• 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:
    Insoluble material is separated from a coal liquefaction product by use of a promoter liquid prepared from a fraction of the coal liquefaction product. The promoter liquid is prepared from a fraction having a 5 volume percent distillation temperature of at least 250 DEG F. preferably at least 400 DEG F. and a 95 volume percent distillation temperature of at least 350 DEG F. and no greater than 750 DEG F. by hydrogenating the fraction to raise the characterization factor thereof to at least 9.75.
    公开号:SU718016A3
    申请号:SU731975277
    申请日:1973-11-06
    公开日:1980-02-25
    发明作者:К.Се Морган；Дж. Снелл Джордж
    申请人:Дзе Ламмас Компани (Фирма)；
    IPC主号:
    专利说明:

    partially hydrogenated naphthalenes, three-sided naphthalenes and tetrahydronaphthalene, so that the liquefied coal product can be discharged to such an extent that its ash content is less than the weight. and ash removal is carried out exclusively by gravity sedimentation. The characteristic factor is an indicator of the degree of aromatization of the paraffininess of hydrocarbons and petroleum distillates, with most paraffinic substances having a higher characteristic factor. The second solvent used in the decalting is one solvent which has a characteristic factor of more than 9.7 and which is also less aromatic than the solvent used in the hydrogenation step, i.e. the characteristic factor of the second solvent has a value that is usually 0.25 units larger than the characteristic factor of the solvent used in the hydrogenation step. The characteristic factors for various substances are given: Anthracene8.3 Naphthalene8.4 218-260s - coal distillate 8.8 287-482s - coal distillate 9.1 315-482 С - coal distillate 9.0 204-232s - coal Distillate 9.4 Petrol-9.8 Tetrahydronaphthalene 9.8 0-xylene 10.3 Decagidronaphthalene 10.6 Cyclohexane 11.0 Kerosene with a temperate boiling point 218-260 011.9 p-Dodecyl benzdl 12.0 Propylene oligomers (penzymer) 12.2 Tseten12.8 Tridecan12.8 p-hexane 12.9 Hexadecan or cetane 13.0 Amount of second solvent used to enhance the separation of sulfur solids from the hydrogenation products of coal, and varies depending on the liquid used, the solvent for hydrogenating the coal, the coal used as the starting material, and the method of performing the hydrogenation should be minimized to reduce the total cost of the process. . In general, the weight ratio of the second solvent to the carbon solution may be in the range of 0.2: 1 to 3, preferably from 0.3: 1 to 2.0: 1 and, most preferably, from 0.3: 1 to 1.5: 1. It should be noted that the second solvent can be obtained by hydrogenation of the fraction obtained from the coal extract. In particular, the fraction having a distillation temperature of 5 vol. % 12lc and a distillation temperature of 95% by volume of 177-399 ° C, which is necessary for the second solvent, is obtained from the coal product by fractional distillation. In general, such a fraction is in excess compared with the fraction required to obtain the second solvent (a product having a distillation temperature of 5% by volume and 95% by volume, identical to the temperatures of the second solvent distillations, is continuously formed during coal hydrogenation) and, accordingly, only one part of the fraction is used to produce the second solvent, while the remainder forms part of the finished hydrogenation product. . The natural fraction, which in the cocoa count should be used as a second solvent, should be subjected to controlled hydrogenation to obtain a second solvent having the required degree of aromatization, i.e., a characteristic factor above 9.75. In accordance with the present invention, all or part of the fraction is subjected to hydrogenation in a known manner to produce a second solvent having the required characteristic factor. Typically, such hydrogenation is dried at a temperature of about 232454 ° C and a pressure of about 28.1140, 6 kg / cm in the presence of a suitable hydrogenation catalyst, for example, nickel tungsten sulfide, nickel molybdate, nickel molybdenum sulphide. It should be understood, however, that the invention should not be limited to such conditions, hydrogenation does not form part of the invention, except that they are used to obtain a liquid solvent having the necessary characteristic factor. The second solvent can also be prepared by mixing a substance having a characteristic factor below 9.75, with a substance having a characteristic factor above 9.75, the resulting mixture