• 제목/요약/키워드: exotherm

검색결과 22건 처리시간 0.025초

에탄올처리 재생 작잠 견피브로인 필름의 구조 특성 (Structural Characteristics of Regenerated Antheraea pernyi Silk Fibroin Film treated with ethanol)

  • 우순옥;권해용;엄인철;박영환
    • 한국잠사곤충학회지
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    • 제42권2호
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    • pp.114-119
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    • 2000
  • Effects of ethanlo treatment on the structural and thermal characteristics of regenerated Antheraea pernyi silk fibroin (RSF) were investigated. Infrared spectroscopy and X-ray diffractometry showed that the conformational transition of RSF might be affected by concentration of ethanol and its treatment time. The structure of RSF was rapidly changed from random coil to $\beta$-sheet conformation when RSF was treated with les than 75% ethanol concentration. However, RSF treated with ethanol(100%) did not show conformational change. Differential scanning calorimetry showed that exotherm at 232$\^{C}$ disappeared and the intensity of endotherm at 228$\^{C}$ decreased with treatment of 75% ethanol. Dynamic thermal analysis showed that loss modulus (E") and tan $\delta$$\_$E/ of RSF treated with aqueous ethanol was broaden and shifted to higher temperature in comparison with those of untreated RSF.

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Synthesis of Polyacrylonitrile as Precursor for High-Performance Ultrafine Fibrids

  • Kim, Subong;Kuk, Yun-Su;Jin, Fan-Long;Park, Soo-Jin
    • Bulletin of the Korean Chemical Society
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    • 제35권2호
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    • pp.407-414
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    • 2014
  • Polyacrylonitrile (PAN) copolymers with different methyl acrylate (MA) contents were synthesized via solution polymerization and used as precursors for high-performance PAN ultrafine fibrids. The chemical structures of the copolymers were characterized using Fourier-transform infrared spectroscopy and $^{13}C$ nuclear magnetic resonance spectroscopy. Their particle sizes and aspect ratios increased with increasing viscosity, and the degree of crystallinity increased with decreasing concentration of copolymer solution. In contrast, their peak temperature and heat of exotherm increased with decreasing concentration of the copolymer solution. The aromatization indices (AIs) of the fibrids increased with increasing heat-treatment time; however, the AIs decreased when the heat-treatment temperature was higher than the onset temperature of the copolymers. On the other hand, the crystal sizes of the fibrids decreased with increasing concentration of the copolymer solution when the MA content was held constant.

Preparation and Thermal Properties of Enaminonitriles-Terminated Reactive Polymer Precursors

  • 박원순;길덕수;공명선
    • Bulletin of the Korean Chemical Society
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    • 제19권3호
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    • pp.291-295
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    • 1998
  • Various enaminonitriles-terminated reactive polymer precursors containing rigid aromatic and flexible alkyl units were prepared from the corresponding diamines and 1-chloro-1-phenyl-2,2-dicyanoethene (1). All the enaminonitriles-terminated precursors were characterized by spectroscopies and elemental analysis. They were highly soluble in DMF and NMP, and partially soluble in common organic solvents such as THF and acetone. They showed a large exotherm around 350 ℃ attributable to the thermal polymerization by crosslinking of the dicyanovinyl group. Upon heating the precursors, heat-resistant and insoluble network polymers were obtained. Thermogravimetric analyses of the precursors containing rigid aromatic moiety exhibited thermal stability with a 10% weight loss around 420-480 ℃ and 75-88% residual weight at 500 ℃ under nitrogen.

Preparation and Thermal Properties of Poly(enaminonitriles-ester)s Derived from Dicyanovinyl-Containing Bis-Hydroxy Monomers

  • 김종태;공명선
    • Bulletin of the Korean Chemical Society
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    • 제18권3호
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    • pp.328-333
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    • 1997
  • Dicyanovinyl-containing bis-hydroxy monomers, p-bis[1-(4-hydroxypiperidinyl)]-2,2-dicyanovinyl]benzene (2), p-bis[1-[1-(2-hydroxyethyl)piperazinyl]-2,2-dicyanovinyl]benzene (3), p-bis[1-(4-hydroxyphenylamino)-2,2-dicyanovinyl]benzene (4) and p-bis[1-[N-methyl-(N-hydroxyethyl)amino]]-2,2-dicyanovinyl]benzene (5) were prepared from p-bis(1-chloro-2,2-dicyanovinyl)benzene (1) and the corresponding amino alcohol. The poly(enaminonitriles-ester)s with a variety of chemical structures in the main chain were prepared from them. The chemical structure of polymers was confirmed through the syntheses of their corresponding model compounds. The polymers are easily soluble in polar aprotic solvents such as DMF, DMSO and NMP. Brittle and hard films can be cast from DMF solutions of polymers. Most polymers showed a large exotherm in DSC analyses and undergo a curing reaction around 350 ℃ to form insoluble materials. The polymers consisting of rigid aromatic moieties show 80-88% residual weight at 500 ℃ under nitrogen.

