• Title/Summary/Keyword: char formation

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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.

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.

A Complete, Reductive Depolymerization of Concentrated Sulfuric Acid Hydrolysis Lignin into a High Calorific Bio-oil using Supercritical Ethanol

  • Riaz, Asim;Kim, Jaehoon
    • KEPCO Journal on Electric Power and Energy
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    • v.2 no.3
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    • pp.447-452
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    • 2016
  • It is imperative to develop an effective pathway to depolymerize lignin into liquid fuel that can be used as a bioheavy oil. Lignin can be converted into liquid products either by a solvent-free thermal cracking in the absence air, or thermo-chemical degradation in the presence of suitable solvents and chemicals. Here we show that the solvent-assisted liquefaction has produced promising results in the presence of metal-based catalysts. The supercritical ethanol is an efficient liquefaction solvent, which not only provides better solubility to lignin, but also scavenges the intermediate species. The concentrated sulfuric acid hydrolysis lignin (CSAHL) was completely liquefied in the presence of solid catalysts (Ni, Pd and Ru) with no char formation. The effective deoxy-liquefaction nature associated with scEtOH with aid hydrodeoxygenation catalysts, resulted in significant reduction in oxygen-to-carbon (O/C) molar ratio up to 61%. The decrease in oxygen content and increase in carbon and hydrogen contents increased the calorific value bio-oil, with higher heating value (HHV) of $34.6MJ{\cdot}Kg^{-1}$. The overall process is energetically efficient with 129.8% energy recovery (ER) and 70.8% energy efficiency (EE). The GC-TOF/MS analysis of bio-oil shows that the bio-oil mainly consists of monomeric species such as phenols, esters, furans, alcohols, and traces of aliphatic hydrocarbons. The bio-oil produced has better flow properties, low molecular weight, and high aromaticity.

Influence of Pyrolysis Conditions and Type of Resin on the Porosity of Activated Carbon Obtained From Phenolic Resins

  • Agarwal, Damyanti;Lal, Darshan;TripathiN, V.S.;Mathur, G.N.
    • Carbon letters
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    • v.4 no.2
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    • pp.57-63
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    • 2003
  • In polymer precursor based activated carbon, the structure of starting material is likely to have profound effect on the surface properties of end product. To investigate this aspect phenolic resins of different types were prepared using phenol, mcresol and formaldehyde as reactants and $Et_3N$ and $NH_4OH$ as catalyst. Out of these resins two resol resins PFR1 and CFR1 (prepared in excess of formaldehyde using $Et_3N$ as catalyst in the basic pH range) were used as raw materials for the preparation of activated carbons by both chemical and physical activation methods. In chemical activation process both the resins gave activated carbons with high surface areas i.e. 2384 and 2895 $m^2/g$, but pore size distribution in PFR1 resin calculated from Horvath-Kawazoe method, contributes mainly in micropore range i.e. 84.1~88.7 volume percent of pores was covered by micropores. Whereas CFR1 resin when activated with KOH for 2h time, a considerable amount (32.8%) of mesopores was introduced in activated carbon prepared. Physical activation with $CO_2$ leads to the formation of activated carbon with a wide range of surface area (503~1119 $m^2/g$) with both of these resins. The maximum pore volume percentage was obtained in 3-20 ${\AA}$ region by physical activation method.

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Hydrocarbon Synthesis of Waste Lignocellulosics by Liquefaction Reaction of Thermochemical Deoxyhdrogenolysis Method (II) (목질폐재(木質廢材)의 열(熱)-화학적(化學的) 탈(脫)산소-수소첨가반응(환원반응)에 의한 액화(液化)탄화수소의 합성 (II))

  • Lee, Byung-Guen
    • Journal of the Korean Wood Science and Technology
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    • v.19 no.4
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    • pp.80-84
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    • 1991
  • Lignocellulosic biomass including acetosolv ricestraw and spruce lignin were liquefied and converted into liquid hydrocarbons by catalytic hydroliquefaction reaction. These experimental works were carried out in 1-liter-capacity autoclave using 50% tetralin and m-cresol solution respectively as soluble solvent and Ni. Pd. Fe and red mud as catalyst. $H_2$ gas was supplied into the reactor for escaltion of deoxhydroenolysis reaction. Catalyst concentrations were 1 % of raw material based on weight. The ratio between raw materials and soluble solvent are 1g and 10cc. The reaction conditions are 400-$700^{\circ}C$ of reaction temperature, 10-50 atms of reaction pressure. The highest yield of hydrocarbon, so called "product oil" showed 32% and 5.5% of lowest char formation when red mud was used as catalyst. The product oil yields from those of other catalysts were in the range of 20-29%. The influence of different initial hydrogen pressures was examined in the range d 30-50 atms. A minimum pressure of 35 atms was necessary to obtain a complete recovery of souble solvent for recycling.

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Cross-section micrography of burning pulverized coal particles (연소중 미분탄의 단면관측)

  • 한재현;최상민
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.13 no.4
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    • pp.717-725
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    • 1989
  • An experimental investigation on the combustion behavior of pulverized coal particles was performed using the cross-section micrography techniques while sample coal particles were collected in-situ from the flow reactor. The coal particles were representative of pulverized bituminous coal undergoing a raped pyrolysis and combustion, however, quenched at the time when the particles were deposited onto a sample plate. The internal structure of coal was observed to change as deposited. Upon injection into a flow reactor, bituminous coal particles showed many holes which represented internal pore formation during the pyrolysis. The relative portion of the remaining matrix of coal was decreasing as the residence time progressed. This direct observation of cross-section of burning particles enabled better understanding of the coal combustion behavior.

