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Cover1-
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小嶋 勝衛
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1-4
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佐藤 俊宏, 赤沢 貴博, 高橋 智, 貝原 巳樹雄
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5-6
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It was found that principal component analysis was a potent method for classifying coals. By selecting appropriate coals and their characterized parameters, we could make a rational classification system of coals in the world.
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沖 裕壮, 犬丸 淳, 二宮 善彦
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7-10
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The computer controlled scanning microscopy (CCSEM) is expected as effective analysis tool for minerals in coal. But the effect of analytical condition on the error of obtained data is not clarified well. In this report, relations between analytical conditions, such as threshold for particle recognition, and measurement time for EDS, was considered.
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二宮 善彦, 水野 敏之, 沖 裕壮, 桑原 隆, 山下 亨
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11-14
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The computer controlled scanning electron microscopy (CCSEM) method for quantitative coal mineral analysis was developed. Standard samples such as quartz, kaolinite, calcite, pyrite, mixed these minerals and Hunter Valley coal were measured with four measurement organization to confirm the standardization of measuring. Mineral contents and particle diameter distributions corresponded well with these organizations.
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高橋 義和, 片桐 元, 島根 幸朗, 吉澤 徳子, 丸山 勝久, 山田 能生, 原田 道昭
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15-18
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The X-ray diffraction technique proposed by Hirsh are very useful for characterization of graphite structures in coal. The technique uses Fourier transforms of (002) diffraction peaks. For standardization and unification, optimum conditions for measurements, such as slits and sampling steps, were determined and the Hirsh formulas were coded for computation. It was found that the same results were given using some different apparatuses
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島根 幸朗, 高橋 義和, 片桐 元, 吉澤 徳子, 丸山 勝久, 山田 能生, 原田 道昭
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19-22
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X-ray diffraction (XRD) analysis provides the information on carbon structure in coal. We have developed a standardized procedure to obtain some structural parameters from the XRD profiles, i.e., average number of layer stacking, layer distance and a ratio of stacking layers in coal. The difference between the data collected according to this procedure at three different research institutes was evaluated statistically. It was found that coals with grown layer stacking had higher ordered layer structure, but that this ordering had the limit.
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足立 幸弘, 菅原 均, 小川 仁, 山田 能生
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23-26
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Bituminous, subbituminous and weathered subbituminous coals were used to elucidate the mechanism of spontaneous ignition of coal. These coals showed the different ignition behavior in contact with air at 50℃. Thus the change of radical concentration with the reaction of oxygen was monitored by in situ ESR. As result it was found that the initial exothermal reactions of the coal in air correlate with the occurrence of the additional radicals on the coal surface.
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三輪 優子, 片桐 元, 原田 道昭
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27-30
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Vespel spinning module has appreciable ^<13>C background signals in DD/MAS spectra. This background can be almost completely suppressed using composite pulse sequences. We have investigated the quantitative reliability of background suppression technique in solid state NMR measurement.
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野村 正勝
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31-36
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佐藤 芳樹, 小寺 洋一, 山口 宏, 辰元 克充
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p.
37-40
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Liquid-phase cracking of low rank coal (Buckskin, Taiheiyo and Yallourn coals) at 350〜440℃ under 2MPa of initial nitrogen atmosphere has been studied to produce upgraded coal with high heating value, reducing the tendency to spontaneous ignition. Liquid-phase cracking of Buckskin (USA subbituminous) coal using iron oxide catalyst in the presence of t-decalin at 440℃ gave 11.6wt% of gas, 8.9wt% of oil and 74.0wt% of upgraded coal with small amount of water. Gaseous product consisted of mainly carbon dioxide (62wt%) and methane. Heating value of the upgraded coal increased to 7,440kcal/kg, as compared with 4,610kcal/kg of untreated coal and the behavior of spontaneous ignition was greatly improved by the liquid-phase cracking.
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吉田 貴紘, 飯野 雅, 鷹觜 利公, 加藤 健次
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p.
41-44
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Temperature-variable dynamic viscoelastic measurement was applied to residues of a coking coal after extraction. Tanδ, which is the ratio of viscous modulus (G") to elastic modulus (G') and can be an useful parameter of fluidity of sample, gave the highest for all residues, whose fluidities were not observed by a Gieseler plastometer. Maximum tanδ decreased in the low extraction yield ranges, suggesting that low molecular weight components are essential to occur coal softening.
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則永 行庸, 飯野 雅
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p.
