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1. 发明专利

JPH09142849A IRON SULFIDE AND ITS PRODUCTION 失效
公开(公告)号：JPH09142849A
公开(公告)日：1997-06-03
申请号：JP15287396
申请日：1996-05-27
申请人： ASAHI CHEMICAL IND , NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： KAI SADA , MATSUE YUJI , SAKURAI MASAAKI , IMADA KUNIHIRO , IGUCHI KENJI
IPC分类号： C01G49/12 , B01J27/043 , C10G1/06
摘要： PROBLEM TO BE SOLVED: To produce an iron sulfide capable of manifesting excellent handleability and hydrogenating catalytic activities in liquefying coal or hydrogenolysis reaction of a heavy oil and provide an efficient method for producing the iron sulfide. SOLUTION: This iron sulfide has 20-300μm 50% particle diameter (hereinafter referred to as d50 ) in cumulative distribution based on the volume of secondary particles mainly formed of primary particles having components of 85-100% FeS2 , 5-0% Fe1- XS (X is 0-0.2), 5-0% Fe3 O4 and 10-0% FeSO4 on the weight basis according to an X-ray diffractometry and 10-400nm particle diameter.

2. 发明专利

JPH1176823A SLURRY CATALYST FOR DECOMPOSING HEAVY HYDROCARBON AND ITS MANUFACTURE 失效
公开(公告)号：JPH1176823A
公开(公告)日：1999-03-23
申请号：JP25261097
申请日：1997-09-03
申请人： ASAHI CHEMICAL IND , NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： KAI SADA , HAYASHI SHIGEYOSHI , SAKURAI MASAAKI , ASO TATSUJI , IGUCHI KENJI
IPC分类号： B01J23/745 , B01J27/043 , C10G1/06 , C10G1/08 , C10G47/06
摘要： PROBLEM TO BE SOLVED: To provide a slurry catalyst and its preparation method wherein an iron compound (a catalytic active constituent) is prevented from growing during reaction, and further high activity is provided in coal liquefaction or heavy oil hydrogenation decomposing reaction. SOLUTION: In oil of 40 to 60 wt.% total amount wherein a mixture of coal and an iron compound catalyst of which d50 (50% particle size of cumulative distribution of volume standard of secondary particle in which primary particle is aggregated) is 20 to 30 μm, is mixed in oil, they are crushed and ground together until an average particle size of the coal becomes 20 μm or under. Thereby, a slurry catalyst for decomposing heavy hydrocarbon wherein the decomposed crushed iron compound is stuck in a thin film state onto a surface of the coal finely dispersed in the oil, can be manufactured.

3. 发明专利

JP2001026785A METHOD FOR COAL LIQUEFACTION 失效
公开(公告)号：JP2001026785A
公开(公告)日：2001-01-30
申请号：JP20180499
申请日：1999-07-15
申请人： AGENCY IND SCIENCE TECHN , MITSUI SEKITAN EKIKA KK , NIPPON STEEL CORP , ASAHI CHEMICAL IND
发明人： OKADA YASUO , IGUCHI KENJI , HANEDA MORIYA , IMADA KUNIHIRO , AIHARA YOICHI , SAKURAI MASAAKI , SHIBATA MASAO , SAKAKI TAKESHI
IPC分类号： B01J27/043 , C10G1/06
摘要： PROBLEM TO BE SOLVED: To provide a method for coal liquefaction ensuring a catalyst aggregation to be prevented during temperature rising process and under liquefaction reaction conditions, thereby high catalytic activity to be elicited and liquefied oil yield to be improved. SOLUTION: This method for coal liquefaction comprises the following steps: a slurry is made by mixing coal with a solvent and a catalyst and then subjected to high-temperature and high-pressure conditions in the presence of hydrogen to effect hydrogenolysis of the coal to produce the objective liquefied oil; wherein an anionic surfactant is included in the slurry.

