• 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:
    1500337 Liquefaction of coal LUMMUS CO 14 March 1975 [18 March 1974] 10847/75 Heading C5E Insoluble material including ash is separated from a coal liquefaction product by obtaining therefrom a solid-free stream and a flowable solidcontaining stream having an ash content of 6-18 wt. per cent, and stripping the latter to remove liquid components boiling at up to 900‹ F. and to leave a solid-containing stream having a benzene solubles content of at least 35 wt. per cent. Preferably the product is separated into two streams by gravity settling at 300-600‹ F. and 0-500 p.s.i.g. for 0À1-8 hours in the presence of a liquid promoter having a characterization factor (as defined) of at least 9À75, and preferably at least 0À25 higher than the liquefaction solvent. The weight ratio of promoter to liquefaction product may be 0À2-3À0. A preferred promoter is a 425-500‹ F. boiling range kerosene. Preferably two gravity settlers are used, the net overflow constituting the solid-free stream and the final underflow the solid-containing stream. The stripper may be a vacuum flash distillation tower. In an embodiment, finely-divided coal is liquefied with a 600-900‹ F. boiling range solvent, with or without added H 2 , and the extract is treated to remove components boiling at up to 600‹ F. The treated extract is then mixed with a 425-500‹ F. promoter and subjected to gravity settling. The net overflow passes to a recovery zone and the net underflow is stripped, the components separating at up to 900‹ F. being passed to said recovery zone. In the recovery zone fractionation is carried out to obtain a 425-500‹ F. promoter fraction, a 600-900‹ F. liquefaction solvent fraction and a residual fraction.
    公开号:SU953987A3
    申请号:SU752119272
    申请日:1975-03-17
    公开日:1982-08-23
    发明作者:С.Сче Морган；Дж.Снелл Джордж
    申请人:Дзе Ламмас Компани (Фирма)；
    IPC主号:
    专利说明:

    The present invention relates to methods for de-isolating products of hydrogenated coal that can be used in the chemical industry. Known methods for de-ashing treatment of hydrogen-containing products obtained by liquefying coal by means of spinning, centrifuging, and settling i. However, the effectiveness of such methods is low. Thus, during filtration, fast fusion of pores occurs with the formation of a layer of filtering material deposited on the surface of fvptra. The method of settling is characterized by a low sedimentation rate and inefficiency in the removal of ash. The centrifuging method is not efficient enough; it is due to the high cost and difficulty of transporting particulate impurities. The closest to the isofotene is the method of de-isolating the hydrogenation products of your coal by mixing the solution of coal hydrogenation products in the first solvent with a second solvent having a characteristic factor K, defined by the formula 9 (TF41TZI5 where Td is the molar average temperature). Q is the specific gravity of the liquid at 15 ° С, g / cm no less than 9.75. In addition, the second solvent has a characteristic factor faster than the characteristic 2 factor of the first solvent and has a distillation temperature of 5% by volume of not less than 121. С , The distillation temperature is 95 vol.% 177-3 9 9 ° C and contains at least 35 vol.% 2 soluble substances in benzene. Then the tar products are divided into a stream directed to fractionation and to a stream containing solid impurities and ash. The latter stream is directed to the stage of distillation of liquid products boiling at a temperature below 482 C. However, some of the distilled light fractions are lost. 3 95398 The circuit of the Invention is to reduce the loss of light fractions. This goal is achieved by the method of decontaminating coal hydrogenation products by simulating a solution of the products of coal hydrogenation products in a first solvent with a second solvent,. which has a characteristic K factor determined by the formula l9 (Tbv2T3 15 k p 7 where Tg is the molar average boiling point of the liquid, C; is q is the weight of the liquid at 15 ° C, g / cm I not less than 9.75 and higher the characteristic factor of the first solvent, 20 the distillation temperature is 5 vol.