45-48
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Viscoelastic properties of the pelletized Upper Freeport coal and its extracts were characterized by means of controlled stress oscillatory rheometry. The measured modulus of rigidity was resolved into storage and loss components, as a function of temperature and oscillation frequency. Although the time-temperature superposition procedures were apparently allowed to construct the master curves reduced to 643K, the temperature dependencies of the shift factor can never explained by WLF equation. Arrhenius type plots of the shift factors shows that the activation energy is temperature-dependent.
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渡辺 泉, 坂西 欣也, 持田 勲
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p.
49-52
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Changes in coal aggregate structure were analyzed by temperature-variable XRD during heating and solvent swelling. The heat treatment below 400℃ intensified the diffraction around 20° for lower ranked coals of Beulah Zap and Wyodak, while the diffraction around 26° was weakened. In contrast, the heating above 450℃ intensified significantly the diffraction around 26° with rapid decrease in the peak intensity at 20°. The swelling of the coals were found enhanced by the heat treatment around 350℃, reflecting the change in the XRD patterns. The changes in coal aggregate structure are discussed based on the XRD profiles during heating and solvent swelling.
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則永 行庸, 飯野 雅
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p.
53-56
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Blind Canyon coal was swollen by deuterate pyridine and was subjected to ^1H NMR relaxation measurements. The effect of solvent-to-coal mass ratio (S/C) on the relaxation characteristics was examined. The fractional amount of mobile hydrogen yielding the exponential decay,f_<MH>, was increased up to 0.5 with increase in S/C. However, f_<MH> kept almost constant value above S/C=2.24, indicating that there exist the solvent impenetrable regions in the swollen coal even at S/C=4.72. Although there exist at least two distinct structural regions in the swollen coals based on the transverse relaxation characteristics, the measured longitudinal relaxation was best characterized by a single component as spin diffusion is rapid in the swollen coals. The dynamics of spin diffusion were revealed using a partially modified Goldman-Shen pulse sequence and analyzed by a simple mathematical model of a two phase system. The interdomain spacing, d, was estimated based on the diffusive path length for each spatial dimension. The d value evaluated under one-dimension was 15nm and agreed with d determined by small angle neutron scattering, suggesting that the domain shape is sheet.
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国谷 昌浩, 則永 行庸, 飯野 雅
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p.
57-60
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Pyridine soluble portions of Upper Freeport (UF) and Illinois No. 6 (IL) coals were mixed with N-methyl-2-pyrrolidinone (NMP). Annealings of the mixtures at 353K could produce stable gelly materials. Viscoelastic properties of gel were characterized by means of controlled stress oscillatory rheometory at temperatures between 223 and 273K. The measured modulus of rigidity was resolved into storage and loss components, as a function of temperature and oscillation frequency. Time-temperature superposition procedures were apparently allowed to construct the master curves reduced to 243K. It was found that the moduli of the gel formed from IL are larger than that from UF at equivalent temperatures and frequencies. IR spectra of the gels indicate that the hydrogen bonding interaction between the extracts and NMP plays a key role on the stabilities of the gels.
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高橋 一弘, 増井 祥宏, 則永 行庸, 飯野 雅
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61-64
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The effect of addition of tetrabutylanmoium salts on the extraction of seven different kinds of coals with carbon disulfide-N-methyl-2-pyrrolidinone (CS_2-NMP) mixed solvent (1:1 by volume) was investigated. Addition of some salts considerably increased the extraction yield of some coals. For Upper Freeport coal, in particular, the addition of a very small amount, 0.25mol/kg-coal of tetrabutylammoniumfluoride increased the extraction yield from 59.8 to 83.9%. The effect of anion types on the extraction yield was also examined. It was found that the polarizability of anion is responsible for the increment of the extraction yields. The fractionations and FT-IR analyses of the extracts indicate that the extracts produced with the additive contain heavier and aromatic-richer constituents than that without additives.
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鈴木 正郎, Oja Vahur, 則永 行庸, 飯野 雅
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p.
