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松村 明光, 小寺 洋一, 請川 孝治, 美藤 裕, 須賀田 正泰, 古本 正史, 永野 幹夫
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p.
189-192
発行日: 1994/08/31
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Solvent extraction of phenolic compounds from Wyoming coal-derived kerosene fraction has been studied using a batch and a continuous solvent extraction plant. An extraction rate of phenol and cresols increased with the increase of methanol/feed ratio, and decreased with the increase of water added in the case of high methanol/feed ratio, howevre increased at low methanol/feed ratio. A selectivities of phenol and cresols in extracts decreased with increasing methanol/feed ratio. A material balance was caluculated from the data by the continuous solvent extraction operation.
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山下 亨, 逢坂 進
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p.
193-196
発行日: 1994/08/31
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X-ray photoelectron spectro scopy (XPS), which can provide information on the chemical state of elememts, was applied to the direct determination of organic sulfur forms in coal. Analysis data from model compounds were used to interpret sulfur 2p signals from coal in terms of the amounts of alkyl sulfide and thiophenic sulfur. The relation of XPS results to the carbon structure, such as aromatic carbon fraction, were discussed. Temperature programmed reduction analysis was carried out in order to compare the data.
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山田 理, 安田 肇, 曽根田 靖, 小林 光雄, 牧野 三則, 海保 守
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p.
197-200
発行日: 1994/08/31
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Depth profiling anlyses of oxidized coal was carried out by using step scan FT-IR/PAS spectrometer with a phase modulation technique. Variation of modulation frequency and phase angle gave considerably different spectra reflecting a depth profile of coal particle. Range of sensible depth was estimated by microscope observation of oxidized coal. Step scan FT-IR/PAS method was also applied to analyses of gasification chars. Depth profiling PAS spectra of gasification chars could be obtained using slow step scan and low modulation frequency.
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森野 美鶴, 鷹觜 利公, 飯野 雅
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p.
201-203
発行日: 1994/08/31
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Coals were extracted with CS_2-N-methyl-2-pyrrolidinone mixed solvent at room temperature. The residue or extract was packed into column using chloroform as a mobile phase. Polystyrene standard samples and cata-typed polycyclic aromatic hydrocarbons were injected as a probe to investigate micropore structure (cross-link structure) of coal and interaction between the probe molecule and the coal. The elution behaviors of the probes were discussed from the mechanisms of the size exclusion and the chemical adsorption.
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熊谷 淳, 原口 博
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p.
204-207
発行日: 1994/08/31
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The use of low rank coal leads to reduce the coke strength because of leading to reduce the caking property of coking coal. We have tried to understand this mechanism by extracting and analyzing the caking component of low rank coal and Coking coal. And then, it has found that the caking component is decomposed by radical attacking from low rank coal, and thus the caking property reduce.
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則永 行庸, 熊谷 治夫, 真田 雄三, 佐々木 正秀, 小谷川 毅
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p.
208-211
発行日: 1994/08/31
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Pretreatment of lignite including drying of low rank coal is one of the most important processes for its utilization. Volume shrinkage and recovery of lignite have been measured with a swelling apparatus at 30℃. Dewatering with conc. H_2SO_4 is a reversible process, while conventional drying process is not with respect to volume changes. Volume changes during dewatering and drying process of lignite are responsible to the molecular association and inter- and intra- molecular bonding. Spin-spin relaxation times of proton in lignite molecules and associated water molecules are also providing the characterization during the dewatering and drying process.
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鷹觜 利公, 飯野 雅, 中村 和夫
原稿種別: 本文
p.
212-215
発行日: 1994/08/31
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A computer simulation using computer-aided molecular design (CAMD) was applied to the construction of three-dimensional coal structure. Molecular models for pyridine soluble constituent of Chinese bituminous coal (Zao Zhuang coal) with various length of intercluster bond which connects between two aromatic clusters, were constructed, and the energy-minimum conformation was determined by CAMD of the molecular mechanics and the molecular dynamics. To evaluate the constructed models, the density simulation for the molecular models was conducted, and the density was determined. The simulated density of the model in which the length of intercluster bond is two carbon atoms, was found to be in good agreement with that determined experimentally.