%, not less than 121 ° C, the distillation temperature is 177–399 ° C and contains not less than soluble substances in benzene Anthracene Naphthalene Coal Tar Fraction 21 Coal Tar Fraction28 Coal Tar Fraction 31 Fraction coal tar2o benzene tetrahydronaph ling O -Ksilol decahydronaphthalene Cyclohexane kerosene fraction with temperature ki 218.3 - AND -Dodeshshbenzol Oshgomery propylene (pentamer) -hexane Tseten tridecane, and hexadecane or cetane 74 35 vol% with further separation products on mixing flow on pitted emy frakiionir Jeanne and to the stream containing solid impurities and ash in the amount of 6-18 wt.%, directed to the distillation distillation of liquid products, boiling at a lower temperature with obtaining a residue after distillation with a content of soluble substances in benzene ® or less than 35 vol. % The characteristic factor K is an indicator of the degree of aromatization and paragasification of hydrocarbons and petroleum fusions. More paraffinized materials have higher values of the characteristic factor K. Since the second solvent has a characteristic factor K higher than the first (not less than 0.25), therefore it is less aromatic. For various substances, the characteristic factor K has the following meanings. , 8.3-260, 8.8 7.8 - 482, 9.1 5.6 - 482, 9.0 4.4 - 232.2 ° C 9.4 9.4. 9.8. 10.3 10.6 11.6 Pensions 11.9 12.0 12.2 12.8 12.8 12.9 13, O 595 As the second solvent, kerosene or kerosene fractions based on paraffin or mixed base, middle distillates, light gas oils are used. or gas oil fractions based on paraffinic or mixed oils, alkylated side-chain benzenes containing 10 or more carbon atoms, paraffinic hydrocarbons containing more than 12 carbon atoms, light oils or light oil fractions derived from crude oils, single olives containing more than 12 carbon atoms, fully hydr ogenetized naphthalenes and substituted naphthalenes, propylene oligomers (pentamer and above), ketrahydronaphases, heavy 4 aigia of naphtha and so on. Most preferably used are kerosene ({fractions, light oils, fully hydrogenated naphthalenes and replaced with naphthalenes and replaced with naphthalene and replaced with naphthalene and replaced with naphthalene, etc.) The amount of the second solvent used depends on its type, on the type of the first solvent, on the method of coal production. The weight ratio of the second solvent to the first is (0.2: 1) (3, O: 1), preferably (0.3: 1) (2.0: 1) and (0.3: 1) - (1, 5: 1). The drawing shows the principal scheme of the method. Ground stone powdery ugold, usually bituminous, subbiotic or lignite, mainly bituminous coal, is injected into the zone of solvating and cooking, coal paste 2, in which, through line 3, solvent is used to liquefy the coal (first solvent). Solvents are used as such solvents - hydrogen donors, solution gels that do not give up hydrogen, or their mixtures. As a rule, a solvent boiling at 315.6 482, 2C is used, which is obtained from the coal hydrogenation product. The first solvent is added to the coal in an amount sufficient to obtain the required degree of liquefaction, and, in particular, is added in an amount that provides the weight ratio of solvent to coal (1: 1) (2, O: 1), preferably (1, 5: 1) (5: 1). The coal paste from zone 2 is directed to coal hydrogenation zone 4, which can be catalytic and non-metropolitan. Hydrogenation can be carried out in a fixed catalyst bed, in a progressively moving catalyst bed qpa, or in a rarefied and fluidized bed. Hydrogenation is preferably carried out in boiling (pseudo-oleaginous) upstream. The hydrogenation product of coal, containing a liquid coal extract of a dissolved carbon-containing substance in a coal solvent and an insoluble substance (ash and undissolved coal), is sent to the separation zone 5, in which the fraction boiling to 315.6 ° C is distilled off. The latter is discharged through line 6. The separation zone 5 may include atmospheric or vacuum columns. The coal liquefaction product, free from components boiling up to 315 ,, is withdrawn from separation zone 5 via line 7 and mixed with a second solvent supplied via line 8. As a second solvent, a 5% volume fraction is used. . % of which is at temperature on the order of 212.8 ° C | a 05% by volume at 260.0 ° C, which is a derivative of a naphthenic or parafisshove distillate. The displaced product flow, the liquefaction of coal and second solvent along line 9 are introduced into the gravitational sedimentation zone, which includes the gravity sludge 10 and 11. The solid-free flows from the gravity sedimentation tanks 1O and 11 are diverted