has a characteristic factor above 9.75 and boiling characteristics such as described above. The use of mixed substances is a convenient way to regulate the characteristic actor. The products of hydrogenation of coal before mixing them with the second solvent are processed to separate, at least, those components that boil until the distillation temperature reaches 96 vol. % of second solvent. With this products. hydrogenation of coal is free from components that boil in the range of components present in the second solvent, thereby contributing to the subsequent regeneration of the BT ipofo solvent from the products of coal hydrogenation. The drawing is a diagram of the installation that implements the proposed method. Milled or crushed coal, usually bituminous, sub-bituminous, or lignite, preferably bituminous, is introduced along line 1 into zone 2 of carbon solvation and suspension, along with coal hydrogenation solvent fed through line 3. The solvent for hydrogenating coal can be one of the widely used solvents containing up to hydrogen burrows, non-hydrogen donor solvents, and mixtures thereof. Thus, in particular, the solvent for the hydrogenation of coal is a solvent that is regenerated by the me product of the hydrogenation of coal and which is not subjected to the hydrogenation of its regeneration method. The solvent is added to the coal in an amount "sufficient for. carrying out the required hydrogenation and, in general, is added in an amount sufficient to provide a solvent to coal weight ratio of from 1: 1 to 20: 1 and, preferably, from 1.5: 1 to 5: 1. The coal mass is removed from zone 2 through line 4 and introduced into coal hydrogenation zone 5, in which coal is converted to liquid products. Hydrogenation zone 5 may be catalytic or non-catalytic with no or no added hydrogen. The hydrogenation can be carried out in a settled catalyst bed, in a pseudo-liquid catalyst bed, in a swelling bed or in a fluidized bed; Coal hydrogenation products, consisting of a liquid coal extract containing a carbon substance, dissolved in a coal hydrogenation solvent, and an insoluble substance (ash and unreacted coal) are removed from the hydrogenation zone 5 through line 6 and introduced into zone 7 of the separation separation from coal hydrogenation product, at least P9., those substances that boil to
    6 Achieve a distillation temperature of 95 vol. % liquid up to 287c, intended for use as a second solvent in the separation of insoluble matter. Zone 7 of the compartment may contain a chamber or tower of a suck-up pickup and is intended to separate components boiling at temperatures up to 287s. Coal hydrogenation products, free from components boiling at temperatures up to 28 ° C, are removed from the separation zone 7 via line 8, mixed with a second solvent fed through line 9, with a controlled degree of aromatization, i.e. the characteristic factor of the second solvent has a value which, in general, is 0.25 units more than the characteristic factor of the solvent for the hydrogenation ugg. As described, in particular, secondly, the solvent is the kerosene fraction, which has a distillation temperature 5 about. % and 95 vol. % in the Range, for example, 218-260 ° C and obtained from a naphthenic or paraffinic distillate. The combined stream of coal hydrogenation and second solvent products through line 10 is introduced into a separation zone 11 consisting of a gravity settling tank. The drain, usually free of insoluble matter, is removed from the separation zone 11 via line 12 and introduced into the regeneration zone 13 to regenerate the second solvent and the various fractions of the coal extract. The IS zone of regeneration may consist of one or more distillation columns. As described, in particular, the regenerated zone. The recovery of the first fraction, which has a distillation temperature of 5 vol.%, is effective. % and 95% by volume, from 216 to 2 ° C, which is used as a second solvent to enhance the separation of solids from the carbonated hydrogenation product; a second fraction (260SIS C), which can be used as a mixed feed for distillation; the third fraction (315-482С), a part of which can be used as a coal hydrogenation solvent, introduced via line 3, and another part of it, regenerated as a product with low ash content and low sulfur content, which can be used as fuel or subjected to further processing. The second solvent recovered in the regeneration zone is admixed to the hydrogenation product in the pipeline (line) 8. Additionally, the second diluent.
