• Title/Summary/Keyword: Thermal reaction

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Microwave-Syntheses of Zeolitic Imidazolate Framework Material, ZIF-8 (마이크로파에 의한 Zeolitic Imidazolate Framework 물질, ZIF-8의 합성)

  • Park, Jung-Hwa;Park, Seon-Hye;Jhung, Sung-Hwa
    • Journal of the Korean Chemical Society
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    • v.53 no.5
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    • pp.553-559
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    • 2009
  • One of zeolitic imidazolate framework materials (ZIF), ZIF-8, has been synthesized with microwave irradiation and conventional electric heating at $140{\sim}180^{\circ}C}$. ZIFs are porous crystalline materials and are similar to metal organic framework (MOF) materials because both ZIFs and MOFs are composed of both organic and metallic components. ZIFs are very stable and similar to zeolites because ZIFs have tetrahedral networks. ZIF-8, with a decreased crystal size, can be synthesized rapidly with microwave irradiation. The microwave synthesis of ZIF-8 is completed in 4 h at $140{^{\circ}C}$ and the reaction time is decreased by about 5 times compared with the conventional electric heating. The ZIF-8 obtained by microwave heating has larger surface area and micropore volume compared with the ZIF-8 synthesized with conventional electric heating. It can be confirmed that ZIF-8s show type-I adsorption isotherms, explaining the microporosity of the ZIF-8s. Based on FTIR and TGA results, it can be understood that the ZIF-8s have similar bonding and thermal characteristics irrespective of heating methods such as microwave and conventional heating.

A Study on the Preparation of Halogen Free M-P Flame Retardant and Its Application to Composite Material (비할로겐 M-P 난연제 제조 및 복합재료 응용 연구)

  • Lee, Soon-Hong
    • Journal of the Korean Society of Safety
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    • v.24 no.6
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    • pp.63-71
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    • 2009
  • In order to improve flame retardancy, the halogen free organic melamine phosphate(M-P) flame retardant was synthesized from melamine and phosphoric acid by the reaction of precipitation. The ignition test was carried out preparing hybrid flame retardant compound($H_bFRC$) consisting of organic M-P and inorganic Mg$(OH)_2$ as a flame retardant in the polyolefin resins. The flame retardancy and mechanical properties of flame retardant aluminum composite panel($H_bFRC$-ACP) were performed to investigate the possibility of the composite material, which was contained M-P, as a inner core for $H_bFRC$-ACP. For this study, the results of ignition test indicate that a char formation and drip suppressing effect, and combustion time reduced as the content of M-P increased. The limited oxygen index(LOI) values were measured 17.4vol% and 31.5vol% for LDPE only and $H_bFRC$-3(M-P content: 15wt%), respectively. And it was verified that the $H_bFRC$-3 was needed more oxygen quantity with the increase of M-P content when it combustion. Also, the results from thermogravimetric analysis were observed endothermic peak at $350^{\circ}C$ and $550^{\circ}C$, it was confirmed predominant thermal stability though the wide temperature range by the mixture of M-P and Mg$(OH)_2$. The LDPE-ACP (using only LDPE as a inner core), $35.13kW/m^2$ of heat release rate(HRR) and 13.43MJ/m2 of total heat release(THR) were measured while the $H_bFRC$-ACP, $10.44kW/m^2$ of HRR and 1.84MJ/m2 of THR were measured by results of cone calorimeter test. In case of $H_bFRC$-ACP, the average gas emission amount of CO and $CO_2$ could be decreased down to 25% and 20%, respectively, in comparison with LDPE-ACP. The mechanical properties such as tensile strength, bending strength and adhesion strength of $H_bFRC$-ACP were revealed slightly high values $54N/mm^2$, $152N/mm^2$ and 120N/25mm, respectively, compared with LDPE-ACP. It was confirmed that flame retardancy was improved with the synergy effect because of char formation by M-P and hydrolysis by Mg$(OH)_2$. The result of this study suggest that $H_bFRC$ can be applied for an adequate halogen free flame retardant composite material as a inner core for ACP.

