octate as initiator and catalyst. The synthesized polymer was identifide by FT-IR spectrophotometer. The crystallization and cold crystallization of polymer were investigated on the effect of crystallization temperature, time and cooling rate using differencial scanning calorimetry. The degree of crystallization was increased with the increase of crystallization time at 25℃. The crystallization temperature was increased with the degree of cooling rate. When sample was reheated, recrystallization and cold crystallization were shown in sample which was cooled at the scan rate above 20℃/min. The crystallization degree of PGA which was crystallized bewteen 120℃ and 140℃ was more than that of PGA which was crystallized at 100℃ and 160℃.