    The solvent can be introduced into the system through conduit 14.
    The condensed product containing the dispersed insoluble substance removed from the separation zone 11 through pipe 15, is brought into the light ends stripping zone 16, in which. the substance (boiling at a temperature below 482c, is distilled off and introduced into the regeneration zone 13 / through., pipeline 17. Rich in ashes of distillate sludge in the pipeline, 18 can then be subjected to calcination or coking.
    The invention will further be treno in the following examples. All parts and percentages are given by weight.
    All hydrogenated carbon solutions used in the following de-ashting examples, with the exception of Example 7 (40% coal and 60% solvent) were prepared from a coal mass or suspension containing 30 wt. % bituminous coal (Illinois 6) and 70% weight, 315-482% of coal distillate. This coal mass was fed together with hydrogen B an upward flow of a catalytic reactor containing a conventional catalyst. The reactor operated at temperatures and pressures within 399-454С and 70.3-140.6 kg / cm, respectively. The product flowing out of the short-circuit catalytic reactor was released after cooling to temperatures in the range of 121-204 seconds to the high-pressure separator. The contents of the separator were reduced to atmospheric pressure and the liquid product rich in ash was removed. This product will be referred to hereinafter as coal solution or ash-rich coal solution, or hydrogenated coal solution. /
    Table 1 shows the analytical data obtained for the ash-rich coal solution used in the desoldering solvents examples. .Table
    no-angle
    distillate t Kamen218-260
    , 78
    BUT coal
    distillate t
    Example, 300 g of ash-rich coal solution No.; 1 and 1200 g of liquid A are loaded into a two-liter cylindrical stainless steel cylinder with electrically heated, Ballast size: 11.74 cm in diameter and 45.7 cm in length on the straight side. The cylinder is equipped with a bottom exhaust valve. The contents of the balloon are rocked and heated bo for 30 minutes and then left to settle in the vertical. position for 4 hours at 260 ° C without hesitation. At the end of the precipitation period, 150 g of ash-rich, condensed noToi a are removed through a bottom valve. The remaining part of the contents of the cylinder is removed through the bottom valve and this poor ash solution is examined for ash content. The ash content in a lean ash solution Of 25 wt.%, Which corresponds to the removal of ash by 57%. This example illustrates the inefficiency of the aromatic type of liquid; the characteristic factor is below 9.75, despite the use of the ratio of the second solvent to the 4: 1 angle solution. PRI mme R 2. 300 g of the ash-rich solution 2 and the mixture (300 g of liquid D and 300 g of liquid B) are added to the two-liter can described in Example 1. The contents of the can are heated by rocking for 30 minutes, and then left in a vertical position to sediment for 4 hours with no reading. At the end of the precipitation period, 258 g of rich ash from the condensed stream is removed through the bottom valve. The rest of the contents of the cylinder are removed through the bottom valve, and this poor ash plant grows for ash content. The ash content in the low ash solution is 0.01 wt. %, which corresponds to the removal of ash by 98%. This example illustrates the effectiveness of a liquid mixture with a 1: 1 ratio of second solvent to carbon solution: Approx. The 1500 mm gummed glass reservoir is used in the experiment. It is equipped with a four-blade turbine stirrer, a thermometer, a heating grid, a reflux condenser and a dropping funnel. 600. g of ash-rich coal solution No. 4 is loaded into a 1500-millimeter gummed tank. The vase is heated with stirring to 30 minutes. 