4. 发明专利

JPH08311458A METHOD FOR LIQUEFYING COAL BY USING HIGHLY ACTIVE CATALYST CONTAINING SULFATE 失效
公开(公告)号：JPH08311458A
公开(公告)日：1996-11-26
申请号：JP14133995
申请日：1995-05-17
申请人： NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK , ASAHI CHEMICAL IND
发明人： ENDO KOHEI , IGUCHI KENJI , HAYASHI SHIGEYOSHI , TAMURA NOBUHIRO , KAI SADA
IPC分类号： B01J27/043 , B01J27/053 , C10G1/06 , C10G1/08
摘要： PURPOSE: To liquefy coal in a high catalytic activity in a high yield of soft oils at a low cost by using iron sulfide containing a sulfate as the catalyst. CONSTITUTION: Coal is liquefied at a higher efficiency by using an iron sulfide catalyst containing 5-30wt.% iron sulfate. The coals used suitably are bituminous coal, subbituminous coal and brown coal. The coal is heated to 300-900 deg.C. The temperature is usually desirably 400-500 deg.C, because the rate of liquefaction is low at low temperatures, and carbides and gases are produced in larger amounts at high temperatures. If a sufficiently hydrogenated medium oil is used, fresh hydrogen is not necessary for the liquefaction. The medium oil is added in an amount of 100-400% based on the coal. It is suitable that the medium oil used is liquefied coal or a product of its hydrogenation. The amount of the catalyst used is suitably 0.5-2% based on the anhydrous ash-free coal. The catalyst used is a product obtained by firing commerically available ferrous sulfate or ferrous sulfate recovered from iron slag and containing a small amount of various metal salts at 250-1,000 deg.C in the presence of sulfur in a fluidized bed oven.

5. 发明专利

JPH11323349A COAL LIQUEFACTION 失效
公开(公告)号：JPH11323349A
公开(公告)日：1999-11-26
申请号：JP14828898
申请日：1998-05-14
申请人： MITSUI SEKITAN EKIKA KK , NIPPON STEEL CORP
发明人： OKADA YASUO , IGUCHI KENJI , NOGAMI YOSHINOBU , IMADA KUNIHIRO , MOCHIZUKI MICHIHARU
IPC分类号： C10G1/00 , C10G1/06 , C10G1/08
摘要： PROBLEM TO BE SOLVED: To provide, for a coal liquefaction process having continuous multi- stage liquefaction reactors, an effective coal liquefaction method whose operation condition is controlled, according to the progress of the reaction in liquefaction reactors, by the property of a solid org. material in samples of the contents taken out of the reactors. SOLUTION: In a coal liquefaction method where a coal is mixed with a solvent for liquefaction and a catalyst to form a slurry, and a liquefied oil is manufactured by hydrocracking the slurry under a high pressure and high temp. condition while supplying a gas mainly composed of hydrogen, its operation condition is controlled, according to the progress of the reaction in liquefaction reactors, by sampling the contents of each reactor of the liquefaction process comprising continuous multi-stage liquefaction reactors and evaluating the property of a solid org. material.

6. 发明专利

JPH10298557A LIQUEFACTION OF COAL 失效
公开(公告)号：JPH10298557A
公开(公告)日：1998-11-10
申请号：JP10924197
申请日：1997-04-25
申请人： NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： AIHARA YOICHI , IMADA KUNIHIRO , MOCHIZUKI MICHIHARU , IGUCHI KENJI , NOGAMI YOSHINOBU
IPC分类号： C10G1/06
摘要： PROBLEM TO BE SOLVED: To produce a liquefied coal wherein a solvent for liquefaction of coal to be recycled is surely judged in terms of stabilization of the solvent by determining the time when each of the concentrations of specific substances contained in the solvent result in a certain convergence and hence a recovery of stabilized liquefied oil is increased and a running time required for the stabilization is lessened. SOLUTION: This method comprises the following steps: preparing a coal slurry 4 by blending coal 1 and a solvent and catalyst for liquefying coal; producing a liquefied oil by heating and pressurizing the coal slurry 4 in the presence of hydrogen 5 so as to be subjected to pyrolysis and hydrocracking reaction; fractionating the liquefied oil into a product oil, circulating solvent 14 and liquefied residuals 13 by distillation under normal and reduced pressures; hydrogenating the circulating solvent 14 by heating and pressurizing the solvent 14 in the presence of hydrogen 15 and a catalyst for solvent hydrogenation; and recyclably employing the resultant solvent in the first slurry-preparing process. In the above liquefied process, when the variation of the respective concentrations of paraffin, pyrene, biphenyl, dibenzofuran and/or anthracene falls within the range of 2% per day, the solvent in question is judged as a stabilized solvent.

