• Title/Summary/Keyword: thermal polymerization

Search Result 470, Processing Time 0.029 seconds

Polymerization and Thermal Characteristics of Acrylonitrile/Dicyclohexylammonium 2-Cyanoacrylate Copolymers for Carbon Fiber Precursors

  • Kim, Ki-Young;Park, Woo-Lee;Chung, Yong-Sik;Shin, Dong-Geun;Han, Jin-Wook
    • Carbon letters
    • /
    • v.12 no.1
    • /
    • pp.31-38
    • /
    • 2011
  • This study experimentally investigated dicyclohexylammonium 2-cyanoacrylate (CA) as a potential comonomer for polyacrylonitrile (PAN) based carbon fiber precursors. The P(AN-CA) copolymers with different CA contents (0.19-0.78 mol% in the feed) were polymerized using solution polymerization with 2,2-azobis(isobutyronitrile) as an initiator. The chemical structure and composition of P(AN-CA) copolymers were determined by proton nuclear magnetic resonance and elemental analysis, and the copolymer composition was similar to the feeding ratio of the monomers. The effects of CA comonomer on the thermal properties of its copolymers were characterized differential scanning calorimetry (DSC) in nitrogen and air atmospheres. The DSC curves of P(AN-CA) under nitrogen atmosphere indicated that the initiation temperature for cyclization of nitrile groups was reduced to around $235^{\circ}C$. The heat release and the activation energy for cyclization reactions were decreased in comparison with those of PAN homopolymers. On the other hand, under air atmosphere, the P(AN-CA) with 0.78 mol% CA content showed that the initiation temperature of cyclization was significantly lowered to $160.1^{\circ}C$. The activation energy value showed 116 kJ/mol, that was smaller than that of the copolymers with 0.82 mol% of itaconic acids. The thermal stability of P(AN-CA), evidenced by thermogravimetric analyses in air atmosphere, was found higher than PAN homopolymer and similar to P(AN-IA) copolymers. Therefore, this study successfully demonstrated the great potential of P(AN-CA) copolymers as carbon fiber precursors, taking advantages of the temperature-lowering effects of CA comonomers and higher thermal stability of the CA copolymers for the stabilizing processes.

The Investigation on Thermal Aging Characteristics of Oil-Paper Insulation in Bushing

  • Liao, Rui-jin;Hu, En-de;Yang, Li-jun;Xu, Zuo-ming
    • Journal of Electrical Engineering and Technology
    • /
    • v.10 no.3
    • /
    • pp.1114-1123
    • /
    • 2015
  • Bushing is the key link to connect outer and inner insulating systems and also the essential electric accessory in electric power system, especially in the high voltage engineering (AC 1000kV, DC 800kV). This paper presented the experimental research of thermal aging characteristic of oil-paper insulation used in bushing. A thermally accelerated aging experiment at 90℃ was performed. The bushing models containing five layers of paper were sealed into the aging vessels and further aged for 250 days. Then several important parameters associated with the aging were observed and evaluated. The results showed that the degree of polymerization (DP) of papers gradually decreased. The DP values of outermost layer and middle layer fit well into the second-order kinematic model and first-order kinematic model, respectively. Less deterioration speed of the inter-layer paper than outer layer was confirmed by the variation of DP. Hydrolysis was considered as the main cause to this phenomenon. In addition, the logarithm of the furfural concentrations in insulation oil was found to have good linear relationship with DP of papers. Interestingly, when the aging time is about 250 days and DP is 419, the aging process reaches an inflection point at which the DP approaches the leveling off degree of polymerization (LODP) value. Both tanδ and acid number of oils increased, while surface and volume resistivity of papers decreased. The obtained results demonstrated that thermal aging and moisture absorbed in papers brought great influence to the degradation of insulating paper, leading to rapid decrease of DP and increase of the tanδ. Thus, the bushing should be avoided from damp and real-time monitoring to the variation of tanδ and DP values of paper is an effective way to evaluate the insulation status of bushing.

Preparation and Characterization of Vapor-Grown Carbon Nanofibers-Reinforced Polyimide Composites by in-situ Polymerization (In-situ 중합법에 의한 기상성장 탄소나노섬유/폴리이미드 복합재료의 제조 및 물성)

  • Park, Soo-Jin;Lee, Eun-Jung;Lee, Jae-Rock;Won, Ho-Youn;Moon, Doo-Kyung
    • Polymer(Korea)
    • /
    • v.31 no.2
    • /
    • pp.117-122
    • /
    • 2007
  • In this work, the mechanical and electrical properties, and thermal stability of vapor-grown carbon nanofibers/polyimide (VGCNFs/PI) composite film synthesized by in-situ polymerization were investigated in terms of tensile properties, volume resistivity and thermogravimetric analysis (TGA), respectively. From the results, the addition of VGCNFs with a certain amount into polyimide led to obvious improvement in tensile strength. The volume resistivity of the films was decreased with increasing the VGCNFs content and the electrical percolation threshold appeared between 1 and 3 wt% of VGCNFs content, which was probably caused by the formation of interconnective structures among the VGCNFs in a composite system. The thermal stability of the film was higher than that of pure PI one. This result indicated that the crosslinking of VGCNFs/PI Composites was enhanced by well-distribution of YGCNFs in PI resin, resulting in the increase of the thermal stability of the resulting composites.

