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Cover1-
発行日: 1995/10/26
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原稿種別: 目次
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三木 啓司, 古屋 武, 佐藤 芳樹
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1-4
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Synthesis of monooxygenase model was attempted to apply its functions to the solubilization of coals. The model could oxidize various aliphatic and aromatic compounds to hydroxylated derivatives predominantly at ambient conditions. The catalytic activity of oxygenase model related to coal solubilization reaction is discussed.
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四分一 弘, 長島 進, 阿尻 雅文, 新井 邦夫
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5-8
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Supercritical water extraction of Japanese sub-bituminous (Taiheiyo) coal was conducted with semi-batch type reactor (380℃, 25-40MPa) and the results were compared with that for supercritical toluene extraction (380℃, 15-30MPa). Higher coal conversion (55wt%) and liquid yield (45wt%) were obtained for supercritical water extraction, and this is found to be because of (1) the inhibition of polymerization or recombination of the primary products of thermal decomposition of coal, perhaps due to the radical quenching with H or OH, and (2) the hydrolysis of ether or ester bond in coal.
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永石 博志, 吉田 忠, 吉田 諒一
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9-12
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Liquefaction experiments were conducted in a 50cm^3 magnetically stirred autoclave at various temperatures and heating rates under 10MPa-N_2 with exess amount of tetralin. Change of pyridine insoluble yield with heating rate at least 623K to 673K showed the maximum yield in ca. 10 to 20K/min of heating rate range. These profile suggested that the less reactive component, such pyridine insoluble of which reactivity is different from original coal components, formations took place during heating via pyridine solubles produced from coal.
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木戸口 晃, 神田 伸靖, 伊藤 秀伸, 平出 政隆, 谷道 治作
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13-16
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Reactions in the initial stage of coal liquefaction of two kinds of subbituminous coals were studied. A novel kinetic model was proposed and kinetic constants were determined. Weight fractions of each components estimated from those kinetic constants fitted with the results of experiments carried, out with a rapidly heating autoclave.
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古明地 東, 今井 潤, 兼子 隆雄, 蔭山 陽一
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17-20
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Pretreatment of brown coal in solvent is effective to suppress the formation of the carbonate scale in the liquefaction. Making use of Tetralin as H-donor solvent or 1-Methyl naphthalene as non-donor solvent, the influence of pretreatment condition to liquefaction yield and decomposition of oxygen-functional groups were investigated in this paper.
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奥山 憲幸, 安室 元晴, 平野 龍夫, 奥井 利明, 勝島 眞一, 蔭山 陽一
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21-24
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In order to improve economics of coal liquefaction process, it is important to make light oil in a high yield. In this paper, effects of the boiling point range of solvent to increase lighter oil fraction were studied using an autoclave and a continuous BSU. According to heavier solvent recycled, the ratio of light fraction yield in total distillate increased, but the fraction to be recycled as solvent was shortage. An addition of coal liquid bottom (CLB) showed large effect to increase both lighter fraction and solvent fraction combined with the recycle solvent whose boiling point range was 300 to 420℃.
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上杉 研二, 古明地 東, 金持 真理子, 兼子 隆雄, 蔭山 陽一
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25-28
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The effect of heating conditions during initial stage on yield of liquefaction products was investigated on Yallourn coal. Low THFI yield and high HS yield of liquefaction product were obtained by liquefaction after thermal treatment at 350℃ for 30 minutes with catalyst and hydrogen donor solvent. The effect of thermal treatment was considered to suppress retrogressive reaction during initial stage by efficient hydrogen transfer due to the contribution of catalyst mainly.
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川端 睦麿, 相原 洋一, 今田 邦弘, 坂脇 弘二, 野上 義信, 井口 憲二, 坂木 剛, 柴田 昌男, 廣末 英晴
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29-32
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The effects of particle size distribution of pulverized coal, coal moisture content, additive and slurry temperature on rheological property of slurry were studied. It was found that each factor, especially slurry temperature, affected on rheological property. Furthermore, each coal had the optimal coal moisture for decreasing slurry viscosity.
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大隈 修, 増田 薫, 進藤 照浩, 金持 真理子, 松村 哲夫
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p.