through lines 12 and 13 respectively , 14 are directed to the line 15 to distill off the second solvent and the various 4 coal extracts. Such a zone may consist of one or more distillation columns to produce different fractions. In the distillation zone 15, a fraction of the first and second solvents is obtained. A portion of the first solvent fraction through line 16 is sent to zone 2. Another part of this fraction is withdrawn from the installation via line 17. The second solvent fraction is withdrawn through line 18 and then served along line 8 to mix coal with the solution of hydrogenation products in the first solvent. The fraction boiling above 482.2 C, with a low ash content and low sulfur content, is discharged in 1P shps. A stream containing insoluble matter dispersed in it in 6–18% of ash is withdrawn from the gravitational sedimentation zone along the pine line 2O and sent to the distillation zone of the light fractions 21, in which the distillate is removed (|), temperature below 482.2С The last oi are watered through line 22 and sent to the distillation zone 15. These residues of live coal kenmen, devoid of light fractions, are withdrawn through line 23. The latter have a minimal amount of soluble benzenes, i.e. about 35 wt.% to maintain the flow, the honor of the stream. Do not be dehydrated or coked. Part of bottoms can be used as fuel for production. Catalyst. Contacting method. Coal paste feed rate at 65.6 s. Total gas feed rate at - .4, normal CONDITIONS, cm / h. Constant volume velocity of liquid at 65, hT. Working pressure (total), jcr / cm. Hydrogen partial pressure at the reactor exit, kg / cm V Operating temperature, "1 The liquid product containing ash is cooled to 14.8.9 s and sent to one of two interchangeable gas-liquid separators high pressure and coupled steam allelic trubakda. When the first separator is filled chimerically with 80% liquid product, I connect the second separator, and the contents of the first are transferred to the receiver of a low-pressure, burned-out product. The yKufsfioe low pressure receiver contents are pumped to a mixed tank equipped with double walls for steam supply. Then the goals of the game. In addition, they can be used as feedstock in the process of partial oxidation during the production of hydrogen. A second solvent can be additionally introduced into the system via line 24. Example. Coal paste containing 40 wt. % coal Illinois field and 60 wt. % of the njM 315.6-482.2 C of the pasty oil obtained by the distillation of the coal tar is mixed with hydrogen and continuously fed through a preheater to a reactor operating in the upstream fluidized bed operating in the following mode. The temperature of the mixture of hydrogen and coal paste in the heater increases to about 357 ,. Cobalt molybdate on alumina particles (particle size 8-12 mesh) Upward fluidized bed 84.4 415.6-443.3 The product is pumped through an electrically heated coil into the column to distill light fractions under the conditions of. standing equilibrium. The light distillation unit operates at a temperature of about 315, and atmospheric pressure. The feed rate of the product is about 18.9 l / h and the nitrogen input for washing is 75. The overhead vapor from the distillation column of the light fractions is condensed and collected in a 2O8.2 l vessel. The residual product is collected in the receiver, from which it is then pumped into a steam-heated mixer with a capacity of 1893 liters. Residual product containing about 4.4 wt. % ash, has an initial. boiling point higher than 482.2 С adjusted for atmospheric pressure 76О mm Hg. Art. 12OO g of residual product in a thick-walled steel vibrating flask with a capacity of 2 liters, with electric heating. The contents of the boiling flask are heated to 204 with shaking. 60 g of a kerosene distillate boiling at 218.3 254, 4 ° C, having a characteristic factor of 11.9, is added to the vibrating flask and the temperature of the mixture is increased to 254.4 265 bs with shaking. Copba is placed in a vertical position and the contents are left to stand for 4 hours at 204 ,. 