65-68
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Upper Freeport (UF) and Illinois No. 6 (IL) coals were extracted with carbon disulfide-N-methyl-2-pyrrolidinone (CS_2-NMP) mixed solvent (1:1 by volume) and the extracts were subsequently fractionated by using pyridine and toluene or acetone. These extracts were mixed with NMP and annealed at 353K. Melting or gel-to-sol transition temperatures of the gelly samples were determined as a function of extracts concentration by using a needle penetrometer. The heats of dissociation of cross-links (ΔH_g) was estimated by applying Eldridg-Ferry equation to the experimental results. It was found that the ΔH_g range from 15 to 21kJ/mol which corresponding to the dissociation energy of hydrogen bonds. The apparent viscosities (η_a) of the samples were estimated by analyzing the penetration-temperature curves based on an existing relationship between the penetration rate and the viscosity. During melting of the gel, η_a is decreased approximately 4 orders of the magnitude by a temperature increase of 20K. The temperature dependency of η_a is described by Andrade's equation. The apparent activation energies for the viscous flows were rather high, i.e., 80-370kJ/mol
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中川 朝之, 古牧 育男, 坂輪 光弘, 西川 恵子
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p.
69-72
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Change in the surface fractal dimension (D_s) of Witbank coal with heat treatment was studied using small angle X-ray scattering. It was found that D_s shows peculiar changes depending on temperature and heating rate. Especially in the presoftening stage, D_s decreased with increasing temperature. From thermogravimetric and differential scanning calorimetric analyses, we concluded that this was derived from a physical structural change in coal.
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廣 真誉, 貴傳名 甲, 村田 聡, 野村 正勝
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p.
73-74
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We characterized chemical structure related to the coal plasticity. RuO_4 catalyzed oxidation reaction of coal was performed to analyze the structural features of the coking and non-coking coals, Goonyella and Witbank coals. The results showed several differences in aliphatic portion of coal. We also characterized the released gas and tar fractions and the resulting char fraction during heat-treatment. We discussed the structural diffrence between two coals based on the above results.
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三浦 孝一, 前 一広, 草川 拓巳, 熊野 明子
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p.
75-78
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In situ FTIR measurements were performed for the Argonne premium coals to estimate the change in hydrogen bonding through heat treatrnent. Neat coal samples were placed in a specially designed cell and they were heated from room temperature up to 300℃ in an inert atmosphere. FTIR spectra were collected in every 20℃ using the DRIFT method and the spectra ranging from 2400 to 3700cm^<-1> were divided into 6 hydrogen bonded OH peaks and other peaks. The strength distribution of hydrogen bonding (HBD) at each temperature was well estimated by analyzing the divided peaks by the method proposed by the authors. By utilizing the HBD the changes in enthalpies through the desorption of water, the glass transition, and the decomposition of OH groups were well estimated. The validity of the proposed in situ FTIR measurement method and the analysis method for obtaining HBD was well clarified.
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App4-
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礒田 隆聡, 高木 英行, 草壁 克己, 諸岡 成治
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p.
79-82
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The effect of the local structures on pyrolysis reactivity of coal was investigated by molecular orbital (MO) calculation using WinMOPAC program.
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呉 志恒, 杉本 義一, 川島 裕之
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p.
83-86
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In order to study nitrogen release from different nitrogen structures during coal pyrolysis, two model coals have been prepared using cellulose and well-defined nitrogen compounds. Nitrogen structures in the model coals have been analyzed by pyrolysis GC-NPD and GC-MS. Nitrogen release during pyrolysis of the model coals without and with catalyst has been studied in a fixed-bed reactor at 50℃/min up to 1000℃. Pyrolysis results show that iron catalyst is effective on nitrogen removal for both pyrrolic and pyridinic nitrogen. However, calcium catalyst is only effective for pyridinic nitrogen.
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河内 基樹, 貴傳名 甲, 村田 聡, 野村 正勝
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p.
87-90
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Alkyl radical formation during heat treatment of coal is considered to be the key reaction of gas formation in the coal liquefaction reaction. In this study, the heat treatment of both coal and its model compounds with polycyclic aromatic compounds was studied in order to understand the behavior of alkyl groups. The result of the reaction of model compounds shows that most reactive substituent is methoxy group and that this reaction proceeds by the attack of hydrogen atom at ipso position on the aromatic ring. The result of the reaction of coal corresponds to that of model compounds very well.
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阿部 有紀, 松岡 浩一, 富田 彰
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p.
91-94
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The hydrothermal reactions of mineral matter in coal and lime were carried out at 300℃ under autogeneous pressure in an autoclave. The hydrothermal products of Illinois #6 coal with lime were very effective for desulfurization. To determine the effective species, quartz or kaolinite was allowed to react with lime. These reaction products could absorb SO_x more effectively than raw lime.