33-36
発行日: 1995/10/26
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The structure of preasphaltene derived from Victorian brown coal during liquefaction was investigated by GPC analysis etc. These analyses make clear that the preasphaltene consists of three components; polar-higher molecuar weight (PH), polar-lower molecular weight (PL) and non-polar (NP) components. At the first stage of liquefaction reaction, the preasphaltene which includes much PH is produced, then it is converted into other lighter fractions such as asphaltene (others) through two main reaction paths as follows; (1) PH→others, (2) PH→PL→NP→others.
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進藤 照浩, 奥山 憲幸, 奥井 利明, 勝島 眞一, 蔭山 陽一
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p.
37-40
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Thermal treatment in liquefaction solvent was applied to Victorian brown coal as pretreatment for suppression of the scale formation during coal liquefaction. In order to improve reactivity of pretreated coal. the effects of hydrogenated solvent, hydrogen gas and catalyst were investigated. Hydrogenated solvent was effective to suppress the reduction of coal reactivity. Pretreatment with hydrogen gas and catalyst (pyrite) seemed effective to increase the coal reactivity.
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池田 耕一, 望月 通晴, 今田 邦弘, 三田 茂, 野上 義信, 井口 憲二
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p.
41-44
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Coal slurry sample was withdrawn from the first reactor of 1t/d Process Supporting Unit (PSU) with a reactor sampler and analyzed. On the basis of properties of the sample and material balance, behavior of coal liquefaction in the reactor was investigated.
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相原 洋一, 川端 睦麿, 池田 耕一, 今田 邦弘, 野上 義信, 井口 憲二
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p.
45-48
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Liquefaction tests were conducted on several coals and catalysts at 1t/d Process Supporting Unit (PSU), and effects of coals and catalysts on composition of obtained coal derived oil were studied. There was difference in paraffin content of coal derived oil among four kinds of coals. Among three kinds of iron sulfide catalysts, natural pyrite accelerated cracking of normal paraffins in the oil.
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糸永 真須美, 今田 邦弘, 井口 憲二
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p.
49-52
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The characteristics of residue in coal liquefaction process were discussed. To stabilize the discharging of residue from vacuum colume in PSU, it's important to estimate the characteristics of liquefaction residue, for example the viscosity. It was discussed that the inference of ash volume fraction and chemical structure in the organic entity of residue on the viscosity of liquefaction residue. Also the equation to estimate the viscosity of liquefaction residue with considering above results was proposed.
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畑 和明, 和田 健司, 渡部 良久, 光藤 武明
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p.
53-56
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Activity of iron sulfate/sulfur as a catalyst precusor in the coal liquefaction using syngas-water was investigated. FeSO_4/S was the excellent catalyst precusor for Wandoan coal to achieve the high oil yield (oil yield 46.2%, conversion 90.1%) in the two-step liquefaction (400℃, 60min+425℃, 60min) in combination with the pretreatment at lower temperature.
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神戸 正純, 石原 篤, 加部 利明
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p.
57-60
発行日: 1995/10/26
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Effects of addition of pyrrhotite and sulfur on hydrogen transfer in liquefaction of Taiheiyo coal were investigated using tritium and ^<35>S tracer methods. With the pyrrhotite catalyst, the hydrogen addition to coal and liquefaction products increased with the addition of sulfur. A part of added sulfur participated in the sulfur. exchange reaction with the pyrrhotite catalyst.
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小方 英輔, 西嶋 昭生, 石渡 健一郎, 堀江 一之
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p.
61-64
発行日: 1995/10/26
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Oxidation of pyrite catalyst under air were investigated by of XRD and weight change. Synthetic pyrite was oxidized to szomolnokite FeSO_4・H_2O as one of ferrous sulfates even at room temperature. It suggests that iron and sulfur atoms in the strict pyrite structure were moved and rearraged even at room temperature. Activities of pyrite to 1-methylnaphthalene (1-MN) and 1-[4-(2-phenylethyl) benzyl] naphthalene (PEBN) hydroconversion were decreased by the oxidation under air. The low active pyrites oxidized was reactivated by enough sulfur addition to the reaction system.
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谷口 英夫, 岡本 信次, 三枝 智子, 池永 直樹, 鈴木 俊光
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p.
