• Title/Summary/Keyword: decomposition temperature

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Synthesis Characteristics of ZnO Powder from Precursors Composed of Nitrate-Citrate Compounds (Nitrate-Citrate 혼합 전구체로부터 ZnO 입자의 합성반응 특성)

  • Yang, Si Woo;Lee, Seung Ho;Lim, Dae Ho;Yoo, Dong Jun;Kang, Yong
    • Korean Chemical Engineering Research
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    • v.54 no.3
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    • pp.299-304
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    • 2016
  • Characteristics of self-propagating reaction for the preparation of ZnO powder from precursors composed of nitrate and citrate compounds were examined. The ratio of C/N was maintained in range of 0.7~0.8 to initiate the self-propagating reaction between the reducing citrate and oxidizing nitrate groups. The samples were decomposed thermally by using TGA. The sudden decomposition occurred in the range of X > 0.5 in a very short time with a very sharp decrease of mass, indicating that the self-propagating reaction would occur. Friedman, Ozawa-Flynn-Wall and Vyazovkin methods were employed to predict the activation energy, reaction order and frequency factor of the reaction rate in the rate determining step of X < 0.5 range. The activation energy increased with increasing fractional conversion in the range of 46~130 (kJ/min). The reaction order decreased in the range of 2.9~0.9, while the frequency factor increased in the range of 85~278 ($min^{-1}$), respectively, with increasing the rate of temperature increase.

Synthesis of Polyurethane Foam/Organonanoclay/Phosphates Composites and its Characterization (폴리우레탄폼/유기나노점토/포스페이트 복합체의 합성과 그 특성)

  • Park, Kyeong-Kyu;Lee, Sang-Ho
    • Elastomers and Composites
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    • v.46 no.4
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    • pp.343-351
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    • 2011
  • We prepared polyurethane foam/cloisite30B/phosphates composites and characterized their rise time, density, cell morphology, and thermal properties. The composites were synthesized with polyadipatediol-cloisite30B composite (f=2.0), polyether-polyol (f=4.6), polymeric 4,4-diphenyl methane diisocyanate (f=2.5), and D-580 (phenyl polyoxyalkenyl phosphate). As a blowing agent, cyclopentane and distilled water were used at various concentrations of D-580 from 0 to 2.81 wt%. The rise times of PUF/Closite30B/Phosphate composites blown with distilled water were faster than those blown with cyclopentane by 30%. The composites blown with cyclopentane had spherical-shape cells and the cell diameter was decreased with increasing D-580 wt%. While $T_g$ of the composites blown with cyclopentane linearly decreased with increasing the D-580 content, the $T_g$ of the composites blown with distilled water increased with the D-580 content. All PUF/Closite30B/Phosphate composites began to decompose from $250^{\circ}C$. The composites blown with cyclopentane showed the second thermal decomposition at temperatures higher than $500^{\circ}C$. The thermal stability of all composites increased with the D-580 content. The effect of D-580 on the thermal stability of the composites was measured higher at the composites blown with distilled water.

Corrosion Characteristics of Fe-Si, Ni-Ti and Ni Alloy in Sulfuric Acid Environments (황산 환경에서 Fe-Si, Ni-Ti계 및 Ni 합금의 내부식성 특성)

