• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention is an improvement in the process for hydrogenation of a finely divided coal and oil slurry wherein the improvement comprises subjecting the hydrogenation products to a first phase separation to obtain a liquid fraction and a gaseous fraction. The gaseous fraction is subjected to a second phase separation to obtain a liquid fraction having a boiling range between about 200 DEG C. and about 500 DEG C., which fraction is used to preheat the coal and oil slurry by direct mixing therewith.
    公开号:SU722490A3
    申请号:SU772541902
    申请日:1977-11-10
    公开日:1980-03-15
    发明作者:Вюрфель Хельмут
    申请人:Саарбергверке Аг (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a method of carbon liquefaction by catalytic oxidation and can be used in the coal industry. Coal liquefaction methods are known using 11D2 hydrogenation processes. The closest to the invention is a method of hydrogenating coal by mixing the latter with thickened oil to obtain coal slurry, feeding it under pressure for heating and then for catalytic hydrogenation in the presence of hydrogen 3, Cobalt, molybdenum, nickel, iron carrier x. Hydrogenation is carried out at 400-450 ° C, pressure 70-210 atm. The resulting hydrogenation products are separated by gaseous and liquid phases. Liquid hydrogenation products obtained from the distillation of the liquid phase, the oil fraction and bottoms are partially recycled for mixing with the coal mixture supplied for heating. When such a process is carried out, compounds that are difficult to hydrogenate and which impede the process are difficult to hydrogenate. In addition, difficulties arise during the heating of the initial mixture and recirculation supplied for the hydrogenation due to the high viscosity of the feed, as well as the swelling capacity of the coal in the heating apparatus. This leads to the need to move the coal slurry with the aid of strong pulsations, as a result of which the equipment used is greatly worn out. The aim of the invention is to increase the efficiency of the method. This goal is achieved by the proposed method of coal hydrogenation by mixing crushed coal with trowel oil to obtain coal slurry, feeding it under pressure for heating and then for catalytic hydrogenation in the presence of hydrogen. the subsequent separation of the hydrogenation products into gaseous and liquid phases, condensation of the gaseous phase at a pressure equal to the hydrogenation pressure, and partial recirculation of the mixture to the coal mixture obtained
    at condensation of fraction with t, kip. 200-500 0,
    Preferably, the fraction with bp 200-500 s is heated before mixing with the coal mixture and 10-30 wt.% Of this fraction is fed to catalytic hydrogenation to control the hydrogenation temperature.
    Distinctive features of the method are to conduct condensation of the gaseous phase at a pressure equal to the hydrogenation pressure, partially recycling to the coal mixture obtained during condensation of the fraction with m.p. 200500 ° C, as well as in the preferred process conditions.
    A schematic diagram of the method is shown in the drawing.
    Fine-grained coal in line 1 serves B mixer 2. Here in line 3 serves trowel oil. The amount of coal in the mixture is 58-60% by weight, oil 4042% weight.1.
    The mixture is compressed using a pump 4 to a pressure of about 200 bar, heated in series-connected heat exchangers 5 and b (also due to the direct introduction of a hot hydrocarbon fraction into it) up to 400 ° C and fed to the hydrogenation reactor 7, where in the presence of Hydrogen and catalyst are hydrogenated and hydrogenated at moderate temperatures. Hydrogen required for the reaction is fed through line 8. Inside the reactor 7 there is an open center at both ends. A tube 9 inside which the reaction mass moves upward according to the airlift principle. Outside the pipe, the flow is directed in the opposite direction; as a result, the hot reaction mass from the upper part of the reactor continuously flows downwards, where it is intensively mixed with the mixture of coal and oil. The latter is thereby heated to an initial hydrogenation temperature of about 430 ° C.
    The head fraction from reactor 7 is sent to reactor 10,
    The head fraction of the reactor 10 is the target product and consists of gaseous low-boiling hydrocarbons, higher-boiling liquid hydrocarbons and solids, such as unreacted ash coal, catalyst particles.
    In addition, this fraction contains hydrogen and water vapor. The fraction is sent to a hot separator 11, in which at a temperature of about. 430 ° C phase separation occurs.
    In the lower part of the hot separator, the liquid phase containing solids is collected, which is withdrawn through line 12. The oil contained in this fraction can be used as a trowel.
    The fraction formed at the top of the hot separator is transferred to a heat exchanger 6, where it is cooled to approximately 370 ° C, partially coended, and then subjected to phase separation in the separator 13.