35Og of the ash-rich bottom layer is diverted through the bottom valve in the presence of small amounts of water and then the same amount of 1 product is diverted from the upper ash-depleted layer to a separate receiver. The ash content in the upper and lower layers is determined. A sample of the lower layer is removed from the light fractions in a vacuum under laboratory conditions until noK reaches the upper boiling point of fraccia 471.1-482.2 ° C corrected for atmospheric pressure. The vacuum in the column was filled with nitrogen, and the remaining precipitate was removed. This vacuum residue, devoid of light fractions, is subjected to a fluidity test at a temperature of about 287, in the atmosphere of an azeta on a Brookfield viscometer. Samples of the stripped light fractions of the lower layer are also analyzed for the content of insoluble benzenes and ash. The obtained ex-chemical and analytical data are summarized in Table. 1 .. PRI mme R 2. Similar to the example, except that the sample from the lower layer is 49 O. Example 3, similar to example 1, except that the sample from the lower layer is 650 g .; Note 4. Similar to the example, except that the sample from the lower layer is 73 O. The data of the analysis of the product of the lower layer, of the light fractions, are presented in Table. 2. As B1SHNO from the data of examples 1-4, with an increase in the ash content in the lower layer (fraction) before the light fractions are distilled off, the weight ratio ipt to ash in the lower layer, devoid of light fractions, decreases. PRI me R 5. 350 g of high-grade bottom ash sample ash is loaded into an electrically heated 500-cm stainless steel container equipped with an internal thermocouple, a drain valve, and two-way branch connections. The contents of the tank are heated to 254.4-265.6 ° C and allowed to stand for 3 hours with the same tetlterateu. Then, the upper part of the lateral connection of 100 g of ash depleted upper secondary storage is diverted to the collector. An equal amount of secondary bottom layer enriched in ZOPA is discharged through a milking valve. The ash content of the secondary upper and lower layers obtained in this process is 0.01 and 1O, respectively, 0 wt. .%. The remainder of the secondary lower layer is subjected to distillation in vacuum to the temperature, lc (limit of the boiling point), corrected for an absolute pressure of 760 mm Hg. Art. Cube residue is examined for fluidity at 287.8 C in nitrogen atmosphere on a Brookfield viscometer. The content of ash and insoluble benzenes in the residual distillation product is also determined. The residual pendentary suction or the intracellular lower layer devoid of the lungs (|) of the skin contains an DA, 6 wt. % ash and 55.4 wt.% HepacTBOjMMbix of benzenes and remains fluid at 287.8 ° C. The amount of soluble benzenes (EP) is 44, its weight. % and the ratio of their components to ash in the secondary, devoid of pegkvk. fractionally, the bottom layer is 2.27 weight. % Thus, prv increase social network. ash in the lower layer, directed to the lifting of light fractions, from 7% (in example 4) to 10% (in example 5), the weight from the bottom in the lower layer, deprived of light fractions, decreases correspondingly from 2.55 to 2.27 .
    Table 1
    Sample weight of the lower layer, g
    The amount of the sample taken from the total, weight,%
    Ash content in the lower layer, weight. %
    Ash content in the upper layer, weight. %
    Ash content (A), weight. %
    Insoluble benzenes (BN), wt. %
    Viscosity determination on a Brookfipd's 287.8 C viscometer
    Soluble benzenes (BR) (BR 1OO-BN), wt. %
    权利要求:
    Claims (2)
    [1]
    1. Gizzhrovshgy coal and tar. Bulletin of the Bureau of Mines USA 1 633, 1968, p. 91-103.
    [2]
    2.Patagg of the USSR by application
    N 1975277 / 23-26, class C 10 G 1/06, 1973 (pragotte).
    类似技术:
    公开号 | 公开日 | 专利标题
    SU953987A3|1982-08-23|Method for deashing products of coal hydrogenation
    US3856675A|1974-12-24|Coal liquefaction
    CA1037400A|1978-08-29|Synthetic crude from coal
    US4455216A|1984-06-19|Polarity gradient extraction method
    SU718016A3|1980-02-25|Method of deashing the products of coal hydrogenation
    US4279739A|1981-07-21|Process for separating bituminous materials
    US3947346A|1976-03-30|Coal liquefaction
    US3974073A|1976-08-10|Coal liquefaction
    US2564409A|1951-08-14|Extraction of oleiferous materials
    US2895902A|1959-07-21|Removal of metal contaminants from residual oils
    US4169044A|1979-09-25|Re-refining used lube oil
    US5139621A|1992-08-18|Azeotropic distillation process for recovery of diamondoid compounds from hydrocarbon streams