An Analysis of Dynamic Characteristics of RDX Combustion Using Rigorous Modeling (상세 모델링을 통한 RDX 연소 동특성 분석)

  • Kim, Shin-Hyuk;Yeom, Gi-Hwoen;Moon, Il;Chae, Joo-Seung;Kim, Hyeon-Soo;Oh, Min
    • Clean Technology
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    • v.20 no.4
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    • pp.398-405
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    • 2014
  • In the treatment of spent high energetic materials, the issues such as environmental pollution, safety as well as working capacity should be carefully considered and well examined. In this regard, incineration has been recommended as one of the most promising processes for the disposal of such explosives. Due to the fact that high energetic materials encompass various types and their different characteristics, the technology development dealing with various materials is not an easy task. In this study, rigorous modeling and dynamic simulation was carried out to predict dynamic physico-chemical phenomena for research department explosive (RDX). Plug flow reactor was employed to describe the incinerator with 263 elementary reactions and 43 chemical species. Simulation results showed that safe operations can be achieved mainly by controlling the reactor temperature. At 1,200 K, only thermal decomposition (combustion) occurred, whereas increasing temperature to 1,300 K, caused the reaction rates to increase drastically, which led to ignition. The temperature further increased to 3,000 K which was the maximum temperature recorded for the entire process. Case studies for different operating temperatures were also executed and it was concluded that the modeling approach and simulation results will serve as a basis for the effective design and operation of RDX incinerator.

Study on the Polymerization Characteristics of Isoprene through Nitroxide Mediated Controlled/"living" Radical Polymerization Techniques (Nitroxide 매개 리빙라디칼 중합법에 의한 isoprene의 중합특성에 관한 연구)

  • Hong, Sung-Chul
    • Elastomers and Composites
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    • v.44 no.1
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    • pp.55-62
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    • 2009
  • In this study, investigation on the polymerization characteristics of isoprene through nitroxide mediated controlled/"living" radical polymerization techniques was attempted. In the presence of acetol, linear increase of isoprene conversion with time and low polydispersities of the resulting polymers ($M_w/M_n$ < 1.5) were observed, which suggest successful controlled/"living" radical polymerization of isoprene. The microstructure of the resulting polyisoprene was composed of $\sim$ 22% of 3, 4, $\sim$30% of 1, 4-cis and $\sim$ 48% of 1, 4-trans. The optimum polymerization temperature was 145 $^{circ}C$, below which no significant polymerization behavior was observed. Non-cyclic nitroxide, such as di-tert-butyl nitroxide (DTBN) could not mediate the polymerization, whereas cyclic nitroxides (2, 2, 6, 6-tetramethyl-1-peperidine 1-oxyl (TEMPO) and 4-oxo-2, 2, 6, 6-tetramethyl-1-peperidine 1-oxyl (oxoTEMPO)) were successfully employed for the polymerization. However, isoprene dimerization reaction through Diels-Alder process was also observed at the given polymerization condition, which afforded a significant amount of limonene. Isoprene thermal autoinitiation was also possible, which was, however, considered to be not significant under the given polymerization condition.

Preparation and Properties of Phytosphingosine Ascorbate with Retaining Skin Development Effects (피부 활성을 갖는 Phytosphingosine Ascorbate의 합성)

  • Min, Seok-Kee;Jin, Yong-Hoon;Park, Woo-Jung;Eom, Sang-Yong;Kim, Jong-Heon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.30 no.2
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    • pp.167-172
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    • 2004
  • In the human skin, vitamin C (L -ascorbic acid) that is well known as the activated materials has effects that is skin anti-aging and wrinkle repair by giving impetus to collagen biosynthesis and anti-oxidation, and that is the sun screen, a wound recovering, inhibition melanogenesis and so on. In spite of its effects, vitamin C has the defects of the skin stimulation and easily oxidized instability by water, air, heat and light. For solving their matters, many investigation is advanced and its results are synthesized the various vitamin C derivatives. And yet they have not solved the unstable property of vitamin C and were still insufficient for the comparing with the effect of the pure vitamin C itself. In this study, in order to prepare vitamin C derivative of being improved the stability and to apply vitamin C effect in the skin, we prepared new vitamin C derivative, phytosphingosine ascorbate, by using phytosphingosine, one of sphingolipids, which have a distinguished skin affinity. Phytosphingosine ascorbate can be prepared as the ionic bond between amine group (-NH$_2$) of phytosphingosine and hydroxy group (-OH) of vitamin C by way of the relatively simple reaction. So the structure and properties of the synthesized phytosphingosine ascorbate was confirmed the use of elemental analysis (C 58.3 : H 9.3 : N 2.8 : O 29.5), MALDI TOF-MS (Mw=492.58), Ultraviolet spectra (268.5nm), lH NMR, FT-IR spectra, thermal analysis (m.p=l54$^{\circ}C$), HPLC and so on. And we could confirm the anti-bacterial and anti-oxidation effects. Based on these results, we could confirm to prepare a new material that was expected of both effects of vitamin C and phytosphingosine and that is improved properties of vitamin C.