    In the lower part of the separator, a liquid fraction is collected with a boiling point temperature of 280-420 ° C (medium and heavy oil). A portion of this fraction is fed by pump 14 through lines 15 and 16 to be mixed with a mixture of coal and zatironoy oil, as a result of which it is diluted and further heated. Another part of the fraction can be sent via line 17 directly to reactor 10 to ensure a stable temperature.
    Heating the feed to the onset temperature — the hydrogenation reactions in reactor 7 can be accelerated using heat exchanger 18.
    The advantage of this additional preheating in comparison with the heating of a mixture of coal with trowel oil is a much lower tendency in this case of coal to carbonization.
    In addition, a significant amount of hydrogen is dissolved in the liquid phase separated in the separator 13, which, together with the liquid phase, again enters the hydrogenation reactor.
    A portion of the liquid phase from the separator 13 through lines 19 and 20 is fed to a distillation column 21; where it is divided into oil fractions by diverting along the lines indicated by 2
    The head fraction from the separator 13 through line 23 is sent to the heat exchanger 5, where it is cooled by indirect heat exchange with the original coal mixture of coal with trowel oil, partially condensed and then subjected to phase separation in the separator 24. The hydrogen-containing gas that forms as a head fraction , is fed through line 25 to the stage of washing under pressure with oil into the apparatus 26, then by pump 27 through line 28 is recycled to the system.
    The liquid product from the bottom of the separator containing medium oil, naphtha and water, is passed along lines 29 and 20 to a distillation column 21.
    During the distillation process, along with the separation of water, the fractions are separated into oil fractions, which are also diverted via lines 22. Some distillation products can be supplied via line 30 to mixer 2 as trowel oil.
    Further processing of the fractions withdrawn along lines 22 into products such as gasoline, fuel oil, wasp, and is carried out, in particular, by hydrocracking. It is important that the indicated fractions do not contain impurities of high-boiling components C, for example, asphaltenes deposited on the catalysts used). Such impurities may be entrained in the head fraction of the hot separator 11, then enter the liquid phase discharged from the separator 13 and into the distillation column 21.
    To prevent this, it is expedient to thoroughly clean the head fraction removed from the hot separator 11. The cleaning is carried out not directly in the hot separator 11. For this, part of the liquid phase of the separator 13 is fed through line 31 to the top of the hot separator 11. As a result, the mass exchange of the liquid fraction with vapors contaminated with high-boiling components, in particular asphaltenes, increases in intensity due to the nozzle 32, a so-called rectification occurs, during which the liquid phase partially evaporates, part of the vapors of the high-boiling components condenses
    Asphaltenes are washed out, which fall into the liquid fraction, collecting at the bottom of the hot separator.
    In this way, the head fraction of the hot separator can be cleaned and its temperature can be regulated, which is of great importance, since in order to avoid coking, the hot separator can be efficiently operated only in a narrow temperature range.
    In addition, the heat generated during the condensation of high-boiling components returns to the process. At the same time, by changing the amount of liquid phase supplied through line 31, the working temperature of the hot separator and, consequently, the condition of separation in it, will be eliminated over a wide range.
    Under certain conditions, it is advisable to transfer to the hot separator 11 instead of the liquid fraction separator 13 a part of the liquid fraction with a lower boiling point of the separator 24 or a mixture of these fractions,
    PRI me R. The raw material used is coal, which has the following characteristics: the content of volatile substances in the anhydrous and ashless state is 40%, the ash content is 6.6%, the calorific value is 31520 kJ / kg,
    The elemental composition of coal in the anhydrous state:
    83.4
    Carbon 5.4
    Hydrogen
    Oxygen 9.0
    Nitrogen 1.5
    0.99
    Sulfur
    0.52
    Chlorine
    Fluorine 0.003
    Carbonate (SOL)
    1.32
    250 t / h of finely ground coal is fed to mixer 2 via line 1, 169.4 g / h of trowel oil through line 30, and also 4 t / h as catalyst. Coal pulp is obtained as a result of mixing. Last contains {weight,%) 60 solids fi 40 oils, 423.4 t / h of coal Xsica
    5 with a pump 4 is brought to a pressure of 200 bar, heated in heat exchangers 5 and 6, as well as by direct supply of the hot hydrocarbon fraction to a temperature of 400 s
    0 and fed to the reactor 7, in which coal is hydrogenated in the presence of hydrogen and a catalyst at an average temperature of 470 ° C.