7. 发明专利

JPH07207273A LIQUEFACTION OF COAL 失效
公开(公告)号：JPH07207273A
公开(公告)日：1995-08-08
申请号：JP1777794
申请日：1994-01-19
申请人： NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： MOCHIZUKI MICHIHARU , ENDO KOHEI , IGUCHI KENJI , YAMAGIWA HISASHI
IPC分类号： C10G1/00 , C10G1/06 , C10G1/08
摘要： PURPOSE:To liquefy coal at good efficiency of reaction by grinding coal, classifying and collecting coal particles with a specified particle diameter, forming a coal slurry from the remaining coal particles, and subjecting this slurry to the step of coal liquefaction and the step of solvent hydrogenation. CONSTITUTION:Feed coal is sent from a feed tank 14 to a primary crusher 16, crushed, fed from a feeder 17 to a grinder/dryer 18, and ground and dried to a water content of about 2% with hot air sent from a hot air generator 19. About 150mum or larger coarse particles are recycled from a classifier 20, and about below 150mum particles are classified into 32mum or coarser particles and 32mum or finer particles with a dry classifier 24, the 32mum or finer particles containing 7% or above CaO, SiO2 and Fe2O3 are discharged from the system, and the 32mum or finer particles having a CaO content of 7% or below and the 32mum or coarser particles are sent to a coal weighing tank 23. These coal particles are mixed with a liquefaction solvent and a liquefaction catalyst, slurried, and subjected to a liquefaction reaction under applied heat and pressure in the presence of hydrogen. The liquefied oil is separated into a solvent and residues, part of the solvent is hydrogenated, and the formed oil is recycled as a coal liquefaction solvent.

8. 发明专利

JPH11335674A ESTIMATION OF PRODUCT IN COAL LIQUEFYING REACTION 失效
公开(公告)号：JPH11335674A
公开(公告)日：1999-12-07
申请号：JP7861299
申请日：1999-03-23
申请人： NIPPON CORN OIL KK , MITSUI SHIPBUILDING ENG , NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： NAMIKI YASUKI , KOBAYASHI MASATOSHI , KIDOGUCHI AKIRA , ITO HIDENOBU , HIRAIDE MASATAKA , IMADA KUNIHIRO , IGUCHI KENJI
IPC分类号： C10G1/06 , C10G1/00
摘要： PROBLEM TO BE SOLVED: To provide a technique for estimating and simulating by which the amount of a produced liquefaction product can be estimated by using a true residence time in a coal liquefying reaction. SOLUTION: This method comprises estimating the amount of outflow for each component of an effluent from a coal liquefying reactor composed of a high-temperature and high-pressure vessel type reactor, assuming the amount of the outflow for each component of the effluent and calculating the vapor-liquid equilibrium composition of the mixture of the composition in the reactional vessel, further calculating the volume flow rates of the vapor phase and the liquid phase in the reactional vessel, calculating the residence times in the reactional vessel of the vapor phase and liquid phase from the gas holdup in the reactional vessel calculated from the volume flow rate and an empirical formula, calculating the amount of outflow for each component of the effluent from a rate equation of first-order irreversible reaction derived from the residence times in the reactional vessel, the amount of the inflow for each component of an inflow material into the reactor and a specific coal liquefying reactional model, comparing the initially assumed amount of the outflow for each component with the amount of the outflow for each component obtained by the calculation and repeating a series of calculations until the two amounts of the outflow for each component coincide within the range of a constant error for each component.