65-68
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Three kinds of iron carbonyl-sulfur complexes such as (Fe(CO)_3S)_2, (CH_3SFe(CO)_3)_2 and (t-BuSFe(CO)_3)_2 were prepared in order to obtain dispersed active iron catalyst for coal liquefaction. Liquefaction of Yallourn coal in 1-methylnaphthalene with iron complexes was carried out at 693K, 5.0MPa for 60min. All these iron carbonyl-sulfur complexes afforded higher conversions and oil yields as compared to the other iron-sulfur catalyst.
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桜井 正昭, 林 重嘉, 松江 雄二, 甲斐 貞, 鹿住 登, 遠藤 幸平, 野上 義信, 井口 憲二
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p.
69-72
発行日: 1995/10/26
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The development of a dry production method for synthetic iron sulfide catalyst was conducted using a small scale appratus with the production capacity of 10kg/hr. The dry production method would be expected to have larger productivity than the wet production method. The product catalyst has 92 weight percent of iron disulfide content and about 100 micron of the average particle size (secondary) which is easily crushed to submicron level by ultrasonic treatment. The liquid yield using the product catalyst by autoclave coal liqefaction test is 4 percent higher than that of the wet method catalyst.
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小山 徹, 田沢 和治, 佐藤 光一, 兼子 隆雄, 蔭山 陽一
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p.
73-76
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The effect of crystallite size of pyrrhotite on liquefaction activity was discussed. The sulfidation experiment of γ-FeOOH catalysts showed that liquefaction activity increased with decrease in crystallite size of pyrrhotite after sulfidation. Liquefaction activity of iron catalysts increased as crystallite size of pyrrhotite in recovered catalysts became smaller, and decreased with formation of troilite.
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佐藤 光一, 安室 元晴, 小山 徹, 奥井 利明, 兼子 隆雄, 勝島 眞一, 蔭山 陽一
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p.
77-80
発行日: 1995/10/26
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Several types of iron compounds are used with sulfur as disposable catalyst in coal Liquefaction Process. This paper discusses the effects of catalyst type on products yield and properties of coal liquid bottom (CLB). It was found that γ-ferric oxyhydroxide (FeOOH) was superior to increase the distillate yield and the extent of hydrogenation of aromatic rings.
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田沢 和治, 小山 徹, 兼子 隆雄, 蔭山 陽一
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p.
81-84
発行日: 1995/10/26
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A cation exchange method was used to prepare iron-loaded Yallourn coal. Ca, Mg and Na in coal were removed completely by cation exchange with iron (II) sulfate aq. solution at pH 3.5. The iron-loaded coal by cation exchange method was shown slow formation of active phase as pyrrhotite (Fe_<1-x>S) by decomposition of iron carboxylate followed by sulfidation. Consequently, the iron-loaded coal gave a lower coal conversion. Another iron-loaded coal was prepared by adding ammonia water for residue of iron cation in aq. solution after cation exchange treatment. The iron-loaded coal by this method found to give better activity at a lower amount of cation exchanged iron and a higher amount of iron hydroxide on the iron-loaded coal. It was considerd that iron hydroxide on coal easily formed pyrrhotite by sulfidation before thermal decomposition of coal started.
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稲葉 利晴, 神田 伸靖, 津久井 裕, 橋本 孝雄
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p.
85-88
発行日: 1995/10/26
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The AWIP catalyst^1),which is composed of iron particles and coal support, has a high hydrogenation activity in coal liquefaction reaction. To identify if the high performance might due to the supporting, the crystal size, particle size, component and chemical activity of iron catalyst were analyzed, when the iron catalyst crystals were attached on carbonblack particles to simulate the composite attaching on coal particles. The support keeps iron particle size fine, and make different kind of iron sulfide.
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野上 義信, 井口 憲二, 川端 睦麿, 今田 邦弘
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p.
89-92
発行日: 1995/10/26
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Liquefaction tests were conducted on Tanito Harum coal at 1t/d Process Supporting Unit (PSU). And the effect of pulverized natural pyrite, wet method and dry method synthetic iron sulfidies as coal liquefied catalyst on the product yield was studied. As a result, the liquefied oil yield at the use of the dry method synthetic iron sulfide was higher than those at the use of the other catalysts. At 465℃ Max conditions, the oil yield was 61.8wt% (daf coal basis), equivalent to 4.65bbl/t-daf coal.