Study on Utilization of Converter Slag as Concrete Admixture

  • Satou, Masaki;Tsuyuki, Naomitsu;Umemura, Yasuhiro;Harada, Hiroshi
    • 대한전자공학회:학술대회논문집
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    • 대한전자공학회 2001년도 The 6th International Symposium of East Asian Resources Recycling Technology
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    • pp.514-519
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    • 2001
  • Converter has been slag produced 10 million tons per year in Japan. It is a steel making by product produced in the same way as the blast-furnace slag. Though blast-furnace slag is being used effectively as a concrete admixture, the converter stag has never been used effectively because of the expansion action of contained free lime and iron oxide. This is an important environmental problem in the steel industry. Beta-2CaOSiO$_2$(beta-C$_2$S) is contained 40 percent in converter slag, therefore it is very promising as a concrete admixture. We proposed an accelerated aging processes capable of stabilizing the converter slag in a short time. The converter slag is dipped into alkali aqueous solution after heating at low temperature. It was subsequently ground to a grain size of 75 ${\mu}{\textrm}{m}$ , inner 30 percent of OPC. The properties of mortar and concrete using the blended cement were determined. As a result, it has become apparent that the expansion was reduced and long term compressive strength was increased while that at early ages was not so remarkable. The hydration exotherm rate was lower than that of the OPC.

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기계적 합금화에 의한 Al-25at%Nb 혼합분말의 상형성 거동 (Phase Formation Behavior of Mechanical Alloyed Al-25at% Nb Powder Mixtures)

  • 이상호;김동관;이진형
    • 한국재료학회지
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    • 제5권8호
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    • pp.997-1004
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    • 1995
  • 기계적 합금화(mechanical alloying:MA) 방법에 의해 원소 Nb와 Al의 혼합분말로부터 금속간 화합물 NbA1₃와 비정질상을 얻었다. 혼합분말의 조성은 Nb-45wt%Al(75at%Al)으로 하였으며, 기계적 합금화는 고에너지 SPEX8000 mixer/mill을 사용하여 72시간까지 행하였다. 얻어진 분말은 XRD, DTA, SEM 및 TEM으로 분석했다. 기계적 합금화 초기 단계의 분말은 층상 구조를 나타냈고, 정상상태에 도달하였을 때는 분말 내에서 원소 Nb와 Al이 균일하게 분포되어 있었다. 4시간 기계적 합금화를 하였을 때 금속간 화합물 NbA1₃가 형성되었다. 기계적 합금화된 분말들은 안정한 NbA1₃형성 및 응력 완화에 해당되는 600℃ 근처에서 큰 발열 peak을 나타냈다.

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Azomethine 기를 가지는 신소재 액정 에폭시 (LCE)와 지방족 아민의 경화반응 (Curing Reaction of Noble Liquid Crystalline Epoxy (LCE) with Azomethine/Aliphatic Amine)

  • 김상욱
    • 한국재료학회지
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    • 제11권9호
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    • pp.786-791
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    • 2001
  • $\alpha$,$\omega$-Bis(4-glycidyloxybenzylidene-4-aminophenyl)methane (BGBAM) was synthesized from the initial materials, 4-hydroxylbenzaldehyde (HBA), 4,4'-methylenedianiline (MDA) and epichlorohydrin. The DSC trace for BGBAM shows two endotherms associated with the liquid crystalline phase transition around $104.2^{\circ}C$ and the isotropic transition around $171.2^{\circ}C$, and it also has a broad exotherm in the range of $178~300^{\circ}C$ due to the anionic homopolymerization of BGBAM. DSC curve for the curing of BGBAM with hexamethylene diamine (HMD) shows an endothermic peak around $93^{\circ}C$ attributed to the melting of BGBAM. It also has three exothermic peaks around $128.4^{\circ}C$ and $180.2^{\circ}C$ associated with the epoxide-amine reaction and weak peak in the range of $200~263^{\circ}C$ related to the anionic homopolymerization between the unreacted epoxide groups. The activation energy values of cure reaction by Kissinger method are 66.5, 67.3 and 90.6 kJ/mol for $T_{pl},\; T_{p2}\; and \;T_{p3},\; respectively$. The kinetic parameters by isoconverional method are similar value to those from Kissinger method.

