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이범재(Bum Jae Lee),신대현(Dae Hyun Shin) 대한공업교육학회 1981 대한공업교육학회지 Vol.6 No.2
The relationships of polymer structure to mechanical properties were studied in Carboxyl Terminated Polybutadiene (CTPB) and Hydroxyl Terminated Polybutadiene (HTPB) gumstocks. CTPB, HTPB prepolymer having various molecular weights and average functionality were crosslinked with EPOXIDE, ISOCYANATE curing agents of different functionalities and molecular structure, crosslink density was used and measured by solvent swollen compression modulus method. Crosslink density was closely related with mechanical properties, especially in modulus and elongation at rupture. A single linear relationship between γ(experimental crosslink density) and E_0 (Young`s modulus) was held regardless of gumstock cure systems. This relationship was reasonably in agreement with the simple kinetic theory of rubber elasticity.
고체 추진제용 폴리우레탄 바인더를 위한 새로운 폴리에테르 공중합체 디올(HTPE)의 합성
신범식(Bum-Sik Shin),이범재(Bum-Jae Lee),유호준(Ho-Joon You),박영철(Young-Chul Park) 한국추진공학회 2008 한국추진공학회 학술대회논문집 Vol.2008 No.5
Hydroxy-terminated polyether의 새로운 합성방법인 양이온 개환 공중합에 의해서 Ethylene oxide와 Tetrahydrofuran을 공중합 하였다. 중합은 1,4-Butandiol 존재 하에 BF3.THF를 촉매로 반응이 진행되어 잘 제어된 Polyetherdiol을 합성할 수 있었다. Polyurethane 반응은 Polyetherdiol과 경화제로써 I-PDI/N-100 혼합물을 사용하였고, 경화촉매로 TPB/MA 혼합물을 사용하여 합성하였다. 이렇게 합성된 Polyurethane은 현재 미국에서 시판중인 ATK HTPE를 이용한 Polyurethane과 기계적 특성과 경화 거동을 비교 분석하였다. Novel synthetic routes were proposed for hydroxy-terminated Poly(EO-co-THF) by Cationic ring-opening copolymerization of Tetrahydrofuran(THF) and Ethylene oxide(EO). It was carried out using Boron trfluoride tetrahydrofuranate(BF3?THF complex) as catalyst in the presence of 1,4-butandiol. The resultant products are well-defined linear polyetherpolyol. Polyurethane(TPU) were prepared using resultant polyetherpolyol with IPDI/N-100 as curing agent and TPB(Triphenylbismuth) /MA(Maleic anhydride) mixture as cure catalyst. Mechanical properties of TPU prepared from poly(EO-co-THF) polyol were investigated and compared with polyurethane using ATK HTPE
Glycidyl Azido Copolyetherdiol을 이용한 Polyurethane의 합성과 특성분석
신범식(Bum-Sik Shin),이범재(Bum-Jae Lee),박영철(Young-Chul Park),황갑성(Kab-Sung Hwang) 한국추진공학회 2008 한국추진공학회 학술대회논문집 Vol.2008 No.11
양이온 개환중합법을 이용하여 Epichlorohydrin(ECH)과 Tetrahydrofuran(THF)을 공중합 하였다. 중합은 1,4-Butandiol 존재 하에 BF3THF를 촉매로 사용하여 잘 제어된 Copolyetherdiol을 합성하였다. 분자량은 [monomer]/[diol]비를 조절하였고, 공중합체 조성은 ECH와 THF의 투입몰비를 변화하여 조절하였다. 합성된 Copolyetherdiol의 Chlorine기는 SN2반응을 이용하여 Azide기로 치환하였다. 합성된 고분자를 프리폴리머로 사용하여 경화제인 N-100/IPDI와 경화촉매인 TPB/MA 혼합촉매를 이용하여 Polyurethane을 합성하여 경화거동과 기계적 특성은 비교 분석하였다. The well-defined copolymers derived from Epichlorohydrin(ECH), Tetrahydrofuran(THF) were synthesized by Cationic ring-opening polymerization(CROP) with 1,4-Butandiol, a initiator, and BF3THF Complex, a catalyst via Activated monomer mechanism, which could lead to hydroxyl-terminated polyethers. The molecular weight of polymers were dependant on the ratio of [monomer]/[diol], Copolymer structures were controlled by monomers feed ratio, ECH and THF added. This polymers were functionalized from Chlorine group to Azide group using SN2 reaction. Synthesized polymers were found to be as the prepolymer for polyurethane. Polyurethane was synthesized in the presence of N-100/IPDI mixture, a curing agent, and TPB(triphenyl bismuth)/MA(Maleic anhydride) mixture, a catalyst system. The curing behavior and mechanical properties of polyurethane after mixing with various prepolymer’s composition and the molecular weight were studied.