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前田 昌彦, 山口 由美, 徐 炎華, 中島 常憲, 大木 章, 前田 滋
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p.
95-98
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Determination of arsenic, mercury and lead in NIST standard coals was done using ICP-AES or AAS method. Several tests were also conducted to find a suitable and practical method for the exact determination of the said toxic heavy metals in coal. By use of hydrothermally-treated alginic acid (HTTAA), removal of arsenic and lead in some coal samples was conducted. The leaching ability of HTTAA was comparable to that of EDTA.
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平戸 瑞穂, 和田 信幸
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p.
99-100
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平戸 瑞穂, 和田 信幸
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p.
101-104
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平戸 瑞穂, 和田 信幸
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p.
105-106
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奥山 憲幸, 田村 正明, 嶋崎 勝乗, Lambok H. Silalahi, 兼子 隆雄
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p.
107-110
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Solvent de-ashing is an effective way to separate solids from CLB (coal liqued bottom, bp>420℃). In the 50t/d Pilot Plant project for the liquefaction of Victorian brown coal, high efficiency and reliability of the solvent de-aching method were demonstrated using coal derived naphtha for a de-ashing solvent. In this paper, de-ashing characteristics of the CLB from Banko coal were examined using a batch type settler, campared with the case of Yallourn coal. It was recognized that the settling velocities of the solids in CLB are influenced by the depth of hydrogenation, not to coal sorts. Settling velocities of highly hydrogenated CLB were comparatively slower due to the lower concentration of heavier matter such as TI-THFS. It was confirmed that the settling velocity at a desireble level was able to be controled using a light naphtha for a de-ashing solvent.
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佐藤 正昭, 服部 英
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p.
111-114
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An evaluation method for a ring size distribution in a heavy oil is proposed based on the boiling point and molecular weight distributions. There was a difference between the boiling point distribution of the heavy oil obtained from a simulated distillation, and the imaginary one calculated on the assumption that all of the components were straight alkanes. The temperature difference (ΔT) between both distributions at the same distillate content is attributed to non-paraffinic structures in the heavy oil. As compared the aromatic ring size distribution evaluated from this temperature difference with the distribution analyzed by HPLC-MS measurement, both aromatic size distributions were in good agreement each other.
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松村 明光, 佐藤 信也, 斉藤 郁夫, 請川 孝治
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p.
115-118
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A methanol-mediated extraction process was designed to recover phenols from the naphtha fraction of Tanito Harum coal liquid. Then, the feasibility was studied for the commercial scale process. The results show that the total upgrading cost including the extraction cost, hydrogen cost and the income from crude phenol was less than that without extraction.
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与倉 寛人, 松村 幸彦
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p.
119-122
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Co-liquefaction of coal and biomass in supercritical water using a batch reactor was conducted at 400℃, 25MPa. Our recent work showed that by co-liquefaction residue yield decreased and that liquefaction was thus enhanced, but a large amount of heat was lost. In this work, an effective way of recovering heat from co-liquefaction products is discussed.
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App5-
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三浦 孝一, 中野 靖之, 真藤 博之, 前 一広
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p.
123-126
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We have recently presented a new and simple method to estimate the rate parameters of coal pyrolysis reactions using the so-called Distributed-Activation-Energy-Model (DAEM). Using the new DAEM, we analyzed the weight loss curves measured at three different heating rates under a vacuum, 0.1Mpa, and 5Mpa. It was found that the pyrolysis pressure apparently affects the rate parameters, the distribution of activation energy, f (E), and the frequency factor, k_0 (E). The effect was interestingly coal rank dependent. Based on these results discussion was made on a means to estimate true rate parameters of coal pyrolysis reactions.
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坪内 直人, 徐 春保, 大塚 康夫
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p.
127-130
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Formation of N_2 from Ca-loaded low rank coals during pyrolysis at 10K/min to 1350℃ has been studied with a fixed bed quartz reactor, and factors controlling N_2 have been examined. When the Ca is added to the raw coals, it decreases N_2 yield below 750℃ but increases it at 800-1100℃. In the case of the demineralized coals, the Ca added drastically increases N_2 yield at 900-1100℃, and provides 6-fold rate of N_2 formation at around 1000℃. It is suggested that the highly dispersed Ca catalyzes N_2 formation through solid-phase reactions in the high temperature range.
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海保 守, 張 愛華, 山田 理, 安田 肇, Moktar ZABAT, 中野 薫
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p.