  • Kwon, Hyuk-Chul;Kim, Dong-Jin;Kim, Hong-Pyo;Park, Ji-Yeon;Hong, Seong-Deok
    • Korean Journal of Materials Research
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    • v.21 no.1
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    • pp.1-7
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    • 2011
  • Methods of producing hydrogen include steam reforming, electrochemical decomposition of water, and the SI process. Among these methods, the Sulfur iodine process is one of the most promising processes for hydrogen production. The thermochemical sulfur-iodine (SI) process uses heat from a high-temperature-gas nuclear reactor to produce $H_2$ gas; this process is known for its production of clean energy as it does not emit $CO_2$ from water. But the SI-process takes place in an extremely corrosive environment for the materials. To endure SI environments, the materials for the SI environment will have to have strong corrosion resistance. This work studies the corrosion resistances of the Fe-Si, Ni-Ti and Ni Alloys, which are tested in SI-process environments. Among the SI-process environments, the conditions of boiling sulfuric acid and decomposed sulfuric acid are selected in this study. Before testing in boiling sulfuric acid environments, the specimens of Fe-4.5Si, Fe-6Si, Ni-4.5Si, Ni-Ti-Si-Nb and Ni-Ti-Si-Nb-B are previously given heat treatment at $1000^{\circ}C$ for 48 hrs. The reason for this heat treatment is that those specimens have a passive film on the surface. The specimens are immersed for 3~14 days in 98wt% boiling sulfuric acid. Corrosion rates are measured by using the weight change after immersion. The corrosion rates of the Fe-6Si and Ni-Ti-Si-Nb-B are found to decrease as the time passes. The corrosion rates of Fe-6si and Ni-Ti-Si-Nb-B are measured at 0.056 mm/yr and 0.16 mm/yr, respectively. Hastelloy-X, Alloy 617, Alloy 800H and Haynes 230 are tested in the decomposed sulfuric acid for one day. Alloy 800H was found to show the best corrosion resistance among the materials. The corrosion rate of Alloy 800H is measured at -0.35 mm/yr. In these results, the corrosion resistance of materials depends on the stability of the oxide film formed on the surface. After testing in boiling sulfuric acid and in decomposed sulfuric acid environments, the surfaces and compositions of specimens are analyzed by SEM and EDX.

Synthesis and characterization of hydrophobic and hydrophilic cellulose derivative by esterification (친수성과 소수성을 동시에 가지는 아세틸화 셀룰로스 에테르의 합성 및 특성 평가)

  • Kim, Taehong;Lee, Sangku;Son, Byunghee;Paik, Hyun-Jjong;Yoon, Sanghyeon;Lee, Heesoo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.1
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    • pp.31-36
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    • 2013
  • Acetylated Cellulose Ether (ACE), cellulose-based amphiphilic polymer with hydrophilic and hydrophobic, was synthesized and investigated in terms of its solubility and wettability for organic solvents and water. Acetyl group was substituted to the cellulose ether in a hydrophilic polymer by esterification. As a result of FT-IR, the peak corresponding to the hydroxyl group decreased and carboxyl acid peak increased with increasing reaction time and temperature, which signified the increase in the degree of acetylation of the ACE. There were similar thermal decomposition behaviors before and after esterification reaction until $800^{\circ}C$ so that the reaction occurred without significant structural changes of cellulose backbones. The solubility parameter of the ACE had a range of 18.5~26.4, and its viscosity and turbidity were controlled according to the solubility parameter of organic solvents. The ACE showed the hydrophilicity because the contact angle of the ACE was higher than the cellulose ether. These results confirmed that the ACE had the hydrophobicity and hydrophilicity due to the ether which was glucosidic bonding between the glucose units and un-reacted hydroxyl functional groups in the ACE.

Characterization of Poly(methyl methacrylate)-tin (IV) Chloride Blend by TG-DTG-DTA, IR and Pyrolysis-GC-MS Techniques

  • Arshad, Muhammad;Masud, Khalid;Arif, Muhammad;Rehman, Saeed-Ur;Saeed, Aamer;Zaidi, Jamshed Hussain
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3295-3305
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    • 2011
  • Thermal behavior of poly (methyl methacrylate) was analyzed in the presence of tin (IV) chloride. Five different proportions - polymer to additive - were selected for casting films from common solvent. TG, DTG and DTA were employed to monitor thermal degradation of the systems. IR and py-GC-MS helped identify the decomposition products. The blends start degrading at a temperature lower than that of the neat polymer and higher than that of the pure additive. Complex formation between tin of additive and carbonyl oxygen (pendent groups of MMA units) was noticed in the films soon after the mixing of the components in the blends. The samples were also heated at three different temperatures to determine the composition of residues left after the expulsion of volatiles. The polymer, blends and additive exhibited a one step, two-step and three-step degradation, respectively. $T_0$ is highest for the polymer, lowest for the additive and is either $60^{\circ}C$ or $70^{\circ}C$ for the blends. The amount of residue increases down the series [moving from blend-1 (minimum additive concentration) to blend-5 (maximum additive concentration)]. For blend-1, it is 7% of the original mass whereas it is 16% for blend-5. $T_{max}$ also goes up as the concentration of additive in the blends is elevated. The complexation appears to be the cause of observed stabilization. Some new products of degradation were noted apart from those reported earlier. These included methanol, isobutyric acid, acid chloride, etc. Molecular-level mixing of the constituents and "positioning effect" of the additive may have brought about the formation of new compounds. Routes are proposed for the appearance of these substances. Horizontal burning tests were also conducted on polymer and blends and the results are discussed. Activation energies and reaction orders were calculated. Activation energy is highest for the polymer, i.e., 138.9 Kcal/mol while the range for blends is from 51 to 39 Kcal/mol. Stability zones are highlighted for the blends. The interaction between the blended parts seems to be chemical in nature.