350 g of liquid D is added dripping over 1 hour through a dropping funnel. The stirring and internal temperature of the reservoir 17bc are maintained during the addition. The contents of the tank are stirred for an additional 30 MiiH, then the stirring is stopped and the contents of the tank are settled for 4 hours at 116 ° C. 708 g of ash-depleted drain solution is removed from the gum tank and analyzed for ash content. The quarter is then disassembled and the solution is poured from the reservoir. The ash content of the ash depleted drain solution is 0.03 wt. %, which corresponds to the removal of ash by 98.7%. This example illustrates the effectiveness of the liquid solvent of the invention, in the absence of a diluent, with a ratio of the second solvent to the carbon solution of 0.54: 1. EXAMPLE 4 The device used in this experiment is identical to that used in Example 3. 450 g of ash-rich coal solution No. 2 to 650 g of liquid B are loaded into a 1500-mm gummed tank. The mixture is heated to with stirring for 30 minutes, 100 g of liquid D is added by dripping through an addition funnel for 1 hour at. mixing and 17bs inside the tank. The contents of the tank are then mixed with an additional 30 minutes. The stirring is stopped and the contents of the tank are settled for 5 hours. 912 g of the ash-depleted drain solution is separated from the tank and subsequently analyzed for ash content. The tank is then dismantled, and 268 g of ash-rich drain solution is poured from the tank. It was found that the ash content in the ash-depleted drain solution is 0.05% by weight, which corresponds to 96.4% removal of the ash. This example illustrates the effectiveness of a second solvent with a ratio of a second solvent to a carbon solution of 1.4: 1. Example 5: A coal solution 5 rich in ashes is used for decalcification 5. The second desoldering solvent is tetra-. hydronaphthalene and is used when the weight ratio of the second solvent to the carbon solution is 2: 1, at a temperature and pressure of 14 kg / cm with a settling time of about 2 hours. The ash content in the discharge is less than 0.01 weight. %, which corresponds to the removal of ash by 99%. EXAMPLE 6 A coal solution 7 is used for de-ashing, using liquid solvent D. Experimental conditions and results are shown in Table. 3.,
    Table 3 Fluid relative to coal vapor (total) Tank temperature, C of the settling tank, 2 kg / cm Precipitation time, h Drain with ash content, wt.% Depletion of EOLA wt.% Maintenance of the fraction present in the condensed product, wt.% of eagrueck angle, and the torus between the injected fluid and the vaginal fluid
    Hexane Hexane
    D
    Table 4 extension
    The ratio of liquid to coal (weight)
    0.50
    0.59
    Temperature .With
    176:
    176 liter to coal solution (by weight), 50 Temperature, s 204204 Pressure, kg / cm 7.0 O Time precipitated 4, 04.0 ni, h Drain with ash content, 0.770.01 weight. % Ash Removal, 81.099.7 ve. % The content of the fraction + 454c present in the condensed product, wt.% From load 50, 3 26.8 ki of coal Table. 4 shows the difference in effectiveness between hexane and the second solvent of the invention. PRI me R 8. Coal solution No. 7 is deshed into the laboratory using liquid solvent D as follows (see Table 5). That blitz a 5
    Continuation of table.5
    less
    less than 0.01 0.01
    less
    less than 99.7 99.7 27, 5
    26.0
    PRI me R 9. The aromatic distillate fraction is obtained from coal hydrogenation product. It is characterized by a characteristic indicator of 8.8, and the distillation temperature range is 5 vol.% And 95ob. % 218.3-260Ci It is terminated through a preheater, mixed with the preheated hydrogen, and sent to a fixed bed catalytic reactor filled with an industrial sulfided nickel-tungsten catalyst. The purity of the hydrogen stream is 75% N. In this case, the following reaction parameters are used: the volumetric rate is 1.0 h, the operating pressure is 98.4 kgf / cm and the inlet temperature is 343.3 ° C. Hydrogen is introduced into the reactor at a rate of 4 m / l of liquid feed.
    The effluent from the reactor is rapidly cooled to a temperature of 93.3-5.5 s and directed to a high-pressure gas-liquid separator, in which the gas is continuously ventilated with automatic pressure control. At the end of the cycle, high pressure is released to atmospheric pressure, and a liquid product with a characteristic factor of 9.9 is removed from the separator.
    This hydrogenated liquid is then used to remove ash from the coal hydrogenation product, consisting of an insoluble material and a carbonaceous substance, dissolved in the coal hydrogenation solvent (coal distillate).