Preparation of Ion Exchange Membranes for Fuel Cell Based on Crosslinked Poly(vinyl alcohol) with Poly(acrylic acid-co-maleic acid)

  • Kim, Dae-Sik;Park, Ho-Bum;Lee, Chang-Hyun;Lee, Young-Moo;Moon, Go-Young;Nam, Sang-Yong;Hwang, Ho-Sang;Yun, Tae-II;Rhim, Ji-Won
    • Macromolecular Research
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    • v.13 no.4
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    • pp.314-320
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    • 2005
  • Crosslinked poly(vinyl alcohol) (PVA) membranes were prepared at various crosslinking temperatures using poly(acrylic acid-co-maleic acid) (PAM) containing different PAM contents. The thermal properties of these PVA/PAM membranes prepared at various reaction temperatures were characterized using differential scanning calorimetry (DSC). The proton conductivity and methanol permeability of PVA/PAM membranes were then investigated as PAM content was varied from 3 to 13 wt%. It was found that the proton and methanol transport were dependent on PAM content in their function both as crosslinking agent and as donor of hydrophilic -COOH groups. Both these properties decreased monotonously with increasing PAM concentration. The proton conductivities of these PVA/PAM membranes were in the range from $10^{-3}\;to\;10^{-2}S/cm$ and the methanol permeabilities from $10^{-7}\;to\;10^{-6}cm^{2}/sec$. In addition, the effect of operating temperature up to $80^{\circ}C$ on ion conductivity was examined for three selected membranes: 7, 9 and 11 wt% PAM membranes. Ion conductivity increased with increasing operating temperature and showed and S/cm at $80^{\circ}C$, respectively. The effects of crosslinking and ionomer group concentration were also examined in terms of water content, ion exchange capacity (IEC), and fixed ion concentration. In addition, the number of water molecules per ionomer site was calculated using both water contents and IEC values. With overall consideration for all the properties measured in this study, $7{\sim}9\;wt%$ PAM membrane prepared at $140^{\circ}C$ exhibited the best performance. These characteristics of PVA/PAM membranes are desirable in applications related to the direct methanol fuel cell (DMFC).

Synthesis and Characterization of Hybrid Nanocomposites of Pd Nanoparticles Containing POSS(Pd-POSS) and Poly(acrylic acid) via Ionic Interactions (실세스키옥세인을 포함한 팔라듐 나노입자와 폴리아크릴산과의 이온결합에 의한 나노복합체 제조 및 특성평가)

  • Jeon, Jong-Hwan;Lim, Jung-Hyurk;Chujo, Yoshiki;Kim, Kyung-Min
    • Polymer(Korea)
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    • v.33 no.6
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    • pp.615-619
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    • 2009
  • Pd-POSS nanoparticles were produced from the reaction of palladium (II) acetate and octa(3-aminopropyl)octasilsesquioxane octahydrochloride (POSS-${NH_3}^+$) in methanol at room temperature. Pd-POSS nanoparticles with a mean diameter of 60-80 nm were the highly ordered spherical aggregates. In contrast, Pd nanoparticles with a size of 4.0 nm were obtained when POSS-${NH_3}^+$ was not introduced. Pd-POSS/PAA nanocomposites of Pd-POSS nanoparticles and poly(acrylic acid) (PAA) were fabricated by utilizing ionic interactions between positively charged Pd-POSS nanoparticles and negatively charged carboxylate groups of PAA. PAA was used as a cross-linker for the preparation of hybrid nanocomposites with the controlled organized structures of Pd-POSS nanoparticles. That is, the self-organization of Pd-POSS nanoparticles was formed into the shape of continuous lines by using PAA as a cross-linker. The composition, structure, surface morphology, and thermal stability of the Pd-POSS/PAA nanocomposites were studied by FE-SEM, AFM, TEM, FT-IR, and TGA.