    5 lines 8 13.6 t / h of hydrogen, 1 The fraction formed in the upper part of the reactor 7 is fed to the reactor 10,
    The head fraction of the reactor 10 is fed to the hot separator 11 and separated into phases at 450 ° C,
    The liquid fraction of the hot separator 11 is withdrawn via line 12 and fed to a vacuum distillation unit (not shown). From this unit, 45 t / h of oil is fed through line 30 to mixer 2 as a mat oil,
    In quantitative terms
    the head fraction of the hot separator is And is 628.4 t / h. This fraction, which, along with hydrocarbons at the end of the boiling point, also contains hydrogen and water vapor, is fed
    to the heat exchanger 6, where it is cooled to i as a result of heat exchange with i coal kayitsa. , in this case, a partial condensation of the fraction occurs, after which the separation of its phases is carried out in the separator 13,
    The liquid fraction of the separator 13 has a boiling point of about 280 ° C and an end of the boiling point of 420 ° C. 84.6 t / h of this fraction with pump 14 in line 15 and 160.4 t / h in line 16 are mixed
    to coal slurry, so that it is liquefied and heated.
    Part of the liquid fraction of the separator 13 can be fed through line 17 directly to the reactor 10 for
    stabilize the hydrogenation temperature.
    The remaining amount of liquid fraction separator 13 is fed through lines 19 and 20 to the distillation operating under atmospheric conditions.
    column 21,
    权利要求:
    Claims (3)
    [1]
    Claim
    1. The method of coal hydrogenation by mixing the crushed coal with grout oil to obtain coal slurry, applying it under pressure to heat and then to catalytic hydrogenation in the presence of hydrogen, followed by separation of the hydrogenation products into gaseous and liquid phases and partial recirculation of the liquid hydrogenation products into a mixture with with a coal mixture supplied for heating, it is necessary that, in order to increase the efficiency of the process, the gaseous phase is condensed at a pressure equal to w hydrogenation, ig and recycling obtained by direct condensation of the fraction with b.p.. 200-500 ° C.
    [2]
    2. The method according to claim 1, characterized in that the fraction with so Kip. 200-500 ° C before mixing with coal , this mixture is preheated.
    [3]
    3. The method according to claim 1, characterized in that, in order to. Regulate the temperature of hydrogenation,
    10-30 wt.% Fractions with so Kip. 200-
    20. 500 ° C is fed to catalytic hydrogenation.
    类似技术:
    公开号 | 公开日 | 专利标题
    US4152244A|1979-05-01|Manufacture of hydrocarbon oils by hydrocracking of coal
    US4609456A|1986-09-02|Process for converting heavy petroleum residues to hydrogen and gaseous distillable hydrocarbons
    US5811606A|1998-09-22|Process and equipment for treatment of waste plastics
    US4300998A|1981-11-17|Pre-heat vaporization system
    KR20030029842A|2003-04-16|Asphalt and resin production to integration of solvent deasphalting and gasification
    US5064523A|1991-11-12|Process for the hydrogenative conversion of heavy oils and residual oils, used oils and waste oils, mixed with sewage sludge
    SU722490A3|1980-03-15|Method of coal hydrogenation
    GB2191214A|1987-12-09|Production of higher molecular weight hydrocarbons from methane
    US4882037A|1989-11-21|Process for treating a temperature-sensitive hydrocarbonaceous stream containing a non-distillable component to produce a selected hydrogenated distillable light hydrocarbonaceous product
    US4401561A|1983-08-30|Hydrotreating process with ammonia injection to reaction zone effluent
    CA1226840A|1987-09-15|Low temperature carbonization process for coalhydrogenation residues
    EP0116180B1|1988-03-16|Process for smoldering hydrogenation residues
    JPH0678527B2|1994-10-05|Method of catalytic hydrogenation of coal
    US2137275A|1938-11-22|Process of reconstituting and dehydrogenating heavier hydrocarbons and making an antiknock gasoline
