• Title/Summary/Keyword: Thermogravimetric Analysis

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Structural Analysis of Carboxylic Acid-Functionalized Multi-walled Carbon Nanotubes

  • Oh, Weon-Tae;Kim, Jung-Soo;Lee, Geon-Woong
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.63-63
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    • 2007
  • Carboxylated multi-walled carbon nanotubes (MWNTs) were in detail characterized by XRD, XPS, FTIR, and thermogravimetric measurements. Carboxylic acid groups were functionalized to MWNTs using aqueous acid solutions. The change. of sonication and reflux conditions rarely influenced the degree of carboxylation on MWNTs, but reduced the thermal stability of the resulting carboxylated MWNTs. The characteristic Bragg peaks of pristine and carboxylated MWNTs were analyzed by XRD measurements. After acid treatment the diffraction peaks (100), (101), and (102) of pristine MWNTs disappeared, but the diffraction peak (002) was preserved in the carboxylated MWNTs. The introduction of carboxylic acid groups on MWNTs caused to improve the dispersibility of the resulting carboxylated MWNTs in water.

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Studies on Properties of Polyaniline-Dodecylbenzene Sulfonic Acid Composite Films Synthesized Using Different Oxidants

  • Basavaraja, C.;Pierson, R.;Huh, Do-Sung;Venkataraman, A.;Basavaraja, S.
    • Macromolecular Research
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    • v.17 no.8
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    • pp.609-615
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    • 2009
  • Two types of nano composite were obtained by in situ chemical method in polyaniline (PANI)/dodecyl-benzenesulfonic acid (DBSA) system depending on the use of either ammonium persulfate (APS) or ferric chloride ($FeCl_3$) as the oxidant. In order to study the difference of the two composites in the surface characteristics, thermal stability, and electric properties, the composite films were studied by transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and temperature dependent DC electrical conductivity. The results revealed a large difference in the surface morphology, thermal stability, and the microstructure properties between the two composites, and these differences were considered responsible for the molecular order and conductivity.

Study on the Oxidative Stabilization of PVC Pitch by Thermogravimetric Analysis (열중량분석을 이용한 PVC 핏치의 산화 안정화에 관한 연구)

  • Ha, Hyeon-Seung;Lee, Seung-Gu;Kim, Jeong-Il;Ju, Hyeok-Jong
    • Korean Journal of Materials Research
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    • v.7 no.9
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    • pp.738-743
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    • 1997
  • PVC핏치의 제조 조건에 따른 물성 변화 및 산화 안정화에 영향을 미치는 공정 변수를 연구하기 위하여 열중량 분석을 하였다. 산소 분위기를 사용하여 안정화온도, 승온속도 및 가스의 유량을 변화시켜 조사하였다. 안정화 온도가 높아짐에 따라 무게증가를 나타내는 시간구간이 짧아지고 결합되는 산소의 양은 감소하는 경향을 나타내며, 29$0^{\circ}C$정도로 안정화 온도가 높은 경우에는 결합되는 산소의양이 최대점에 도달한 후 다시 감소하는 경향을 나타냈다. 승온속도가 빨라짐에 따라 결합되는 산소의양은 감소하는 경향을 나타내었으나, 가스의 유량은 본 연구에서 설정한 범위 내에서는 영향이 관찰되지 않았다. 핏치 입자 직경이 커짐에 따라 최대 무게증가 값은 감소하고 최대 무게증가를 나타내는 온도는 증가함을 알았다. 그리고, 안정화에 의한 무게증가가 클수록 PVC핏치의 탄소수율은 감소하는 경향이 나타났다.