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渡辺 久典, 鷹觜 利公, 飯野 雅
原稿種別: 本文
p.
216-218
発行日: 1994/08/31
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Althougu it is generally accepted that coals have a three-dimensional cross-linked structure, the details are still unclear. Viscoelasticity of coals are recently studied for the understanding of the macromolecular structure of coal. In this study, coal-solvent gel films were first successfully prepared from coal extracts in organic solvents. Chemical and thermal properties of the gel films showed that a significant amount of solvent was retained strongly in coal sample probably due to strong interactions between the coal and the solvent. The measurement of stress-strain relationship showed that the gel films have some viscoelasticities. The specific properties are discussed related to the macromolecular structure of coals.
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佐々木 皇美, 井戸川 清, 福田 隆至, 成田 英夫
原稿種別: 本文
p.
219-222
発行日: 1994/08/31
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Supercritical Fluids have high diffusibility and solubility. In coal processing, the major interest has been in the development of supercritical extraction to produce liquid fuels from coal. On the other hand, some works have reported concerning the removal of sulfur and ash in coal from a environmental point of view. We have reported the removal of inorganic sulfur with supercritical water, however the mechanism of desulfurization in supercritical water is not so clear. This work attempts to investigate reactions of sulfur compounds in coal with supercritical water. Organic compounds with sulfur functional groups react in supercritical water, and pyrite is changed into iron oxide, however hetero cyclic compound hardly react.
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金持 真理子, 岸本 充司, 兼子 隆雄, 蔭山 陽一
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p.
223-226
発行日: 1994/08/31
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The surface properties of hydrothermal treated coals were assessed with calorimetoric measurement, with acidic or basic proves as adsorbent and isooctane. The heat of adsorption of pyridine per surface area of coal decreased with the treatment temperature. The ratio of heat of adsorption to desorption decreased for pyridine, in contrast to increasing for phenol by hydrothermal treatment of coal. These results suggested that the hydrothermal treatment resulted in change of functional groups which may act as acidic or basic site on coal surface.
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松岡 献二郎, 熊谷 治夫, 真田 雄三
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p.
227-230
発行日: 1994/08/31
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Interaction between Upper Freeport coal and mixed solvent (CS_2-pyridine) was carry out using L-Band EPR at room temperature. The X-Band EPR measurment in solvent with high dielectric constant is difficult due to energy loss of microweve, L-Band EPR makes easy to measure in such situation. Spectrum intensity and peak to peak line width were changed with mixing ratio of solvents.These facts indicate that the changes of inter- and intra-morecular interaction in coal occur in mixed solvent.
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平間 利昌, 細田 英雄, 佐々木 正秀, 原田 道昭, 鈴木 善三, 守富 寛
原稿種別: 本文
p.
231-234
発行日: 1994/08/31
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To elucidate the relation between nitrogen functionality of coals and N_2O and NO_x emissions, six kinds of model compounds were burnt with kerosene and/or coal. No remarkable difference in N_2O and NO_x emission levels was found among the model compounds in spite of the different nitrogen functionality, which suggests the presence of the conversion reaction from HCN to NH_3 mainly in the particle bed.
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楳田 慎一, 駒野 隆宏, 真下 清, 和井内 徹, 杉本 義一, 早水 紀久子, 三木 康朗
原稿種別: 本文
p.
235-238
発行日: 1994/08/31
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Cellulose and wood, Japanese redpine, were thermally decomposed at 200℃ in water to understand the structure change of the coalification process. Cellulose was partially hydrolyzed and converted into brownish materials with lose of H_2O and CO_2, and aromatization. The solid products were characterized by NMR, IR, elementary analysis and the determination of oxygen functional groups.
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中田 正夫
原稿種別: 本文
p.
239-241
発行日: 1994/08/31
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To make solvent radical under coal liquefaction conditions, benzoyl peroxide was added to tetralin- benzyl ether and tetralin-Irinois coal reaction system at around 300-420℃. It was found that benzoyl peroxide made a little increase in benzyl ether disappearing rate and Irinois coal's conversion rate.
