• 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 provides a process for the liquefaction of coal. The comminuted coal is slurried in a solvent or pasting oil and digested, normally under hydrogen pressure, e.g. of 50 to 250 atmospheres partial pressure, under catalytic conditions, at temperatures between about 380 DEG and 500 DEG C., preferably 400 DEG to 470 DEG C. and residence times between about 10 and 100 minutes. The solvent or pasting oil is obtained wholly or mostly by recycling from the distilled fractionation of the reaction products. The solvent system comprises a light fraction in the boiling range up to 200 DEG C. and a heavy residue fraction, boiling mainly above 450 DEG C., there being a more or less well-defined lack of solvent in a boiling range intermediate between 200 DEG and 450 DEG C. Preferably less than 20%, e.g. 5% or less of the solvent system boils between 200 DEG and 450 DEG C. The ratio of low boiling to high boiling solvent is preferably from about 3:1 to 1:3. The process can be controlled so that the coal is converted virtually completely into distillable products, more particularly predominantly in the crude diesel fuel range (200 DEG to 450 DEG C.). Optionally fractionating residue may be recovered as a further valuable product for making exceptionally high grade electrodes by delayed coking at 500 DEG C. followed by graphitization at 1400 DEG C.
    公开号:SU908251A3
    申请号:SU782699000
    申请日:1978-12-20
    公开日:1982-02-23
    发明作者:Клейнян Корнелис；Джон Бойкес Квинтин；Джеймс Драй Леонард
    申请人:Сазол Эен Беперк(Фирма)；
    IPC主号:
    专利说明:

    5) METHOD FOR PRODUCING LIQUID AND GASEOUS PRODUCTS FROM COAL.
    one
    The invention relates to methods for producing liquid and gaseous products from coal and can be used in the chemical industry and the synthetic fuel industry.
    Methods are known for producing liquid products from coal by thermal dissolution of the latter in the presence of both hydrogen donor compounds (tetralin, tetrahydroquinoline) and aromatic hydrocarbons in the subcritical and supercritical states 1 and 12.
    The closest to the invention is a method of obtaining liquid and gaseous products from coal by mixing crushed coal with a solvent boiling at 35-200 ° C, hydrogenating the resulting suspension at, for example, 380-500 ° C under pressure in the presence of hydrogen and a catalyst, fractionating received products-
    recirculating solvent for coal blending 3.
    However, in this method, the total yield of liquid products does not exceed 5 57 by weight of dry coal. The output of the diesel fraction, therefore, is a negligible amount of the output of the liquid products. The purpose of the invention is to increase the yield of the diesel fraction.
    This goal is achieved by the fact that according to the method of obtaining liquid and gaseous products from coal by mixing crushed coal with
    15 solvent boiling at 35–200 ° C, hydrogenating the resulting suspension at 380–500 ° C and elevated pressure in the presence of hydrogen and a catalyst, fractionating the resulting liquid products with recirculation to mix with the crushed carbon solvent in a mixture with the fraction obtained by fractionation liquid products having an initial boiling point of 39, an end of boiling of 450-BOO C, solidifying at 20 ° C and liquid at the hydrogenation temperature of a suspension taken in a solvent: fraction 20-80: 80-20. Distinctive features of the method are that the solvent is recycled in a mixture with a fraction obtained by fractionating liquid coal products having a boiling point of 350-480, a boiling point of an SO-BOO solidifying at 20 ° and liquid at the suspension hydrogenation temperature in the indicated ratio . FIG. 1-2 shows the schemes for implementing the proposed method. The method can be carried out periodically or continuously. Continuously, the method can be carried out according to the principle of the technological scheme presented in figure 1. According to this scheme, the crushed coal, along with the solvent boiling at 35–200 ° C, is fed via line 1 to tank 2, in which coal is prepared. The coal slurry through line 3 is fed to the reactor 4 for hydrogenation at 380-500 ° C and elevated pressure in the presence of hydrogen and an isator. The reaction products through line 5 are fed to a separator 6, in which the unreacted part of the coal is separated, including the ash discharged through line 7. The reaction products are removed through line 8 and partially condensed to separate the gas, which is