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三木 康朗, 杉本 義一
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p.
93-96
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The catalytic activities of supported and unsupported FeS_2 were evaluated concerning with hydrogenation, HDS and HDN in reactions with and without existence of coal. The Alumina supported FeS_2 catalyst showed the highest activity in all reactions, especially in HDS. All of the catalysts were deactivated with the existence of small amount of coal.
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二タ村 森
原稿種別: 本文
p.
97-100
発行日: 1995/10/26
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Hydrogen transfer from tetralin to trans-stilbene at 380℃ was promoted by carbon materials such as activated carbon, carbon black and fullerene-rich soot. They decreased selectivities for 1, 2-diphenylethyl radical stabilization rather than increased bibenzyl yields. Its addition to the aromatic nucleus of trans-stilbene was promoted on the surfaces of the above carbon materials. With metal oxides as catalyst, tetralin hydrogens were also consumed in the reduction of the metal oxides to give little higher bibenzyl yields than without catalyst.
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大嶋 哲, 湯村 守雄, 内田 邦夫, 依田 智, 栗木 安則, 伊ヶ崎 文和, 菅沼 彰, 浜田 俊孝, 藤巻 敦
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p.
101-104
発行日: 1995/10/26
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We synthesized ultra fine particles of Fe, Ni, La, Co and Mo with diameter of 5-20nm. The particles are stable under the atmosphere because they are covered with graphite sheet. Some of these were tested activities as a catalyst of hydrogenation reaction and dehydrogenation reaction. It was found that ultra-fine particles of Ni-carbon composite had high activities as catalysts
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相田 哲夫, 山西 一誠
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p.
105-108
発行日: 1995/10/26
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In order to develope an efficient coal liquefaction process, the effect of the pre-treatment of coal on the efficiency of the catalyst has been examined, which was carried out by the solvent swelling of coal in the various solutions of the metal(Fe, Ni) carboxylate. It was found that the accessibility of the catalyst to the active sites in the coal matrix seemed to be significantly improved, and in the case of the iron catalyst the positive effect of the sulfidation process was not observed.
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谷口 秀樹, 坂西 欣也, 蓮尾 東海, 持田 勲
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p.
109-112
発行日: 1995/10/26
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Highly dispersed catalysts supported on carbon fine particles for the liquefaction of Indonesian coals were investigated in order to achieve the highest oil yield without producing organic residue. The activities of the carbon-supported catalysts for the coal liquefaction were compared in terms of reaction conditions, species of coals, carbons and metals, and effects of catalyst amount and recovery.
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蓮尾 東海, 谷口 秀樹, 坂西 欣也, 持田 勲
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p.
113-116
発行日: 1995/10/26
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Catalytic activity of NiMo supported on hollow carbon black was examined in the liquefaction of Wyoming subbituminus and Yallourn brown coals by pretreatment and the successive two stages at different temperatures. The oil yield in the liquefaction of Wyoming and Yallourn coals at 380℃-120min/440℃-60min provided 67wt% and 68wt%, respectively. The hydrogenation at a lower temperature appears to accelerate the conversion of asphaltene to oil by the successive stage of higher temperature.
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菅野 元行, 村山 勝義, 真下 清, 和井内 徹
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p.
117-120
発行日: 1995/10/26
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Hydrogenolysis reactions of coal liquid related model compounds and coal liquefaction residue (CLR) from Muswellbrook coal were carried out using red mud and sulfur catalysts at 693K for 1 hour. In the hydrogenolysis reaction of 7, 8-benzoquinoline (7BQ) alone, amounts of 7BQ absorbed onto the catalyst surface were lesser than the reaction of 5, 6-benzoquinoline. Therefore, in the reaction of CLR and 7BQ, because 7BQ dissolved and dispersed CLR, the catalyst activity was maintained. Then, the synergistic effects such as the decrease of dichloromethane insoluble and the increase of n-hexane soluble in the products appeared.
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藤本 雅信, 海津 一宏, 山内 のりか, 真下 清, 和井内 徹
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p.