Preparation and Flame Retardancy of Poly(benzoxazole imide) Having Trifluoromethyl Group in the Main Chain (주사슬에 Trifluoromethyl 그룹을 갖는 Poly(benzoxazole imide)의 제조 및 난연 특성)

  • Yeom, Jin-Seok;Choi, Jae-Kon;Lee, Chang-Hoon
    • Elastomers and Composites
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    • v.47 no.4
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    • pp.355-363
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    • 2012
  • A series of poly(hydroxyamide)s (PHAs) having trifluoromethyl group were prepared by direct polycondensation of aromatic diimide-dicarboxylic acids with 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane by thionyl chloride and triethyl amine in N-methyl-2-pyrrolidinone (NMP). The PHAs exhibited inherent viscosity in the range of 0.54-0.96 dL/g at $35^{\circ}C$ in DMAc solution. All PHAs were readily soluble in a variety of organic solvents, whereas the polybenzoxazoles (PBOs) were quite insoluble except partially soluble in sulfuric acid. PHAs were converted to PBOs by thermal cycling reaction with heat of endotherm. The maximum weight loss temperature of the PHAs occurred in the range of $559-567^{\circ}C$. The PBOs showed relatively high char yields in the range of 47-59%. Pyrolysis Combustion Flow Calorimeter (PCFC) results of the PBOs showed 12-19 W/g heat release rate (HRR), and 2.7-3.6 kJ/g total heat release (total HR). The HRR of PBO 1 showed the lowest value of 12 W/g, which was 37% lower than that of PBO 3 (19 W/g).

Comparison of Biochemical Characterization of Korean and Chinese Mung Bean Lectin (한국산 녹두와 중국산 녹두에 있어서 Lectin의 생화학적 특성 비교)

  • Roh, Kwang Soo
    • Journal of Life Science
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    • v.24 no.6
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    • pp.603-611
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    • 2014
  • The lectins were separated from Korean and Chinese mung bean seeds finally via chromatography using Sephadex G-100 and their biochemical features were studied and compared. They showed no hemagglutination with human red blood cells regardless of trypsin treatment and showed hemagglutination with only trypsin treated rabbit red blood cells. The molecular weights of two lectins were identified as 54 kDa and 28 kDa by SDS-PAGE. It was found that while the optimal reaction temperature of the lectin from Korean mung bean was $60^{\circ}C$, that of the lectin from Chinese mung bean seeds was $50^{\circ}C$. It was found also that the most thermal stable temperature of the seed lectin from Korean mung bean seeds was $50^{\circ}C$ and the lectin from Chinese mung bean was $40-50^{\circ}C$. The lectin from Korean mung bean seeds showed the highest activity at pH 3.2 and the lectin from Chinese mung bean showed the highest activity at pH 6.2. It was identified that when treating a denaturant, thiourea and guanidine-HCl resulted in no hemagglutination, so they induced denaturalization. It was identified also that there was no hemagglutination with urea, so it did not induced denaturalization. They showed no septicity to 6 types of carbohydrates including D-glucose. In addition, the lectins from the two mung bean seed had specificity to metal ions.

Pervaporation of Fluoroethano1 and Methacrylic Acid Aqueous Solution Through New Acid-resistant Poly(vinyl alcohol) Membranes (새로운 내산성 PVA가교막을 이용한 불화에탄을 수용액과 메타크릴산 수용액의 투과증발분리)

  • Lee Soo-Bok;Ahn Sang-Man;Chang Bong-Jun;Kim Jeong-Hoon;Lee Yong-Taek
    • Membrane Journal
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    • v.15 no.3
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    • pp.206-212
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    • 2005
  • Acid-resistant poly(vinyl alcohol) (PVA) membranes connected with ethylene and ether groups were prepared via a thermal crosslinking reaction by varying the ratio of PVA to ethylene glycol diglycidyl ether (EGDE). The crosslinked membranes were characterized using FT-IR and swelling tests, respectively. Pervaporation behaviors with the PVA membranes were investigated for aqueous TFEA (2,2,2-trifluoroethanol) as a function of EGDE content and operating temperature. The pervaporation properties far MA (methacrylic acid)/water mixture were also carried out with the optimized PVA membrane. The PVA membranes prepared with EGDE showed more excellent acid-resistance than those crosslinked with gluaraldehyde. The membranes showed high permeation fluxes of 0.1 and $0.3\;km^2h$ and high separation factors of 100 and 900 in the $96\;wt\%$ TFEA and MA aqueous fred mixtures at high temperature above $80^{\circ}C$, respectively. These confirmed theses membranes could be used in esterification membrane reactor process for the production of 2,2,2-trifluoroethylmetacrylate (TFEMA).