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栗木 安則, 湯村 守雄, 大嶋 哲, 内田 邦夫, 伊ヶ崎 文和
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p.
242-244
発行日: 1994/08/31
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The catalytic activity of ultra fine metal sulfide on the hydrogenation of 1-methylnaphtharene (1-MN) was investigated. The metals used were Cobalt, Nickel, Iron andalloy of Iron and Cobalt. The average particle diameters of the metals were about 200A. The experiments were carried out in 50ml stainless steel autoclave at 350-450℃ under the initial hydrogen pressure of 7.9MPa. The structure of sulfided Cobalt was Co9S8, but that of sulfided Nickel was NixSy.
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山本 光義, 前河 涌典, 小谷川 毅
原稿種別: 本文
p.
245-248
発行日: 1994/08/31
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Hydrocracking of cis and trans-Decalin was investigated in the presence of Ru/NiO-ZrO_2-Al_2O_3, Ru/ZnO-ZrO_2-Al_2O_3 and Ru/Fe_2O_3-ZrO_2-Al_2O_3 as catalysts by a high pressure DTA techniques. The Ru/NiO-ZrO_2-Al_2O_3 did not show effective activity for the nuclear hydrocracking of the decalins. On the contrary the Ru/Fe_2O_3-ZrO_2-Al_2O_3 showed a good activity for the nuclear hydrocracking. However, the main products were alkylated cyclohexanes. Any of the catalysts did not show sufficient activity to form paraffinic hydrocarbons. When initial pressure of hydrogen was reduced from 10MPa to 1MPa, the dehydrogenation activity of the decalins was predominant and tetralin was mainly formed. Based on these results, a role of ruthenium is concluded to be the promoter of the hydrocracking of decalins.
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清水 聖幸, 稲葉 敦, 斉藤 郁夫
原稿種別: 本文
p.
249-252
発行日: 1994/08/31
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The present work is a study of the solubilization of coal in a HF/BF_3 -toluene system via an ionic reaction. The reaction was carried out at low temperature (50-150℃) without hydrogen gas in order to evaluate HF/BF_3 as an acid catalyst for coal solubilization with aromatic compounds.
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佐々木 正秀, 永石 博志, 佐々木 皇美, 前河 涌典, 小谷川 毅, 真田 雄三, 千葉 忠俊
原稿種別: 本文
p.
253-256
発行日: 1994/08/31
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Effect of selenium dioxide was examined on decarboxylation of Yallourn coal under nitrogen pressure of 1.0MPa at 473K. It has been shown that selenium dioxide accelerates decarboxylation of aliphatic carboxylic acid in coal structure compared with coal alone. However, the coal structure slightly varies due to decarboxylation. Experiments were also made on liquefaction of Yallourn coal using selenium and selenium dioxide as a catalyst. Both selenium and selenium dioxide catalysts indicate same yields of pyridine and toluene solubles. Selenium dioxide is reduced to selenium under the heat treatment condition. From these results, catalytic effect of selenium becomes a dominant factor of increase in conversion rather than decarboxylation of coal.
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坂西 欣也, 梅沢 達也, 谷口 秀樹, 持田 勲
原稿種別: 本文
p.
257-260
発行日: 1994/08/31
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Recoverable catalysts are prepared for the primary coal liquefaction, using Fe_3Al as a magnetic support. Fe_3Al is examined in terms of its resistivity against H_2S/H_2 atmosphere, the activity for the hydrogenation and liquefaction, and the activation by supporting Ni and Mo, and the surface modifications by grinding or acid treatment.
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佐藤 芳樹, 加茂 徹, 白石 稔
原稿種別: 本文
p.
261-264
発行日: 1994/08/31
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Effect of coal pulverization to fine particle of less than 10μm in diameter on the products distribution and the properties of TS and THFS was compared with the conventional 100 mesh coal. HS yields were higher, but gas yields were lower with larger hydrogen consumption in the case of finely pulverized coal. H/C of TS from the pulverized coal was higher and fa was lower. The effect of the Fe_2O_3-sulfur catalyst concentration on the liquefaction of coals was also discussed
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小谷川 毅, 山本 光義, 前河 涌典, 吉田 忠
原稿種別: 本文
p.