Fabrication of Carbon Microcapsules Containing Silicon Nanoparticles-Carbon Nanotubes Nanocomposite for Anode in Lithium Ion Battery

  • Bae, Joon-Won;Park, Jong-Nam
    • Bulletin of the Korean Chemical Society
    • /
    • v.33 no.9
    • /
    • pp.3025-3032
    • /
    • 2012
  • Carbon microcapsules containing silicon nanoparticles (Si NPs)-carbon nanotubes (CNTs) nanocomposite (Si-CNT@C) have been fabricated by a two step polymerization method. Silicon nanoparticles-carbon nanotubes (Si-CNT) nanohybrids were prepared with a wet-type beadsmill method. A polymer, which is easily removable by a thermal treatment (intermediate polymer) was polymerized on the outer surfaces of Si-CNT nanocomposites. Subsequently, another polymer, which can be carbonized by thermal heating (carbon precursor polymer) was incorporated onto the surfaces of pre-existing polymer layer. In this way, polymer precursor spheres containing Si-CNT nanohybrids were produced using a two step polymerization. The intermediate polymer must disappear during carbonization resulting in the formation of an internal free space. The carbon precursor polymer should transform to carbon shell to encapsulate remaining Si-CNT nanocomposites. Therefore, hollow carbon microcapsules containing Si-CNT nanocomposites could be obtained (Si-CNT@C). The successful fabrication was confirmed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). These final materials were employed for anode performance improvement in lithium ion battery. The cyclic performances of these Si-CNT@C microcapsules were measured with a lithium battery half cell tests.

Preparation of Anhydrous Crosslinked Graft Copolymer Electrolyte Membrane (무가습 가교 가지형 공중합체 전해질 막의 제조)

  • Roh, Dong-Kyu;Koh, Joo-hwan;Park, Jung-tae;Seo, Jin-ah;Kim, Jong-hak
    • 한국신재생에너지학회:학술대회논문집
    • /
    • 2009.06a
    • /
    • pp.270-273
    • /
    • 2009
  • A comb-like copolymer consisting of a poly(vinylidene fluoride-co-chlorotrifluoro-ethylene) backbone and poly(hydroxy ethyl acrylate) side chains, i.e. P(VDF-co-CTFE)-g-PHEA, was synthesized through atom transfer radical polymerization (ATRP) using CTFE units as a macroinitiator. Successful synthesis and a microphase-separated structure of the copolymer were confirmed by proton nuclear magnetic resonance (1H-NMR), FT-IR spectroscopy, and transmission electron microscopy (TEM). This comb-like polymer was crosslinked with 4,5-imidazole dicarboxylic acid (IDA) via the esterification of the -OH groups of PHEA and the -COOH groups of IDA. Upon doping with phosphoric acid ($H_3PO_4$) to form imidazole-$H_3PO_4$ complexes, the proton conductivity of the membranes continuously increased with increasing $H_3PO_4$ content. A maximum proton conductivity of 0.015 S/cm was achieved at $120^{\circ}C$ under anhydrous conditions. In addition, these P(VDF-co-CTFE)-g-PHEA/IDA/$H_3PO_4$ membranes exhibited good mechanical properties (765 MPa of Young's modulus), and high thermal stability up to $250^{\circ}C$, as determined by a universal testing machine (UTM) and thermal gravimetric analysis (TGA), respectively.

  • PDF

Characterization of Nafion/Pt/Polypyrrole Composite Membrane Prepared by Chemical In-situ Polymerization for DMFC (화학적 합성에 의해 제조된 직접 메탄올 연료전지용 나피온/백금/폴리피롤 복합 막의 특성 분석)

  • Park, Ho-Seok;Kim, Yo-Jin;Im, Hun-Suk;Choi, Bong-Gill;Hong, Won-Hi
    • 한국신재생에너지학회:학술대회논문집
    • /
    • 2006.11a
    • /
    • pp.421-424
    • /
    • 2006
  • Nafion/Pt/Polypyrrole composite membranes were fabricated by chemical in-situ polymerization of pyrrole monomers with Pt precursors in Nafion matrix for DMFC. We demonstrated that positively charged pyrrolinum groups of polypyrrole particles were co-interacted with sulfonic groups of Nafion as verified by FT-IR results. Mutual interaction between $Nafion-SO_3^-$ (or negatively charged Pt precursors) and Polypyrrole$-NH_2^+$ influenced the physical properties of pristine Nafion. Thermal property proton conductivity, methanol permeability, and cell performance of pristine and modified Nafion were analyzed for an application of DMFC membrane. Thermal stabilities of sulfonic groups and side chains in Nafion/Pt/polypyrrole composite membranes were higher than those of Nafion due to mutual interaction between sulfonic groups of Nafion and pyrrolinum groups of polypyrrole. Methanol permeabilities of Nafion/Pt/Polypyrrole composite were reduced more proton conductivities with the increase in the content of Pt particles. As a result of that, the enhancement of cell performance by Nafion/Pt/Polypyrole O2 relative to Nafion was more pronounced under the specific experimental condition such as high temperature and more concentrated methanol solution.