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Electron Beam Effects on Lignin Stabilization during Carbonization

  • Lee, Byoung-Min;Kang, Phil-Hyun;Jeun, Joon-Pyo
    • Journal of Radiation Industry
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    • v.7 no.2_3
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    • pp.167-170
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    • 2013
  • Lignin can be a valuable natural chemical resource. Structurally, lignin is a three-dimensional polymer made up of condensed C-C bonds and some ether linkages, most of which are not readily degraded. In this study, lignin carbonization under various electron beam pretreatment conditions was characterized through a thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Raman spectroscopy. Lignin stabilization was controlled by various doses of electron beam irradiation corresponding to 50, 100, 200, 500 and 1,000 kGy; the carbonization process was performed under a nitrogen gas atmosphere at $1000^{\circ}C$ for 1 h. The TGA results showed that a 1,000 kGy lignin dose increased the residue weight from 39.96% to 45.23%, compared to non-irradiated lignin. This observation is in agreement with the XRD and Raman spectroscopy results, in which the two theta degrees and the degree of crystallization were improved by increasing the electron beam irradiation.

Synthesis of Amphiphilic Poly(alkyl methacrylate-b-methacrylic acid) by Group Transfer Polymerization and Selective Hydrolysis

  • Soon Ki Kwon;Weon Jung Choi;Yun Hi Kim;Sam Kwon Choi
    • Bulletin of the Korean Chemical Society
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    • v.13 no.5
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    • pp.479-482
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    • 1992
  • Several poly(alkyl methacrylate-b-t-butyl methacrylate) diblock copolymers were synthesized by group transfer polymerization. The molecular weight of poly(t-butyl methacrylate) segments and the composition of the resulting block copolymers were controlled by the monomer feed ratios and mole ratios of monomer to initiator. The poly(t-butyl methacrylate) block was quantitatively hydrolyzed to poly(methacrylic acid) block by refluxing with a catalytic amount of p-toluenesulfonic acid in dioxane at $100^{\circ}C$ for 12 hrs. The thermogravimetric analysis of poly(alkyl methacrylate-b-t-butyl methacrylate) exhibited the lose of isobutylene and subsequent anhydride formation in the range of $205-300^{\circ}C$.

Synthesis and Characterization of New Liquid Crystalline Fumarate and Maleate Monomers with Two Symmetrical Mesogens

  • 한양규;김경민
    • Bulletin of the Korean Chemical Society
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    • v.20 no.12
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    • pp.1421-1427
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    • 1999
  • 4-Hydroxy-4'-methoxyazobenzene and 4-hydroxy-4'-cyanoazobenzene were synthesized from phenol with p-anisidine and p-aminobenzonitrile through a diazotization reaction, respectively. They were reacted with 2-chloroethanol, 2-(2-chloroethoxy)ethanol, or 2-[2-(2-chloroethoxy)ethoxy]ethanol to produce six kinds of new mesogenic alcohols having an azobenzene group that is sensitive to the ultraviolet. Twelve kinds of new photoresponsive monomers with two symmetrical mesogens were prepared by the reaction of the mesogenic alcohols with fumaric acid or maleic acid through a Mitsunobu reaction. The resulting monomers have different length of flexible ethyleneoxy spacer tethered to azobenzene group. The length of the spacer affected their thermal stability, solubility, and phase transition temperature. Structures of the monomers were identified by FT-IR and ¹H-NMR spectra. Their phase transition temperatures and thermal stability were also investigated by a differential scanning calorimetry (DSC) and a thermogravimetric analysis (TGA). From an optical polarizing microscopy, all the prepared monomers except fumarate-1 and maleate-1 were found to show enantiotropic liquid crystallinity with a smectic texture like focal-conic, fan-shaped, and batonnet textures.

Preparation and Thermal Properties of Enaryloxynitriles End-Capped Polymer Precursors

  • Gil, Dae Su;Gong, Myeong Seon
    • Bulletin of the Korean Chemical Society
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    • v.21 no.6
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    • pp.557-561
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    • 2000
  • Various enaryloxynitriles-terminated reactive polymer precursors containing rigid aromatic units were prepared from various diamines and 1-(p-formylphenyl)-1-phenyl-2,2-dicyanoethene (1). Arylate end-capped model compounds linked with azomethine bond were also prepared by reacting p-formylphenyl benzoate with diamines to compare the curing ability. The oligomers were highly soluble in polar aprotic solvents such as N,N-dimethylformamide, dimethylsulfoxide and N-methyl-2 -pyrrolidinone. They generally showed an exothermic curing process between $280-350^{\circ}C$, attributable to the thermal crosslinking of the dicyanovinyl group in DSC analysis, and no weight loss at curing temperature. Upon heating the polymer precursors, heat-resistant and insoluble network polymers were obtained. Thermogravimetric analyses of the precursors containing rigid aromatic units showed thermal stability with a 77-92% residual weight at $500^{\circ}C$ under nitrogen.