Uranyl Peroxide Compound Preparation from the Filtrate for Nuclear Fuel Powder Production Process (핵연료분말 제조공정 여액으로부터 Uranyl-peroxide 화합물의 제조)

  • Jeong, Kyung-Chai;Kim, Tae-Joon;Choi, Jong-Hyun;Park, Jin-Ho;Hwang, Seong-Tae
    • Applied Chemistry for Engineering
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    • v.8 no.3
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    • pp.430-437
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    • 1997
  • Uranyl-peroxide compound was prepared by the reaction of excess hydrogen peroxide solution and trace uranium in filtrate from nuclear fuel conversion plant. The $CO_3{^{2-}}$ in filtrate was removed first by heating more than $98^{\circ}C$, because uranyl-peroxide compound could not be precipitated by $CO_3{^{2-}}$ remaining in filtrate. The optimum condition for uranyl-peroxide compound was ageing for 1 hr after controling the pH with $NH_3$ gas and adding the excess $H_2O_2$ of 10ml/lit.-filtrate. Uranium concentration in the filtrate was appeared to 3 ppm after the precipitation of uranyl-peroxide compound, and the chemical composition of this compound was analyzed to $UO_4{\cdot}2NH_4F$ with FT-IR, X-ray diffractometry, TG and chemical analysis. Also, this fine particle, about $1{\sim}2{\mu}m$, could be grown up to $4{\mu}m$ at pH 9.5 and $60^{\circ}C$. The separation efficiency of precipitate from mother liquor was increased with increase of pH and reaction temperature. Otherwise, the crystal form of this particle showed octahedral by SEM and XRD, and $U_3O_8$ powder was obtained by thermal decomposition at $650^{\circ}C$ in air atmosphere.

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Roles of Acid-Base Surface Interaction on Thermal and Mechanical Interfacial Behaviors of SiC/PMMA Nanocomposites (산-염기 표면반응이 탄화규소/PMMA 나노복합재료의 열적·기계적 계면특성에 미치는 영향)

  • Park, Soo-Jin;Oh, Jin-Seok
    • Korean Chemical Engineering Research
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    • v.43 no.5
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    • pp.632-636
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    • 2005
  • In this work, the effect of chemical treatments on surface properties of SiC was investigated in thermal and mechanical interfacial behaviors of SiC/PMMA nanocomposites. The acid/base value, contact angles, and FT-IR analysis were performed for the study of surface characteristics of the SiC studied. The thermal stabilities of the SiC/PMMA nanocomposites were investigated by thermogravimetric analysis (TGA). Also the mechanical interfacial properties of the composites were studied in critical stress intensity factor ($K_{IC}$) and critical strain energy release rate ($G_{IC}$) measurements. As a result, the acidically treated SiC (A-SiC) had higher acid value than that of untreated SiC (V-SiC) or basically treated SiC (B-SiC). The acidic solution treatment led to an increase in surface free energy of the SiC, mainly due to the increase of its specific component. Thermal and mechanical interfacial properties of the SiC/PMMA nanocomposites, including initial decomposition temperature (IDT), $K_{IC}$, and $G_{IC}$ had been improved in the acidic treatment on SiC. This was due to the improvement in the interfacial bonding strength, resulting from the acid-base interfacial interactions between the fillers and polymeric matrix.