9. 发明专利

JPH10298559A MEASUREMENT OF RESIDENCE TIME OF COAL SLURRY IN LIQUEFACTION TOWER AND LIQUEFACTION OF COAL THEREBY 失效
公开(公告)号：JPH10298559A
公开(公告)日：1998-11-10
申请号：JP10924097
申请日：1997-04-25
申请人： NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： IKEDA KOICHI , IMADA KUNIHIRO , IGUCHI KENJI , NOGAMI YOSHINOBU , TAKEDA TETSUYA
IPC分类号： C10G1/06 , C10G1/08
摘要： PROBLEM TO BE SOLVED: To provide a method for easily measuring the residence time of coal slurry in a liquefying reaction tower under such a severe condition as high temperatures and pressures without the need of using any hard-to-estimate value, by determining the residence time grounded on a pressure difference within the tower and flow rate of the slurry at the outlet of the tower. SOLUTION: This method for measuring the residence time of coal slurry in a reaction tower for coal liquefaction, which is closely involved in the liquefying characteristics, is directed to such a coal liquefaction process that a coal, liquefying solvent and catalyst are blended for the coal slurry and a liquefying gas is fed into the resultant slurry for hydrocracking in the tower for the coal liquefaction under high temperatures and pressures, and the measurement is conducted by determining a pressure difference within the tower and flow rate of the slurry at the outlet of the tower. The pressure difference measurement is carried out e.g. by using a unit 3 composed of a couple of pressure sensing nozzles 4, 4 inserted into two vertically different positions in the tower 1 and a pressure difference sensing device 5 connected with the couple of nozzles 4, 4 to measure the pressure difference between the couple of nozzles 4, 4 a vertical length H apart from each other. The flow rate of the coal slurry is pref. estimated by sampling the slurry from inside the tower 1 to determine the amount and composition of the sample.

10. 发明专利

JPH09296182A LIQUEFCTION OF COAL 失效
公开(公告)号：JPH09296182A
公开(公告)日：1997-11-18
申请号：JP11252796
申请日：1996-05-07
申请人： NIPPON STEEL CORP , MITSUI SEKITAN EKIKA KK
发明人： ITONAGA MASUMI , IMADA KUNIHIRO , IGUCHI KENJI
IPC分类号： C10G1/06
摘要： PROBLEM TO BE SOLVED: To stably liquefy coal in a constant reactional state by keeping the volume ratio of the vapor phase and a liquid and a solid phases in a reactional column constant, carrying out the hydrogenolysis of a coal slurry, providing a liquefied oil, distilling the liquefied oil, hydrogenating the resultant medium oil and heavy oil, affording a solvent and circulating the resultant solvent for use. SOLUTION: A solvent for liquefying coal is mixed with the coal and a catalyst for liquefying the coal to provide a coal slurry, which is then pressurized and heated in the presence of hydrogen. The volume ratio (Rv ) of the vapor phase and the liquid and solid phases in a mixed phase stream flowing in the container is measured with a CT sensor part 2 and a CT image reconstructing part 6 installed in the reactional column 1 and one or more of the opening of a hydrogen gas flow regulating valve 8, the opening of a coal slurry flow regulating valve 10 and the pressure of the introduced hydrogen are operated and controlled so as to keep the Rv constant. Thereby, hydrogenlysis is carried out to afford a liquefied oil, which is then distilled. Apart or all of the resultant medium oil is mixed with all of the heavy oil, heated and pressurized in the presence of a catalyst for hydrogenating the solvent and hydrogenated to provide a solvent for liquefying the coal. The resultant solvent is then circulated for use in slurrying.

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