121-124
発行日: 1995/10/26
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Alloy hydride has the characteristics of the hydrogen absorption and desorption. Absorbed hydrogen is active on hydrogenation reaction. In this study, Alloy hydrides are used as catalysts of hydrogenation of solvent refined coal, the effectiveness is discussed.
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田口 尚毅, 辻 俊郎, 柴田 俊春, 上牧 修, 伊藤 博徳
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p.
125-128
発行日: 1995/10/26
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Pyrolysis and catalytic cracking reaction of four kinds of coal liquefaction residues were carried out by use of a TG apparatus and a GC with pyrolyzer under inert gases. In the TG analyses, maximum weight decrease of each sample was observed at heating rate of 5℃/min and Ilinois No. 6 coal residue exhibited a little larger weight decrease than others. The catalytic cracking reaction with a FCC catalyst showed that lighter fractions of which the retention time is shorter than naphthalene increased.
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増田 浩司, 梁瀬 寛司, 亀岡 隆, 佐藤 利夫, 葭村 雄二, 島田 広道, 松林 信行, 西嶋 昭生
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p.
129-132
発行日: 1995/10/26
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Newly developed Ni-W/USY-Al_2O_3 hydrocracking catalyst was designed and prepared based on fundamental research in order to produce lighter fractions from middle and heavy distillates of coal-derived liquids. The catalyst developed showed considerable improvements in hydrocracking activity and initial deactivation, as compared to commercially available catalysts. However, precise characterization revealed changes in local structure of active metal and accumulation of carbonaceous material on the catalyst, indicating other possibilities for improving catalytic performance.
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前 一広, 牧 泰輔, 井上 真司, 三浦 孝一
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p.
133-136
発行日: 1995/10/26
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We have succeeded in to dissolve a brown coal oxidized by H_2O_2 up to 92% in polar solvents such as DMF and DMSO. It was found that the oxidation at 60℃ for 2h by H_2O_2 was suitable to introduce many carboxyl groups into coal without destroying the coal structure significantly. The solution was served to several spectroscopic analyses, and average unit structure of the brown coal was presumed to consist of 1.4 aromatic rings attached with 1.0 carboxyl group, 0.6 ketone, 1.9 phenolic OH groups and 0.6 ether group.
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前 一広, 牧 泰輔, 荒木 潤, 三浦 孝一
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p.
137-140
発行日: 1995/10/26
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A new method was developed for solubilizing a brown coal in a conventionally used solvent at room temperature. The coal pretreated with hydrogen peroxide in liquid phase at 60℃ for 2h was extracted by solvent mixtures of methanol and a non-polar solvent by the conventional method. In the solvent consisting of methanol and 1-methylnaphthalene (0.54: 0.46 volumetric ratio), surprisingly, 84wt% of the pretreated coal were extracted.
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安田 肇, 曽根田 靖, 山田 理, 小林 光雄, 海保 守
原稿種別: 本文
p.
141-144
発行日: 1995/10/26
公開日: 2017/03/22
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Enthalpies of sorption for methanol on Taiheiyo coal were investigated by repeated uptake and desorption experiments using fresh and heat treated coal to 125℃. The adsortption isotherm obtained for the heated coal differs from that of the original coal but is similar to that of the oxidized coal which was previously reported. Results of thermal analysis indicate an increase in strong interactions between methnal and a certain sites in the coal which appear to be created during thermal treatment or oxidation processed.
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王 楠, 佐々木 正秀, 吉田 忠, 小谷川 毅
原稿種別: 本文
p.
145-148
発行日: 1995/10/26
公開日: 2017/03/22
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Previously, in our research, the adsorption of methanol, THF and tetralin at coal surface was investigated by flow microcalorimetric measurement and it was found that these solvents interact with coal surface quite differently. In order to examine the interactions of coal surface and solvent quantitatively, not only adsorption and desorption heat, but also adsorption and desorption amount were measured in this research. Based on the experimental results, amount and molar heat of adsorption were determined for both strong and weak adsorption. It was found that although the amount of strong adsorption is only several percent of all the adsorption amount, more than 20% of adsorption heat results from the strong adsorption.
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松方 正彦, 藤本 英和, 上山 惟一
原稿種別: 本文
p.