131-134
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Influence of surrounding gas on the flash-pyrolitic behavior of Taiheiyo coal was investigated under N_2 and He atmosphere. It was found that the coal was decomposed more slowly under N_2 atmosphere. The lag of pyrolysis obserrved in N_2 atmosphere might be attributed to lower thermal conductivity of N_2 gas.
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山田 哲夫, 橋本 晴美, 鈴木 勉
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p.
135-138
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Chars prepared from 35 raw coals and their demineralized coals were gasified under atmospheric pressure of CO_2 at 1173K. In order to clarify the reason of various gasified profiles with conversion, some physical and chemical properties of residual chars with diffrent conversions were measured. The results indicated that modification of some mineral matters in the chars and clystallinity of carbon would have close relation to the gasification rate.
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尾上 薫, 小林 基樹, 堀江 高司, 丸島 渉, 亀井 修, 山口 達明
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p.
139-142
発行日: 1999/10/28
公開日: 2017/03/22
会議録・要旨集
フリー
An innovative method for directly converting brown coal to synthesis gas (hydrogen and carbon monoxide) in a single step was developed. 2.45GHz of microwaves with the desired power level controlled by a waveguide tuner were irradiated into the upperside of the packed bed under successive supply of gases (helium, oxygen/helium, hydrogen or methane), and the effects of irradiation time on coal conversion and the quantifies of hydrogen and carbon monoxide were discussed.
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高瀬 代代人, 高木 英行, 礒田 隆聡, 草壁 克己, 諸岡 成治
原稿種別: 本文
p.
143-146
発行日: 1999/10/28
公開日: 2017/03/22
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Coals were gasified in a flow of oxygen at 500℃, and CO yields were determined as functions of coal ranks and oxygen concentrations.
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牧野 三則, 曽根田 靖
原稿種別: 本文
p.
147-150
発行日: 1999/10/28
公開日: 2017/03/22
会議録・要旨集
フリー
The reactivity of coal on hydrogasification depends significantly on the coal rank as well as other gaseous reactions. The reaction characteristics of two selected coals were examined at a high pressure of hydrogen using a rapid heat reactor. The demineralization and heat treatment of coal prior to hydrogasification reduce their reactivities. For the effects of heat treatment, however, there is a great difference between chars prepared from slow and rapid heating. Chars from rapid heating have much higher reactivities than those from slow heating, although they have been devolatalized to a higher extent than latter.
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張 愛華, 海保 守, 山田 理, 安田 肇, Mokhtar Zabat, 中野 薫
原稿種別: 本文
p.
151-154
発行日: 1999/10/28
公開日: 2017/03/22
会議録・要旨集
フリー
For ARCH process under developing, the residence time of coal particles in reactor is only several seconds, and in this short time, various chemical and physical changes occur, such as rapid heating of coal particles, devolatization, decomposition, condensation and deposition. To understand these changes is important in ARCH process research and it can provide valuable reference to reactor design and furthermore to achieve high production and economic efficiencies. This paper presents the basis data of hydrogasification obtained with a Batch-Type reactor in 1-80s and discusses the initial hydrogasification process through comparison with the results of rapid coal pyrosis.
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後藤 充宏, 越崎 健司, 倉本 浩司, 菊地 隆司, 堤 敦司, 林 潤一郎, 千葉 忠俊
原稿種別: 本文
p.
155-158
発行日: 1999/10/28
公開日: 2017/03/22
会議録・要旨集
フリー
The thermochemical recuperative hydrogen production by rapid steam gasification of brown coal was examined at a heating rate of 80K・s-1 by using a thermobalance reactor. The effects of temperature and heating rate on pyrolysis and steam reforming reactions were investigated at 1073-1173K. The complete steam gasification was found to be achieved within 170s at 1173K and within 1000s at 1073K.
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平戸 瑞穂
原稿種別: 本文
p.
159-164
発行日: 1999/10/28
公開日: 2017/03/22
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丸山 英夫, 野村 和夫, 野口 冬樹, 勝倉 宏次郎
原稿種別: 本文
p.
165-168
発行日: 1999/10/28
公開日: 2017/03/22
会議録・要旨集
フリー
The Development of Coal Hydrogasification Technology to secure a stable supply of substituted natural gas (SNG) from coal at low cost has been performed from FY 1996 as a part of the Japanese governmental new energy program called the New Sunshine Project. This paper reports results from researches on hydrogasication reaction and on configuration of gasifier in succession to the previous paper.
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