removed from the process through line 9. The resulting condensate is fed via line 10 to a distillation column II, from which a fraction boiling at 35-100 ° C is withdrawn via line 12, and a benzene fraction boiling at 100-200 ° C is withdrawn through line 13; 14 is fed to the parator 6, and the residue is recycled through line 15 to mix with the grinding nnym coal. In addition, a distillation fraction boiling at 200-450 ° C is removed from a distillation column through line 16, and a fraction having a boiling point of 350-480 ° C and a final boiling point of 450-600 ° C hardening at 20 ° C and liquid at the suspension hydrogenation temperature (high boiling fraction). The scheme of the method presented in Figure 2 differs from the scheme shown in Figure 1 in that the separation of gas from the reaction products withdrawn along line 9 is carried out before the separation of unreacted coal, including ash. The resulting condensate is fed via line 18 to the distillation device 19, from which the head fraction is withdrawn via line 20, which is then fed to column 21 for fractionation. At the same time, from the device 19, through line 22, the fraction having a boiling point of 350 -, an end of boiling at 450-600 ° C, solidifying at 20 ° C and liquid at the suspension hydrogenation temperature is withdrawn. This fraction, together with the solvent boiling at 35-200 ° C discharged from column 21 via lines 23 and 24, is fed to a separator 25, for example a rotating filter, to separate unreacted coal, including ash. In addition, a diesel fraction is withdrawn from columns 21 via line 26. The liquid products obtained in the separator 25, containing the indicated high boiling fraction and dissolving in the specified ratio, are fed to tank 2 through line 27. Example 1. After washing, Waterberg grade coal is ground in nopoiuoK (12 mm) and saturated with ammonium molybdate solution. After drying, the crushed coal containing 2.9 wt. I Mooo, and an amount of 400 g is fed to a 5 l autoclave, which also serves 2.6 g of sulfur, 600 t of toluene and 600 g of a fraction having a boiling start of 400 ° C and a boiling end of 550 ° C (weight ratio of toluene: fraction 400- 550С 50:50). The autoclave is closed and purged with nitrogen, then set, hydrogen pressure. During these, heated to 450 ° C and for 75 minutes, constantly stirring. this temperature is maintained, the total pressure being 200 these. The autoclave is then cooled to 350 ° C and connected to a refrigeration metering system, with the temperature of the last cooler being minus 60®C. The volatilating gas is measured and, after leaching, the hydrogen sulfide is collected in a vessel. The gas is subjected to mass spectroscopy. At the end of the gas removal from the hot autoclave, pyridine (800 ml) is fed under nitrogen pressure to quantitatively wash out the contents of the autoclave. The contents of the autoclave are thoroughly mixed, cooled to room temperature and filtered under pressure. The pyridine filtrate and all the condensate obtained from a hot autoclave is processed by fractional distillation. The resulting high boiling point fraction CtOO-SSO C) is again used to prepare coal slurry. The resulting products and their output are given in table. 1 Table 1 Output (% of dry, ash-free coal coal) 200-400 C COx,,, NHj The output of the diesel fraction is 59.5 wt. % of the yield of all hydrocarbon products or 73.3 weight. I from the exit of liquid fractions. PRI mme R 2. The method is carried out as in example 1. In this case, 80 g of crushed coal containing 0.5 wt. % Mool, 12C g of toluene, 120 g of the fraction having a boiling point of AOO ° C and a boiling point of 550 ° C (weight ratio of toluene: fraction: AOO-550 ° C 50:50) and 0.8 g of sulfur. In this case, hydrogenation is carried out at and at a pressure of 210 atm for 30 minutes. At the end of the reaction, the hydrogenation products are removed by passing 2000 ml of toluene through the autoclave at 27 ml / min. Then they are fractionated. The high boiling fraction thus obtained (59 ° C) is again used to prepare a coal slurry. The resulting products and their output are given in table.
    table 2

    Output (% by weight of dry, ash-free coal)
    12.7
    HHH S -2bo C 11.9 200N Oh, Nepr angle
    An example. The method is carried out under the conditions of Example 3. Bituminous coal is used as a feedstock.
    权利要求:
    Claims (3)
    [1]
    1. The US patent W 4119524, CL.208-th, published. 1978
    [2]
    2. Patent SShdi 4036721, kl.208-8, published, 1977 ..
    [3]