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폴리스티렌 모르타르의 양생재령에 따른 경화거동 (Setting Behavior of Polystyrene Mortars with Elapsed Curing Time)

  • 최낙운;김한상
    • 콘크리트학회논문집
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    • 제16권1호
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    • pp.54-60
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    • 2004
  • 발포폴리스티렌(EPS)의 효율적인 재활용 기술개발의 일환으로서 폐 발포폴리스티렌을 중합성 모노머인 스티렌에 용해한 고분자 용액에 가교제, 개시제, 촉진제 등을 첨가하여 상온 중합성 결합재를 개발하였으며 이를 이용한 폴리스티렌 모르타르를 제조하여 그 중요한 경화특성인 사용가능시간, 건조양생재령에 따른 발열온도 및 길이변화 거동에 미치는 폐 발포폴리스티렌 용액농도 및 TMPTMA 첨가량의 영향에 대해서 검토하였다. EPS용액을 이용한 결합재 및 폴리스티렌 모르타르의 사용가능시간은 EPS용액 농도 및 TMPTMA 첨가율의 증가에 따라서 짧아지며, 또한 폴리스티렌 모르타르의 경화에 따른 길이변화는 EPS용액 농도 및 TMPTMA 첨가율에 크게 영향을 받는데 이를 적절히 조절하여 경화특성을 제어함으로써 저수축 혹은 무수축 폴리스티렌 모르타르의 제조가 가능하다는 것을 검증하고 있다.

전자 Package 봉착유리의 합성과 결정화 (Synthesis and crystallization of solder glass for electronic package)

  • Kyung Nam Choi;Byoung Chan Kim;Byoung Woo Kim;Hyung Suk Kim;Hee Chan Park;Myung Mo Son;Heon Soo Lee
    • 한국결정성장학회지
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    • 제10권6호
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    • pp.407-411
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    • 2000
  • 전자 package용 저온봉착 유리를 실험적으로 합성하고 이 유리의 결정화 거동을 비등온 조건하에서 열분석기(DTA)를 이용하여 조사하였다. 이 유리의 조성을 미량의 CaO, $SiO_2$$A1_2$$O_3$$P_2$$O_5$ 등이 함유된 PbO-ZnO-$B_2$$O_3$-$TiO_2$유리로부터 결정하였다. 연 티탄산염($PbTiO_3$)생성에 해당되는 결정화 발열이 관찰되었다. 이 $PbTiO_3$의 결정화는 삼차원과정으로 진행되었고 유리기지(glass matrix)로부터 생성되는 이 결정의 평균 활성화에너지는 223$\pm$3 kJ/mo1 이었다.

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가교형 이미드 올리고머 제조 및 듀얼 오브너블 용기(Dual-Ovenable Packaging) 용 폴리에테르이미드에 대한 적용 연구 (Preparation of crosslinkable imide oligomers and Applications in Polyether Imides for Dual-ovenable Packaging)

  • 서종철;박수일;최승혁;장원봉;한학수
    • Korean Chemical Engineering Research
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    • 제48권1호
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    • pp.45-52
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    • 2010
  • 본 연구에서는 Dual-Ovenable Packaging 용 폴리에테르이미드의 수분흡수 특성을 개선하기 위하여 가교구조를 형성할 수 있는 말단기를 포함한 이미드 올리고머를 신규 합성하였으며, 이를 이용한 폴리에테르이미드와 가교구조 (semi-IPN, semi-interpenetrating network)를 형성을 통하여 수분흡수와 열적 특성 변화, 그리고 구조적 특성에 대하여 조사하였다. 가교 말단기와 용액 이미드화법을 이용하여 두 종류의 이미드 올리고머 6FDA-ODA/APA와 6FDA-MDA/MA를 제조하였으며, 그 특성을 고찰하였다. 또한 이미드 올리고머와 $Ultem^{(R)}$ 혼합물의 semi-IPN 구조를 제조하였으며, 열적 성질, 수분흡수 거동, 그리고 박막의 구조적 특징을 TGA, Thin Film Diffusion Analyzer, 그리고 XRD 분석을 이용하여 해석하였다. 제조한 이미드 올리고머는 말단기의 양을 이용하여 분자량 조절이 가능하였다. 그리고, 온도가 증가함에 따라 가교에 의한 발열반응이 일어나며, 가교 가능한 말단기가 증가할수록 발열량이 증가하였다. $Ultem^{(R)}$과 이미드 올리고머 혼합물에 의한 semi-IPN 구조는 이미드 올리고머의 비율이 증가할수록 5와 10% 질량감소 온도가 상승하였다. 또한, 수분에 대한 친화도가 작은 불소기를 함유하는 이미드 올리고머와 패킹정도의 증가로 인하여 semi-IPN의 확산계수와 수분흡수량이 감소하였다. 이와 같이 열적 성질과 수분에 대한 안정성이 떨어지는 단점을 semi-IPN 구조를 통하여 보완할 수 있었다.