    US3079326A|1963-02-26|Double solvent refining of tar
    US3962098A|1976-06-08|Gravity settling
    US4381234A|1983-04-26|Solvent extraction production of lube oil fractions
    US3711400A|1973-01-16|Continuous process for recovering waxes from oily sludges
    US4208263A|1980-06-17|Solvent extraction production of lube oil fractions
    US4040957A|1977-08-09|Separation of insoluble material from coal liquefaction product by use of a diluent
    SU904530A3|1982-02-07|Method of separating tar and solid particles from coal liquflyed products
    US4273645A|1981-06-16|Solvent extraction production of lube oil fractions
    US2060447A|1936-11-10|Working-up of carbonaceous materials
    US3567627A|1971-03-02|Lube extraction with an ethyl glycolate solvent
    US4326948A|1982-04-27|Coal liquefaction
    EP0020094B1|1982-09-29|An improved solvent extraction process for providing lubricating oil fractions
    US3017346A|1962-01-16|Solvent extraction process using dimethyl hydrogen phosphite
    同族专利:
    公开号 | 公开日
    DD116257A5|1975-11-12|
    AU7908375A|1976-09-16|
    LU72033A1|1975-08-20|
    GB1500337A|1978-02-08|
    NL174565C|1984-07-02|
    ZA751336B|1976-02-25|
    FR2264855B1|1978-09-29|
    CA1060828A|1979-08-21|
    JPS50127903A|1975-10-08|
    IT1030365B|1979-03-30|
    NL7503221A|1975-09-22|
    US3954595A|1976-05-04|
    FR2264855A1|1975-10-17|
    DE2510539A1|1975-09-25|
    BE826587A|1975-06-30|
    JPS5711587B2|1982-03-05|
    PL98031B3|1978-04-29|
    JPS5598285A|1980-07-26|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3018241A|1960-10-10|1962-01-23|Consolidation Coal Co|Production of hydrogen-rich liquid fuels from coal|
    US3162594A|1962-04-09|1964-12-22|Consolidation Coal Co|Process for producing liquid fuels from coal|
    US3375188A|1966-12-19|1968-03-26|Lummus Co|Process for deashing coal in the absence of added hydrogen|
    US3790467A|1970-08-27|1974-02-05|Exxon Research Engineering Co|Coal liquefaction solids removal|
    US3687837A|1970-08-27|1972-08-29|Exxon Research Engineering Co|Coal liquefaction solids removal|
    US3808119A|1972-10-12|1974-04-30|Pittsburgh Midway Coal Mining|Process for refining carbonaceous fuels|
    US3852182A|1972-11-07|1974-12-03|Lummus Co|Coal liquefaction|
    US3856675A|1972-11-07|1974-12-24|Lummus Co|Coal liquefaction|
    US3852183A|1972-12-29|1974-12-03|Lummus Co|Coal liquefaction|
    US3791956A|1973-02-16|1974-02-12|Consolidation Coal Co|Conversion of coal to clean fuel|JPS5444002B2|1975-05-21|1979-12-24|
    US4040957A|1976-02-20|1977-08-09|The Lummus Company|Separation of insoluble material from coal liquefaction product by use of a diluent|
    US4090958A|1976-02-23|1978-05-23|Kerr-Mcgee Corporation|Coal processing system for producing a stream of flowable insoluble coal products|
    US4070268A|1976-06-01|1978-01-24|Kerr-Mcgee Corporation|Solvent recovery in a coal deashing process|
    US4119524A|1976-06-01|1978-10-10|Kerr-Mcgee Corporation|Coal deashing process having improved solvent recovery techniques|
    US4090957A|1976-06-01|1978-05-23|Kerr-Mcgee Corporation|System for separating soluble and insoluble coal products from a feed mixture|
    US4077881A|1976-07-08|1978-03-07|The Lummus Company|Separation of insoluble material from coal liquefaction product by gravity settling|
    US4134821A|1977-06-01|1979-01-16|Continental Oil Company|Maintenance of solvent balance in coal liquefaction process|
    US4177135A|1978-03-20|1979-12-04|Kerr-Mcgee Corporation|Use of specific coal components to improve soluble coal product yield in a coal deashing process|
    US4162964A|1978-03-20|1979-07-31|Kerr-Mcgee Corporation|Method of handling ash-rich material in a coal deashing process|
    US4470900A|1978-10-31|1984-09-11|Hri, Inc.|Solids precipitation and polymerization of asphaltenes in coal-derived liquids|
    GB2053955B|1979-07-17|1983-01-26|Coal Industry Patents Ltd|Coal extraction|
    US4404084A|1982-03-11|1983-09-13|Hri, Inc.|Coal hydrogenation and deashing in ebullated bed catalytic reactor|
    CN102206501B|2010-03-30|2013-10-30|神华集团有限责任公司|Gravity discharge method for high-temperature oil residue|
    FR3024378B1|2014-07-31|2020-09-11|Ifp Energies Now|ALUMINA-BASED ADSORBANT CONTAINING SODIUM AND DOPED BY AN ALKALINE ELEMENT FOR THE CAPTATION OF ACID MOLECULES|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/452,409|US3954595A|1974-03-18|1974-03-18|Coal liquefaction|
    [返回顶部]