    3. US Patent W 4019975, class, 208-10 rubles. 1977 (prototype).
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    类似技术:
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    同族专利:
    公开号 | 公开日
    DE2855403A1|1979-07-05|
    FR2412600A1|1979-07-20|
    JPS54122305A|1979-09-21|
    GB2010897A|1979-07-04|
    AU4269578A|1979-06-28|
    BR7808376A|1979-08-07|
    AR218093A1|1980-05-15|
    PL211975A1|1979-08-27|
    AU521473B2|1982-04-01|
    IN151254B|1983-03-19|
    FR2412600B1|1985-07-26|
    GB2010897B|1982-05-19|
    US4251346A|1981-02-17|
    CA1120879A|1982-03-30|
    DE2855403C2|1983-12-15|
    JPS5822500B2|1983-05-09|
    ZA777585B|1979-06-27|
    PL115243B1|1981-03-31|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    FR721779A|1930-08-19|1932-03-08|Ici Ltd|Hydrogenation process under pressure of solid carbonaceous materials|
    GB494834A|1937-02-01|1938-11-01|Ig Farbenindustrie Ag|Improvements in or relating to the extraction of bituminous or brown coal and like solid carbonaceous materials with solvents at high temperatures|
    FR833774A|1937-02-18|1938-10-31|Int Hydrogenation Patents Co|Process for preparing hydrocarbons of interest by destructive hydrogenation of solid carbonaceous materials|
    US3518182A|1968-03-29|1970-06-30|Chevron Res|Conversion of coal to liquid products|
    GB1261707A|1968-06-21|1972-01-26|Coal Industry Patents Ltd|Improvements in and relating to the extraction of materials|
    US3563884A|1968-07-15|1971-02-16|Lummus Co|Delayed coking of coal tar pitches|
    US3540995A|1968-11-14|1970-11-17|Us Interior|H-coal process:slurry oil system|
    US3799865A|1971-11-30|1974-03-26|Nittetsu Chem Ind Co|Process for producing needle-shaped coal pitch coke|
    GB1481689A|1973-11-08|1977-08-03|Coal Ind|Hydrogenation of coal|
    GB1481690A|1973-11-27|1977-08-03|Coal Ind|Hydrogenative treatment of coal|
    GB1481800A|1973-12-12|1977-08-03|Coal Ind|Production of coke|
    US4045329A|1974-01-21|1977-08-30|Hydrocarbon Research, Inc.|Coal hydrogenation with selective recycle of liquid to reactor|
    GB1534332A|1976-01-28|1978-12-06|Veba Chemie Ag|Process for the extraction of coal|
    GB1584306A|1976-08-05|1981-02-11|Exxon Research Engineering Co|Coal liquefaction|GB2051855B|1979-06-18|1983-09-14|Sasol One Ltd|Converting coal into liquid products|
    DE2945353A1|1979-11-09|1981-05-21|Linde Ag, 6200 Wiesbaden|METHOD AND DEVICE FOR CARRYING OUT STRONG EXOTHERMAL REACTIONS|
    DE3038842C2|1980-10-15|1986-06-19|Bergwerksverband Gmbh, 4300 Essen|Process for increasing coal oil recovery from carbohydrate hydrogenation|
    JPS58500169A|1981-07-14|1983-02-03|
    US4402821A|1981-11-13|1983-09-06|Mobil Oil Corporation|Process for liquefaction of coal|
    DE3150991A1|1981-12-23|1983-06-30|Imhausen-Chemie GmbH, 7630 Lahr|METHOD FOR CONTINUOUS PRESSURE HYDRATION OF COAL|
    US4476009A|1983-03-24|1984-10-09|Texaco Inc.|Process for improving the hydrogen donor properties of a coal liquefaction solvent|
    US4609455A|1983-10-19|1986-09-02|International Coal Refining Company|Coal liquefaction with preasphaltene recycle|
    US4510040A|1983-11-07|1985-04-09|International Coal Refining Company|Coal liquefaction process|
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    US4596650A|1984-03-16|1986-06-24|Lummus Crest, Inc.|Liquefaction of sub-bituminous coal|
    DE3420197C2|1984-05-30|1987-06-04|Ruhrkohle Ag, 4300 Essen, De|
    US4737267A|1986-11-12|1988-04-12|Duo-Ex Coproration|Oil shale processing apparatus and method|
    US5338441A|1992-10-13|1994-08-16|Exxon Research And Engineering Company|Liquefaction process|
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    RU2323247C2|2003-08-01|2008-04-27|Дзе Проктер Энд Гэмбл Компани|Fuel for jet engine, gas turbine, rocket engine and diesel engine|
    US20090229463A1|2008-02-15|2009-09-17|Coalstar Industries, Inc.|Apparatus and processes for production of coke and activated carbon from coal products|
    US20110044881A1|2009-08-21|2011-02-24|Stansberry Peter G|Method For The Catalytic Extraction Of Coal|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ZA00777585A|ZA777585B|1977-12-21|1977-12-21|Process for coal liquefaction|
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