    CA1155411A|1983-10-18|Process for hydrogenation of coal
    US4421632A|1983-12-20|Process for hydrogenation of coal
    CA1158191A|1983-12-06|Method for hydrogenating coal
    US4983279A|1991-01-08|Process for the hydrogenation of liquid charge materials which contain carbon
    US1995604A|1935-03-26|Process for producing high grade motor fuel by destructive hydrogenation in a series of conversion stages
    SU1240364A3|1986-06-23|Method of producing liquid hydrocarbons from coal
    US1951792A|1934-03-20|Process for hydrogenating hydrocarbon oils
    CA2238341C|2000-05-16|Process and apparatus for treatment of waste plastic hydrocarbons
    US4159936A|1979-07-03|Process for hydrogenized reconditioning of crude oil or residues derived therefrom into saturated light hydrocarbons
    CA1233777A|1988-03-08|Cleavage and hydrogenation of refractory petroleumresidue products, such as asphaltenes, resins and the like
    US2119350A|1938-05-31|Cracking of liquid hydrocarbon products
    同族专利:
    公开号 | 公开日
    AU3054477A|1979-05-17|
    GB1539648A|1979-01-31|
    DE2651253A1|1978-05-11|
    AU505371B2|1979-11-15|
    PL111846B1|1980-09-30|
    ZA776600B|1978-08-30|
    PL201984A1|1978-07-17|
    DE2651253C2|1984-03-08|
    JPS5384008A|1978-07-25|
    CA1103183A|1981-06-16|
    US4214974A|1980-07-29|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2445343C1|2010-12-09|2012-03-20|Общество с ограниченной ответственностью "Олимпик Интегратор" |Method for direct coal liquefaction|DE677647C|1930-01-18|1939-06-30|I G Farbenindustrie Akt Ges|Process for the processing of pressure hydrogenation products from carbons, tars or mineral oils|
    US2087608A|1932-12-22|1937-07-20|Standard Ig Co|Process for hydrogenating distillable carbonaceous materials|
    US2100352A|1933-01-17|1937-11-30|Ig Farbenindustrie Ag|Catalytic reaction|
    DE933648C|1953-06-27|1955-09-29|Basf Ag|Process for the production of solid and asphalt-free and low-sulfur heavy oil|
    US3321393A|1965-05-10|1967-05-23|Hydrocarbon Research Inc|Hydrogenation of coal|
    US3488280A|1967-05-29|1970-01-06|Exxon Research Engineering Co|Catalytic hydrogenation of coal with water recycle|
    US3519554A|1968-04-08|1970-07-07|Hydrocarbon Research Inc|Residuum recovery from coal conversion process|
    US3652446A|1969-11-17|1972-03-28|Exxon Research Engineering Co|Combination process for liquefaction of coal and catalytic cracking of selected fractions thereof|
    US3823084A|1972-06-30|1974-07-09|W Schroeder|Hydrogenation of coal|
    GB1481689A|1973-11-08|1977-08-03|Coal Ind|Hydrogenation of coal|
    US4097361A|1976-08-24|1978-06-27|Arthur G. Mckee & Company|Production of liquid and gaseous fuel products from coal or the like|
    DE2654635B2|1976-12-02|1979-07-12|Ludwig Dr. 6703 Limburgerhof Raichle|Process for the continuous production of hydrocarbon oils from coal by cracking pressure hydrogenation|DE2943494C2|1979-10-27|1987-04-16|Basf Ag, 6700 Ludwigshafen, De|
    DE3031477C2|1980-08-21|1986-09-18|Saarbergwerke AG, 6600 Saarbrücken|Process for hydrogenating coal|
    US4421632A|1980-09-04|1983-12-20|Wuerfel Helmut|Process for hydrogenation of coal|
    DE3042984C2|1980-11-14|1986-06-26|Saarbergwerke AG, 6600 Saarbrücken|Process for hydrogenating coal|
    US4485008A|1980-12-05|1984-11-27|Exxon Research And Engineering Co.|Liquefaction process|
    DE3585485D1|1984-09-13|1992-04-09|Ruhrkohle Ag|METHOD FOR SETTING THE PROCESS WITH HEAT RECOVERY FOR THE HUMP PHASE HYDRATION WITH INTEGRATED GAS PHASE HYDRATION.|
    DE3505553C2|1985-02-18|1987-04-30|Veba Oel Entwicklungs-Gesellschaft Mbh, 4650 Gelsenkirchen, De|
    DE3523709A1|1985-07-03|1987-01-08|Veba Oel Entwicklungs Gmbh|METHOD FOR PRETREATING THE APPLICATION PRODUCTS FOR HEAVY OIL HYDRATION|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2651253A|DE2651253C2|1976-11-10|1976-11-10|Process for hydrogenating coal|
    [返回顶部]