Solid-State $^{51}V$ NMR and Infrared Spectroscopic Study of Vanadium Oxide Supported on $TiO_2-ZrO_2$

  • Park, Eun Hui;Lee, Man Ho;Son, Jong Rak
    • Bulletin of the Korean Chemical Society
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    • v.21 no.9
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    • pp.913-918
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    • 2000
  • Vanadium oxide catalyst supported on TiO2-ZrO2 has been prepared by adding Ti(OH)4-Zr(OH)4 powder to an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The char-acterization ofthe prepared catalysts was performed using solid-state 51V NMR and FTIR.In thecase ofcalci-nation temperature at 773 K, vanadium oxide was in a highly dispersed state for the samples containing low loading V2O5 below 25 wt %, but for samplescontaining high loading V2O5 equal to or above 25 wt %, vana-dium oxidewas well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2.The ZrV2O7 compound was formed through the reactionof V2O5 and ZrO2 at 773-973 K, where-as the V3Ti6O17 compound was formedthrough the reaction of V2O5 and TiO2 at 973-1073 K. The V3Ti6O17 compound decomposed to V2O5 and TiO2 at 1173 K, which were confirmed by FTIR and 51V NMR.

Flame Retardant Properties of Cotton Fiber with Phosphoric/citric Acid Catalysts and TiO2 (인산/구연산 복합 산촉매 및 이산화티타늄을 적용한 면섬유의 난연 특성)

  • Yang, Heejin;Kim, Samsoo;Lee, Sangoh;Lee, Jaewoong
    • Textile Coloration and Finishing
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    • v.33 no.4
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    • pp.238-249
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    • 2021
  • In this study, the effect on flame retardancy and various physical properties when TiO2 was added with a citric acid/phosphate complex acid catalyst together with Pyrovatex CP new (N-methylol dimethylphosphonopropionamide), a phosphorus-based flame retardant, was studied on cotton fibers. SEM-EDS analysis was performed to confirm the surface characteristics and surface element analysis of the flame-retardant treated cotton fibers, and a vertical carbonization test was performed to confirm the char formation capability and flame retardancy according to the phosphoric acid ratio. By comparing the LOI index before and after washing 10 times, the washing durability of the flame retardant solution containing the phosphoric acid catalyst and TiO2 was tested by LOI index after ten washing cycles. In addition, the influence of the flame-retardant processing on the physical properties were compared including thermogravimetric analysis (TGA), tear strength and whiteness.

Ionic Liquid as a Solvent and the Long-Term Separation Performance in a Polymer/Silver Salt Complex Membrane

  • Kang, Sang-Wook;Char, Kook-Heon;Kim, Jong-Hak;Kang, Yong-Soo
    • Macromolecular Research
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    • v.15 no.2
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    • pp.167-172
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    • 2007
  • The reduction behavior of silver ions to silver nanoparticles is an important topic in polymer/silver salt complex membranes to facilitate olefin transport, as this has a significant effect on the long-term performance stability of the membrane. In this study, the effects ofthe solvent type on the formation of silver nanoparticles, as well as the long-term membrane performance of a solid polymer/silver salt complex membrane were investigated. These effects were assessed for solid complexes of poly(N-vinyl pyrrolidone) $(PVP)/AgBF_4$, using either an ionic liquid (IL), acetonitrile (ACN) or water as the solvent for the membrane preparation. The membrane performance test showed that long-term stability was strongly dependent on the solvent type, which increased in the following order: IL > ACN >> water. The formation of silver nanoparticles was more favorable with the solvent type in the reverse order, as supported by UV-visible spectroscopy. The poor stability of the $(PVP)/AgBF_4$ membrane when water was used as the solvent might have been due to the small amount of water present in the silver-polymer complex membranes actively participating in the reduction reaction of the silver ions into silver nanoparticles. Conversely, the higher stability of the $(PVP)/AgBF_4$, membrane when an IL was used as the solvent was attributable to the cooperative coordination of silver ions with the IL, as well as with the polymer matrix, as confirmed by FTIR spectroscopy.

Selective Production of Monomeric Phenols from Lignin via Two-step Catalytic Cracking Process (2단계 촉매 분해공정을 이용한 리그닌 유래 선택적 페놀화합물 생산)

  • Kim, Jae-Young;Heo, Sujung;Park, Shin Young;Choi, In-Gyu;Choi, Joon Weon
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.3
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    • pp.278-287
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    • 2017
  • In this study, lignin was efficiently degraded via two-step catalytic cracking process and lignin-oil, char, and gas was produced as lignin degraded products. Three kinds of catalysts (MgO, CaO, and Pt/C) were used in first catalytic cracking step and the highest lignin-oil yield (76.2 wt%) was obtained in Pt/C catalyst with the smallest char formation (4.1 wt%). GC-MS/FID analysis revealed that 18 kinds of monomeric phenols existed in lignin-oil and sum of them was the highest in Pt/C condition (97.8 mg/g lignin). Meanwhile, relatively lower yield of monomeric phenols was produced in MgO and CaO condition because of their absorption on catalysts. Lignin-oil produced over Pt/C was introduced to second catalytic cracking process with porous Pd/activated carbon aerogel catalyst. From this process, four kinds of monomeric phenols such as 4-ethylguaiacol, 4-propylguaiacol, 4-ethylsyringol, 4-propylsyringol were selectively produced at 0.89 - 1.82 wt% level.