149-152
発行日: 1995/10/26
公開日: 2017/03/22
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The distributions of surface wettabilities for 3 kinds of coals, Datong, Ensham and Illinois, were determined by a film flotation method. The results of column flotation for each coal were compared with those obtained by the film flotation method. It was found for Datong coal that carbonaceous materials recovery, ash rejection and pyritic sulfur rejection were high, since hydrophobic fractions easily floated and hydrophilic fractions are difficult to float. On the other hand, for Illinois coal carbonaceous materials recovery was very low because substantial amount of hydrophobic fraction remained in the column.
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早坂 和章, 鷹觜 利公, 飯野 雅
原稿種別: 本文
p.
153-156
発行日: 1995/10/26
公開日: 2017/03/22
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The surface tension of coal extracts fractions, i.e., acetone soluble (AS), and pyridine soluble-acetone insoluble (PS) fractions, in N-methyl-2-pyrrolidinone was measured at 25℃ by the Wilhelmy plate method. The surface tension was decreased as AS concentration increased and then its decrease rate became slow down at a certain concentration at which micelle-like coal associates may begin to form. The similar behavior has been reported for the solution of petroleum asphaltene in pyridine. On the other hand, the surface tension of PS, which is a heavier fraction than AS, showed no concentration dependence.
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山本 佳孝, 佐藤 芳樹, 脇坂 昭弘, 竹尾 陽敏
原稿種別: 本文
p.
157-160
発行日: 1995/10/26
公開日: 2017/03/22
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Upon crystallization from mixtures containing five- and six-membered nitrogen heteroaromatic compounds, intermolecular compounds of 1:1 molar ratio are isolated as crystals in which hydrogen bonding occures between the twe molecules. However,there is very little direct experimental evidence to show how crystals of the intermolecular compound are formed through the hydrogen-bondong interaction. We have observed by the measurement of mass spectra of clusters that the hydrogen-bonding complex of indole and isoquinoline is a definate species which forms clusters in solution composed of indole and isoquinoline molecules. This system demonstrates the primary process for the nucleation of the intermolecular compounds.
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川島 裕之, 山下 安正, 稲葉 敦, 斉藤 郁夫
原稿種別: 本文
p.
161-164
発行日: 1995/10/26
公開日: 2017/03/22
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Solid state NMR were measured for pyridine-soaked coals to study the interaction of coal and solvent. <T_1>^H decreased in the order fresh coal>pyridine-soaked coal for high rank coal. For low rank coal. <T_1>^H increased with pyridine soaking. These changes resulted from the mobility changes of coal.
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村谷 剛, 村田 聡, 野村 正勝, 池田 耕一
原稿種別: 本文
p.
165-168
発行日: 1995/10/26
公開日: 2017/03/22
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To develop the advanced application of brown coal, structural study on Australian Yallourn and Indonesian South Banko coals was carried out by using Curie-point pyrolysis and solid state NMR spectroscopy. Since brown coal contains much oxygen (>20wt%), analyses of the oxygen functionalities were thought to be important. As for molecular weight of the brown coals, GPC analyses of extracts were carried out. On the basis of the above data, chemical structural features and properties of the brown coals were discussed.
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高 鴻, 村田 聡, 野村 正勝
原稿種別: 本文
p.
169-172
発行日: 1995/10/26
公開日: 2017/03/22
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We had proposed a model of chemical structure of US subbituminous Illinois No. 6 coal in 1992. After that we found that the quinoline soluble fraction of Illinois No. 6 coal reached 85% yield at 35℃ and 4.9MPa nitrogen pressure for 60min, the extract being completely soluble in DMF. On the basis of detailed analysis of the extract using GPC, ^1H-NMR, ^<13>C-NMR, Py/GC/MS, and FT/IR methods, several more refined unit molecular structures were constructed. The minimumenergy 3D structures and their non-covalent interactions were evaluated using CAMD method.
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杉本 義一, 早水 紀久子, 三木 康朗
原稿種別: 本文
p.
173-175
発行日: 1995/10/26
公開日: 2017/03/22
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Artificial coals were prepared by hydrous pyrolysis of several feedstocks such as cellulose and peat, and their chemical structures and hydrogenation reactivities were compared with those of natural coals.
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