265-268
発行日: 1994/08/31
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Liquefaction of Taiheiyo impregnated a sulfate-promoted iron oxide catalyst was carried out under 10MPa initial hydrogen pressure at 673K, 698K and 723K by a 70ml autoclave with a magnetic stirrer. The way to impregnate the catalyst on the surface of coal was that coal was suspended into a mixture of aqueous solution of ferric sulfate and urea and heated up it in a water bath at 369K to 371K for about 2hrs. The conversion of coal impregnated the catalyst showed remarkably higher value than a conventional mixing way at 723K. Also, addition of sulfur in the reaction did not influence the reaction in terms of coal conversion. This suggests that active state of the catalyst differs from the pyritic catalyst.
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佐藤 光一, 安室 元晴, 進藤 照浩, 小山 徹, 兼子 隆雄, 蔭山 陽一, 井田 徹
原稿種別: 本文
p.
269-272
発行日: 1994/08/31
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Several types of iron oxide are used with sulfur as disposable catalyst in the primary hydrogenation section of Brown Coal Liquefaction Process. This paper discusses the effects of catalyst type and the activities of recovered catalysts on the liquefaction of Brown Coal.
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今井 潤, 小山 徹, 兼子 隆雄, 蔭山 陽一
原稿種別: 本文
p.
273-276
発行日: 1994/08/31
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Deposition behavior of iron catalysts during sulphidation were investigated using stainless-steel test-piece and I-MN as solvent. It was appeared that α-Fe_2O_3 which easily formed large particles by aggregation during the sulphidation. had relatively small amount of deposition on the test-piece and that γ-FeOOH dispersed in solvent had high oil yield and small amount of deposition in coal liquefaction reaction.
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田沢 和治, 金持 真理子, 小山 徹, 兼子 隆雄, 蔭山 陽一
原稿種別: 本文
p.
277-280
発行日: 1994/08/31
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It has been known that fine particles of pyrite are easily oxidized in the atmosphere. In this paper, the transformation of chemical structure of pyrite which was oxidized under various conditions are discussed in relation to the catalytic activity for coal liquefaction. A surface oxidation of pyrite resulted in a lower coal conversion for brown coal liquefaction.It was found that the finely divided particles of pyrite pulverized in the process solvent has a good liquefaction activity, even if the keeping for a long time.
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横山 晋, 中村 久志, 佐藤 正昭, 真田 雄三, 鈴木 優, 町原 勉
原稿種別: 本文
p.
281-284
発行日: 1994/08/31
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Monoaromatic ring fraction separated by NH_2 column HPLC for Akabira coal hydrogenation oil have been subjected to GC-MS/MS analyses by daughter mode to obtain mass spectra for respective component without contamination by coelution of GC column.
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佐藤 正昭, 杉淵 宏志, 大久保 高樹, 横山 晋, 村路 光義, 真田 雄三
原稿種別: 本文
p.
285-288
発行日: 1994/08/31
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Extraction oil and hydrogenation oils derived from residues were characterized by HPLC and MS analyses. It is considered that extraction oil and residues from coal have low molecular weight component and different degree of polymeric component. Chemical structures between the extraction oil and hydrogenation oils derived from three different rank of coals were compared according to compound type distributions. The compound type distributions of both oils for each coal were almost similar. This means that chemical structures of extraction oil and hydrogenation oils derived from residues have no differnce and only the degrees of polymerization are different among extract oil and residues. Furthermore, in high rank coal, the compound type distributions of aromatics are more wide than those in low rank coal because of the increase of aromaticity with coal rank.
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森高 伸吾, 三浦 雅博, 野村 正勝
原稿種別: 本文
p.
289-292
発行日: 1994/08/31
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In order to develop an effective method to obtain aromatic chemicals from coal-derived liquids, analysis and dehydrogenation of heavy naphtha and light oil fractions of three kinds of coal liquefied products have been examined; the materials have been produced by the NEDOL process from Illinois No.6, Wyoming, and Tanitharm coals. It has been found that irrespective of the original coals, the heavy naphtha and light oil fractions can be transformed into those containing naphthalene and methylnaphthalene, respectively, as the major components.