Poly( t-butylstyrene) 그라프트를 가지는 수산기 말단 관능화 폴리올레핀 탄성체의 합성
이형우 ( Hyoung Woo Lee ),조희원 ( Hee Won Cho ),이상민 ( Sang Min Lee ),박샛별 ( Sat Byeol Park ),김동현 ( Dong Hyun Kim ),이범재 ( Bum Jae Lee ) 한국고무학회 2013 엘라스토머 및 콤포지트 Vol.48 No.1
선형 poly(ethylene-ter-1-hexene-ter-divinylbenzene) 소프트 탄성체 블럭내의 styrene 관능기로부터 poly( t-butylstyrene)하드 블록을 graft-from 음이온 중합을 통해 고온에서 사용 가능한 기능성 폴레올레핀 열가소성 탄성체인 polyolefin-g-poly( t-butylstyrene)을 합성하였다. sec-BuLi/TMEDA와 styrene 단위로부터 반응에 의하여 100% 수율의 음이온 개시 자리를 만들고 4-tert-butylstyrene을 graft-from 중합시켜 10,000~30,000 g/mol 분자량을 가지는 블록을 합성함으로서, 고온 Tg를 가지는 폴리올레핀 그라프트 고분자를 얻을 수 있었다. 단량체 함량과 중합시간에 따라 그라프트 분자량이 비례하여 증가하는 효과적인 리빙 중합방법임을 확인하였다. 사슬 말단에 다수의 수산기가 도입된 폴리올레핀 TPE의 합성방법으로서, 리빙 그라프트 고분자 사슬에 계속하여 isoprene을 블록 중합하여 얻어진 polyolefin-g-[poly( t-butylstyrene)-b-high vinyl polyisoprene]의 비닐기와 2-mercaptoethanol간의 thiol-ene 클릭 반응을 이용하는 방법을 통해 진행하였다. 연구 결과, 높은 Tg(>145 ℃)를 갖는 정밀 제어된 기능성 그라프트 형태의 폴리올레핀 기반 TPE를 합성하는 방법을 확립하였다. Polyolefin-g-poly(t-butylstyrene) as one of the high-temperature polyolefin-based thermoplastic elastomers was synthesized by the graft-from anionic living polymerization from the styrene moieties of the linear poly(ethylene- ter-1-hexene-ter-divinylbenzene) as a soft block to form the hard end blocks, poly(t-butylstyrene). The chemistry of the anionic graft-from polymerization involved complete lithiation of the pendant styrene unit of the soft polyolefin elastomer with sec-BuLi/TMEDA followed by the subsequent graft anionic polymerization of 4-tert-butylstyrene with Mn=10,000~30,000 g/mol. The graft-from living anionic polymerization were very effective and the grafting size increased proportionally with increasing monomer concentration and the reaction times. The synthetic methodology for the multi-hydroxyl chain-end modified polyolefin-g-poly(t-butylstyrene) was proposed by using the thiol-ene click reaction between 2-mercaptoethanol and the polyolefin- g-[poly(t-butylstyrene)-b-high vinyl polyisoprene], which was obtained from the subsequent living block copolymerization using polyolefin-g-Poly(t-butylstyrene) with isoprene. The result indicated that this process produced a new well-defined functionalized graft-type polyolefin-based TPE with high Tg hard block(> 145 ℃).
강대현(Dae Hyun Kang),이범재(Bum Jae Lee),윤창배(Chang Bae Yun),김강욱(Kang Wuk Kim) 대한기계학회 2010 大韓機械學會論文集A Vol.34 No.5
고주파열처리(induction hardening)는 엔진의 구동력을 차동장치에서 바퀴까지 전달해주는 부품인 액슬축(axle shaft)의 비틀림 강도를 증가시키기 위해 적용되는 열처리 방법이다. 고주파 열처리 과정의 급속가열과 급속냉각은 소재에 잔류응력과 물성치를 변화시켜 액슬축의 허용 전달토크를 변화시킨다. 본 연구에서는 고주파 열처리한 액슬축의 잔류응력의 분포와 열처리 깊이에 따른 비틀림 강도 변화를 열물성 및 상변태를 고려한 유한요소 해석을 통해 예측하였으며 이를 시험과 비교하였다. Induction hardening has been used to improve the torsional strength and characteristics of wear for axle shaft that is used to transmit driving torque from the differential to the wheel in automobiles. After the rapid heating and cooling processes of induction hardening are carried out, the shaft has residual stress and material properties change; this affects the allowable transmitted torque. The objective of this study is to predict the distribution of residual stress and estimate the torsional strength of induction-hardened axle shafts with residual stress. In this study, the finite element method is used to study the thermomechanical behavior of the material, and the results are compared with experimental results. The results indicate that the torsional strength of the axle shaft depends on the surface hardening depth and distribution of residual stress.