  • PDF

Synthesis and Properties of Energetic Thermoplastic Polyurethane included Glycidyl Azide Polymer (Glycidyl Azide Polymer를 포함하는 에너지화 열가소성 폴리우레탄의 합성 및 성질)

  • Kim, Hyoung-Sug;You, Jong-Sung;Kweon, Jung-Ok;Noh, Si-Tae;Kwon, Soon-Kil;Lee, Jung-Hwan;Yu, Jae-Chul;Choi, Keun-Bae
    • Journal of the Korea Institute of Military Science and Technology
    • /
    • v.12 no.5
    • /
    • pp.660-666
    • /
    • 2009
  • Thermoplastic polyurethane elastomer(PU-TPE) and energetic thermoplastic polyurethane Elastomer(E-PU-TPE) were prepared from Hexamethylene diisocyanate(HDI), 1,4-BD/AA ester polyol and glycidyl azide polymer(GAP-2400) as an energetic material by the addition polymerization. The PU-TPE and E-PU-TPE were characterized by FT-IR and GPC. Viscometer, DSC and UTM were used to investigate the viscose behavior with a various solvent, thermal properties and mechanical properties of PU-TPE and E-PU-TPE, which are of potential interest for the development of high performance binder of energetic solid propellants. It was found that $M_w$ of PU-TPE and E-PU-TPEs are over 100,000 and decreased with increase of GAP-2400 contents. $T_m$ and ${\Delta}H$ as thermal properties decreased and also tensile strength and elongation at break as mechanical properties decreased with increase of GAP-2400 contents.

Synthesis and Thermal Property of Poly(styrene-g-caprolactone) with Well-defined Structure (분자구조가 제어된 Poly(styrene-g-caprolactone)의 합성 및 그라프트 공중합체의 열적 성질)

  • 오병석;안성국;조창기
    • Polymer(Korea)
    • /
    • v.24 no.3
    • /
    • pp.306-313
    • /
    • 2000
  • Polycaprolactone (PCL) macromer containing terminal methacrylate group was synthesized by ring-opening polymerization. The number average molecular weight of PCL macromer was 11600 g/mole and polydispersity index was 1.09. The synthesized PCL macromer was copolymerized with styrene by stable free radical polymerization using 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO), benzoyl peroxide, and well-defined poly(styrene-g-caprolactone)s were synthesized. The synthesized copolymers was characterized by $^1$H-NMR and gel permeation chromatography equipped with multiangle laser light scattering detector. Thermal properties of graft copolymers were investigated by DSC.

  • PDF

Synthesis, chemically and electrochemically polymerization of N-substituted pyrrole containing azo chromophore and its copolymerization with pyrrole

  • Hosseini, Seyed Hossein
    • Advances in materials Research
    • /
    • v.1 no.4
    • /
    • pp.299-310
    • /
    • 2012
  • This article describes the synthesis of a novel N-substituted pyrrole monomer containing an azobenzene group. The 2-[N-ethyl-N-[4-[(4-nitrophenyl) azo]-phenyl] amino] ethyl-3-chloropropionate (RedII) compound was synthesized via reaction of 4-nitro-4'-[N-ethyl-N-(2-hydroxyethyl)-amino] azobenzene (RedI) and 3-chloropropionic acid. RedII was reacted with the potassium salt of pyrrole then 2-[N-ethyl-N-[4-[(nitro phenyl) azo] phenyl] amino] ethyl-N-pyrrolyl propionate (Py-RedII) was prepared. Chemical polymerization of Py-RedII and copolymerization of Py-RedII with pyrrole carried out using $FeCl_3$. Poly (2-[N-ethyl-N-[4-[(nitro phenyl) azo] phenyl] amino] ethyl-N-pyrrolyl propionate) (PPy-RedII) was characterized by UV, IR, $^1HNMR$, $^{13}CNMR$ spectroscopies. Electropolymerization of Py-RedII and electroco-polymerization of Py-RedII and pyrrole were studied using conventional three electrodes system, Ag/AgCl reference electrode, platinum counter electrode and GC disk working electrode. Scanning electron microscopy (SEM), thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC) were used for thermal and rheological studies. The TGA curve of PPy-RedII demonstrated a high thermal stability up to 200°C and its DSC thermogram showed two endothermic peaks at 88 and $122^{\circ}C$. The glass transition temperature of the polymer was found to be above the room temperature. Electrical conductivities of PPy-RedII and it's copolymer with pyrrole (PPy-RedII-co-Py) were studied by the four-probe method and produced conductivities of $7.5{\times}10^{-4}$ and $6.5{\times}10^{-3}Scm^{-1}$, respectively.