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葭村 雄二, 佐藤 利夫, 島田 広道, 松林 信行, 今村 元泰, 西嶋 昭生, 亀岡 隆, 梁瀬 寛司, 肥後 学, 吉冨 末彦
原稿種別: 本文
p.
293-296
発行日: 1994/08/31
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The thermodynamic analyses were done to better understand the catalyst preparation and sulfidation processes. Chemical potential diagrams were used to evaluate the stability/reactivity of the metal, sulfides, oxides, and sulfates using the thermodynamic data base. For the NiMo(CoMo) and NiW/Al_2O_3 catalysts, these analyses suggested a priori that the catalyst treating conditions, such as temperature, p(O_2) and p(H_2O) in calcination, and such as temperature, p(H_2S)/p(H_2) and p(H_2O) in sulfidation, influenced significantly the solid-gas and solid-solid phases interactions among the active components, promoters and γ-Al_2O_3 supports. These thermodynamic analyses would be very useful for designing/selecting the catalytic materials and for optimizing the calcination/sulfidation/hydrotreating-reaction conditions.
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米山 嘉治, 樋口 陽子, 加藤 彰, 加藤 勉
原稿種別: 本文
p.
297-299
発行日: 1994/08/31
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Hydrogenation of polar mixture eluate, PM in coal solubilized by SOLCAL-ZB process was carried out to obtain more detailed information about chemical structure and degree of depolymerisation. The PMs from Yubari and Taiheiyo coals were hydrogenated using Adkins catalyser at the temperature range 280〜400℃ for 5 hours. Structural parameters of HS and BS obtained were estimated by Brown-Ladner equation, and compared with those of untreated one. From these results, it was found that structural parameters, fa, σ and Hau/Ca, of HSs before and after treatment at 280℃ resembled each other, but only the Molecular Weights degreased by apploximately one-half.
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杉本 義一, 三木 康朗, 増渕 友志
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p.
300-303
発行日: 1994/08/31
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Compound groups separated from C_<30>〜C_<40> vacuum gas oil were analyzed by Py-GC. The major cracking products of each compound group were assigned by GCMS and GC-AED. The PY-GC chromatograms of polynuclear aromatic groups provided specific peaks which could be distinguished from those of other groups. The PY-GC technique combined with HPLC separation would be useful to understand the chemical structures of complicated heavy oils.
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鈴木 武志, 張 戦国, 京谷 隆, 富田 彰
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p.
304-307
発行日: 1994/08/31
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The carbon-NO reaction has been studied in the presence of oxygen. Oxygen enhances the reaction rate through the formation of surface oxygen complexes. Not only the oxygen complexes but also nitrogen complexes were formed on carbon surface. These nitrogen complexes were identified by XPS. The peaks were assigned to pyridinic, pyrrolic, quaternary, -NO and -NO_2 type nitrogen. Generally, pyridinic and pyrrolic nitrogen were much more than others. N_2 formation during the NO_x reduction takes place by the reaction of these nitrogen complexes. The effect of the type of carbon on the reduction of NO also was examined by using three carbons with different surface areas. TPR experiments revealed that the carbon with a higher surface area is more reactive, and that carbon-O_2 reaction is essential for the carbon-NO reaction.
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林 順一, A.P. Watkinson
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p.
308-311
発行日: 1994/08/31
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小原 寿幸
原稿種別: 本文
p.
312-315
発行日: 1994/08/31
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For the purpose of removing nitrogen atoms from heavy oil by microbial procedures, the first approach was made to obtain microorganisms capable of degrading quinoline by enrichment culture. The degradation of quinoline by the chosen isolate yielded initially 2-hydroxyquinoline and then 8-hydroxycoumarin. This strain was able to degrade quinoline and a few methylquinolines in a complex basic fraction of coal-liquid. Isolation of mutant bacteria which tolerate fairly high concentration of quinoline is in progress.
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