    315.6-482,) 12.00 g of this solution and 300 g of coal hydrogenation product are added to a two-liter stainless steel swing cylinder, electrically heated. The contents of the balloon are heated using shaking to 260 ° C for min. The contents of the balloon are then allowed to stand in a vertical
    0 position for about 4 hours at 260 ° C without any wiggle. At the end of the period, about 250 g of ash-rich sand flow is discharged through a bottom valve. The rest of the contents of the container is discharged through
    5 The bottom valve also contains 0.01 wt. In this lean skin. % solids, which corresponds to 98% ash removal. Thus, due to the invention, the insoluble substance can be separated from the coal hydrogenation product without the need for filtration. In addition, the separation of ash and insoluble matter can be brought to a maximum of 5 with minimal loss of the desired coal products obtained and with moderate amounts of the second solvent.
    0
    权利要求:
    Claims (2)
    [1]
    Invention Formula
    1. The method of de-ash products
    5 of the hydrogenation of coal, consisting in that a second solvent is added to a solution of the hydrogenation product of coal in the first solvent, characterized in that, in order to reduce the ash content in
    0 products, use a second solvent having a characteristic factor (K) of at least 9.75
    # 9 (, H5
    five
    K where Tt is the molar average boiling point of the liquid, C;
    G is the specific gravity of the liquid at, g / cm, and the characteristic factor of the second solvent is higher than the characteristic factor of the first solvent for hydrogenation of coal, the second solvent has a distillation temperature of 5 vol. % not less than the distillation temperature 95 Vol. % 177-399C.
    2. A method according to claim 1, characterized in that kerosene, kerosene fractions, lighting kerosene, light gas oil, gas oil fractions, heavy leggroins, liquid paraffin and crude oil vaseline fractions, partially hydrogenated naphthalenes are used as the second solvent. , 5
    [2]
    15
    methylene naphthalenes and tetrahydronaphthalene, -; - y --- - - 3. The method according to claim 1, in which the etothoshee second solvent to coal jpacTBopy is from 0.2: 1 up to 3.0: 1,
    4. The method according to claim 1 is distinguished by the fact that a fraction is used as the second race of the yrütel
    71X016
    sixteen
    isolated from rheezolenny coal extract, which is hydrogenated and returned to the desalination zone.
    Sources of information taken into account in the examination
    1. USA Fir Bureau Bulletin 633 Hydrogenation of coal and tar, 1968. p. 91-103.
    2. US Patent 3,607,716, Cl, 208-8, 09.21.71.
    类似技术:
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    同族专利:
    公开号 | 公开日
    DE2355539B2|1980-07-10|
    NL172871B|1983-06-01|
    DE2355539A1|1974-05-16|
    CA1005384A|1977-02-15|
    GB1452610A|1976-10-13|
    FR2205565B1|1978-08-11|
    CS186779B2|1978-12-29|
    FR2205565A1|1974-05-31|
    AU469568B2|1976-02-19|
    LU68728A1|1974-01-08|
    ZA738418B|1974-09-25|
    NL7315261A|1974-05-09|
    BE806788A|1974-02-15|
    AU6214973A|1975-05-08|
    DE2355539C3|1987-06-19|
    JPS4998402A|1974-09-18|
    NL172871C|1983-11-01|
    JPS521923B2|1977-01-19|
    US3852182A|1974-12-03|
    IT999735B|1976-03-10|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
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    US4255248A|1979-09-07|1981-03-10|Chevron Research Company|Two-stage coal liquefaction process with process-derived solvent having a low heptane-insolubiles content|
    US4264429A|1979-10-18|1981-04-28|Chevron Research Company|Two-stage coal liquefaction process with process-derived solvent|
    US4350582A|1979-10-18|1982-09-21|Chevron Research Company|Two-stage coal liquefaction process with process-derived solvent|
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    US4264430A|1979-10-22|1981-04-28|Chevron Research Company|Three-stage coal liquefaction process|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US00304320A|US3852182A|1972-11-07|1972-11-07|Coal liquefaction|
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