The Distribution of phosphorus in the Gomso Bay Tidal Flat (곰소만 조간대에서 인의 시공간적 분포)

  • 양재삼;김영태
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.7 no.3
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    • pp.171-180
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    • 2002
  • The temporal and spatial distributions of phosphorus have been investigated in the Gomso Bay, Korea. TP, PIP, TOP and DIP in sediment were found 548.8mg P kg$^{-1}$ , 426.1mg P kg$^{-1}$ , 122.6mg P kg$^{-1}$ , and 0.217mg P kg$^{-1}$ , respectively with a decreasing order of PIP>TOP>DIP. Any temporal or spatial trend has not been found on the distribution of TP in the sediment, except the high TP values near the mouth of Julpo-chun. We found seasonal patterns high TOP(28.90% of TP) and low TIP(71.10% of TP) in August, but low TOP(15.63% of TP) and high TIP(84.38% of TP) in November. There were three times higher DIP concentration in August than in November. Such case is probably not only due to the enhanced supply of DIP directly from the decomposition of organic matter from overlying water in summer, but also the released phosphate from the adsorbed particulate matter such as PIP under the low pH and Eh conditions at the subsurface layers of the sediment induced by the active microbial respiration of increased organic materials in summer. Primarily, the source of phosphorous from municipal sewage strongly influenced the early stage of the distribution of all the phosphorous in the Gomso tidal flat. Notwithstanding, through the processes of diagenesis in sediment, water temperature and organic contents probably functioned as the key parameters to control the temporal distributions of TOP, TIP and DIP in the Gomso tidal flat.

Synthesis and Characterization of Guanidine Dinitramide Crystal (구아니딘 디나이트라아마이드 결정의 합성 및 특성 분석)

  • Kim, Wooram;Kwon, Younja;Jo, Youngmin;Park, Youngchul
    • Applied Chemistry for Engineering
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    • v.26 no.6
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    • pp.737-742
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    • 2015
  • An environmentally favorable solid oxidizer, guanidine dinitramide ($H_2C(NH_2)NH_2N(NO_2)_2$), with high purity and synthesis yield was prepared using guanidine carbonate ($NH_2C(=NH)NH_2{\cdot}1/2H_2CO_3$). Two different crystalline forms (${\alpha}$-form and ${\beta}$-form) were obtained depending on the solvent used and synthesis process. Despite of the same chemical composition, Raman-IR and TGA-DSC revealed that different structures existed between them. In particular, the thermal analysis showed the exothermic temperature of ${\alpha}$-form at $155.7^{\circ}C$ while $191.6^{\circ}C$ for ${\beta}$-form. The caloric value of ${\alpha}$-form was 536.4 J/g which was 2.5 times larger than that of ${\beta}$-form, 1310 J/g. In addition, ${\alpha}$-form was steeply decomposed with one-step variation, but ${\beta}$-form followed a two-step thermal decomposition pattern.

Life Time Prediction and Physical Properties of Chloroprene Rubber Aged by Seawater (클로로프렌 고무의 해수에 의한 물성 변화 및 노화 수명 예측)

  • Lee, Chan Koo;Yun, Ju Ho;Kim, Il;Shim, Sang Eun
    • Elastomers and Composites
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    • v.47 no.1
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    • pp.9-17
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    • 2012
  • Herein, life time prediction based on the deterioration of physical properties of chloroprene rubber (CR)aged by heat and seawater was performed. CR samples were experienced an accelerated test at $80^{\circ}C$, $100^{\circ}C$, $120^{\circ}C$ for heat aging, and $40^{\circ}C$, $60^{\circ}C$, $80^{\circ}C$ for seawater aging for 20,000 hrs. The change in tensile strength, maximum elongation,hardness was measured. As a result, the decrease in elongation was a major factor causing failure. The life time estimated using an Arrhenius model was 125 years at $23^{\circ}C$ for thermal aging and 9 years at $23^{\circ}C$ for seawater aging. SEM and elemental analysis reveal that cracks were generated and the content of oxygen was increased for CR agined by seawater. FT-IR spectrum shows the new C-O and C = O bonds were generated by the chemical reaction with seawater. Also, the glass transtion temperature was increased and the thermal decomposition was decreased by seawater aging.