Water Resistance and Thermal Properties of Resin Based on Silane-modified Vinyl Acetate-Acrylic Emulsion Copolymers (실리콘 수식 비닐아세테이트-아크릴 공중합체 수지의 방수성 및 열적 성질)

  • Naghash, Hamid Javaherian
    • Polymer(Korea)
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    • v.34 no.4
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    • pp.306-312
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    • 2010
  • Triphenylvinylsilane (TPVS) containing vinyl acetate (VAc), butyl acrylate (BA), and Nmethylolacrylamide (NMA) copolymers were prepared by emulsion polymerization. The polymerization was performed at $80^{\circ}C$ in the presence of auxiliary agents and ammonium peroxodisulfate (APS) as the initiator. Sodium dodecyl sulphate (SDS) and Arkupal N-300 were used as anionic and nonionic emulsifiers, respectively. The resulting copolymers were characterized by using Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC), and dynamic light scattering (DLS). Thermal properties of the copolymers were studied by using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The morphology of copolymers was also investigated by scanning electron microscopy (SEM) and then the effects of silicone concentrations on the properties of the TPVS-containing VAc-acrylic emulsion copolymers were discussed. The obtained copolymers have high solid content (50%) and can be used in weather resistant emulsion paints as a binder.

Rapid Formation of Optically Active and Organosoluble Polyamides Containing L-Alaninephthalimide Side Chain via Microwave Irradiation

  • Mallakpour, Shadpour;Rafiee, Zahra
    • Macromolecular Research
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    • v.17 no.11
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    • pp.901-906
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    • 2009
  • Several aromatic optically active polyamides (PA)s were synthesized from 5-(2-phthalimidiylpropanoylamino)isophthalic acid with various aromatic diamines via direct polycondensation with triphenyl phosphite and pyridine in the presence of calcium chloride and N-methyl-2-pyrrolidone under microwave irradiation and conventional heating conditions. Under the optimized conditions, the reaction mixture was irradiated for 2 min. with a 100% irradiation power (900 W). The resulting polymers were obtained in high yield and moderate inherent viscosity ranging from 0.35 to 0.60 dL/g. All synthesized polymers showed excellent solubility in amide-type solvents. Thermogravimetric analysis revealed a 10% weight loss temperature and char yield at $600^{\circ}C$ in a nitrogen atmosphere of > $350^{\circ}C$ and > 58%, respectively, which suggests that the resulting PAs have good thermal stability.

Crystal Form of Olmutinib

  • Lee, Chang-Yeob;Sohn, Young-Taek
    • Journal of the Korean Chemical Society
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    • v.63 no.1
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    • pp.7-11
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    • 2019
  • Olmutinib, N-[3-({2-[4-(4-methylpiperazine-1-yl)aniline]thieno[3,2-d]Pyrimidin-4-yl}oxy)phenyl]prop-2-enamide dihydrochloride monohydrate, $Olita^{TM}$ is an oral, third-generation epidermal growth factor receptor tyrosine kinase inhibitor (EGFR TKI) that was developed by Boehringer Ingelheim and Hanmi Pharmaceutical Co. Ltd for the treatment of non-small cell lung cancer (NSCLC). The aim of this work was to investigate the existence of polymorphs and pseudopolymorphs of olmutinib. Three crystal forms of olmutinib have been isolated by recrystallization and characterized by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis and powder X-ray diffractometry (PXRD). From the DSC and TG data it was confirmed that Form 1 is monohydrate, Form 2 is dihydrate, Form 3 is 1.5 hydrate. The PXRD patterns of three crystal forms were different respectively. After storage of 1 month at $2^{\circ}C$, 24% RH (Relative Humidity), Form 1, Form 2, and Form 3 were not transformed.