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US3856675A - Coal liquefaction - Google Patents

Coal liquefaction Download PDF

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Publication number
US3856675A
US3856675A US00304319A US30431972A US3856675A US 3856675 A US3856675 A US 3856675A US 00304319 A US00304319 A US 00304319A US 30431972 A US30431972 A US 30431972A US 3856675 A US3856675 A US 3856675A
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Prior art keywords
liquid
coal
promoter
distillation temperature
insoluble material
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US00304319A
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English (en)
Inventor
M Sze
G Snell
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lummus Technology LLC
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Lummus Co
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Filing date
Publication date
Application filed by Lummus Co filed Critical Lummus Co
Priority to US00304319A priority Critical patent/US3856675A/en
Priority to ZA738417*A priority patent/ZA738417B/xx
Priority to LU68727A priority patent/LU68727A1/xx
Priority to BE137296A priority patent/BE806789A/xx
Priority to FR7339068A priority patent/FR2205564B1/fr
Priority to AU62148/73A priority patent/AU469767B2/en
Priority to CA185,185A priority patent/CA1004618A/en
Priority to GB5155273A priority patent/GB1452297A/en
Priority to IT70257/73A priority patent/IT996915B/it
Priority to JP48124890A priority patent/JPS521922B2/ja
Priority to CS7300007641A priority patent/CS186778B2/cs
Priority to DE2355606A priority patent/DE2355606C2/de
Priority to NLAANVRAGE7315260,A priority patent/NL174064C/nl
Application granted granted Critical
Publication of US3856675A publication Critical patent/US3856675A/en
Priority to GB35427/75A priority patent/GB1516145A/en
Priority to DE19752539054 priority patent/DE2539054A1/de
Priority to NLAANVRAGE7510521,A priority patent/NL176791C/nl
Priority to FR7527287A priority patent/FR2283944A2/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
    • C10G1/045—Separation of insoluble materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
    • C10G1/083—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts in the presence of a solvent

Definitions

  • Coal can be converted to valuable products by sub jecting coal to solvent extraction, with or without hydrogen, to produce a mixture of coal extract and undissolved coal residue, including undissolved extractable carbonaceous matter, fusain and mineral matter or ash.
  • Gravity settling techniques have also met with limited success as a result of low settling rates and inefficient ash removal. Centrifugation techniques have also been generally unsuccessful as a result of high cost and the difficulty in separating the lighter finely divided materials.
  • An object of the present invention is to provide for improved coal liquefaction.
  • Another object of the present invention is to provide a new and improved process for separating finely divided insoluble material from a coal liquefaction product.
  • a further object of the present invention is to provide a process for separating insoluble material from a coal liquefaction product which does not require a filtration step.
  • Still another object of the present invention is to provide an improved gravity settler for coal deashing.
  • FIG. 1 is a simplified schematic flow diagram of a coal liquefaction process incorporating the teachings of the present invention.
  • FIG. 2 illustrates a preferred embodiment of a gravity settler for coal deashing.
  • the objects of the present invention are broadly accomplished, in one aspect, by use of a liquid which promotes and enhances the separation of insoluble material from a coal liquefaction product.
  • the coal liquefaction product comprised of a liquid coal extract of dissolved carbonaceous matter in a coal liquefaction solvent and insoluble material (ash and unreacted coal) is mixed with a liquid promoter having an aromaticity less than that of the liquefaction solvent to enhance and promote the separation of insoluble material and provide a liquid coal extract essentially free of insoluble material.
  • the liquid which is employed to enhance and promote the separation of insoluble material from the coal liquefaction product is generally a hydrocarbon liquid wherein T is the molal average boiling point of the liquid R); and G is specific gravity of the liquid (60 F/60 F).
  • the characterization factor is an index of the aromaticity/parafinicity of hydrocarbons and petroleum fractions as disclosed by Watson & Nelson Ind. Eng. Chem. 25 880 (I933), with more parafinic materials having higher values for the characterization factor (K).
  • the promoter liquid which is employed is one which has a characterization factor (K) in excess of 9.75 andwhich is also less aromatic than the liquefac tion solvent; i.e., the characterization factor K of the promoter liquid has a value which is generally at least 0.25, higher than the characterization factor of the liquefaction solvent.
  • the liquid which is used to enhance and promote the separation of insoluble material is further characterized by a 5 volume percent distillation temperature of at least about 250 F. and a volume percent distillation temperature of at least about 350 F. and no greater than about 750 F.
  • the promoter liquid preferably has a 5 volume percent distillation temperature of at least about 310 F. and most preferably of at least about 400 F.
  • the 95 volume percent distillation temperature is preferably no greater than about 600 F.
  • the most preferredpromoter liquid has a 5 volume percent distillation temperature of at least about 425 F. and a 95 volume percent distillation temperature of no greater than about 500 F.
  • the pro moter liquid may be a hydrocarbon; e.g., tetrahydronaphthalene, in which case the 5 volume percent and 95 volume percent distillation temperatures are the same; i.e., the hydrocarbon has a single boiling point.
  • the boiling point of the hydrocarbon must be at least about 350 F. in order to meet the requirement of a 5 volume percent distillation temperature of at least about 250 F. and a 95 volume percent distillation temperature of at least about 350 F.
  • the promoter liquid is preferably a blend or mixture of hydrocarbons in which case the 5 volume percent and 95 volume percent distillation temperatures are not the same.
  • the 5 volume and 95 volume percent distillation temperature may be conveniently determined by ASTM No. D 86-67 or No. D 1160 with the former being preferred for those liquids having a 95 percent volume distillation temperature below 600 F. and the latter for those above 600 F.
  • the methods for determining such temperatures are well known in the art and further details in this respect are not required for a fully understanding of the invention. It is also to be understood that the reported temperatures are corrected to atmospheric pressure.
  • kerosene or kerosene fraction from paraffinic or mixed base crude oils; middle distillates, light gas oils and gas oil fractions from paraffinic or mixed based crude oils; alkyl benzenes with side chains containing or more carbon atoms; paraffmic hydrocarbons containing more than 12 carbon atoms; white oils or white oil fraction derived from crude oils; alphaolefms containing more than 12 carbon atoms; fully hydrogenated naphthalenes and substituted naphthalenes; propylene oligomers (pentamer and higher); tetrahydronaphthalene, heavy naphtha fractions, etc.
  • the most preferred liquids are kerosene fractions; white oils; fully hydrogenated naphthalenes and substituted naphthalenes; and tetrahydronaphthalene.
  • the amount of liquid promoter used for enhancing and promoting the separation of insoluble matter from the coal liquefaction product will vary with the particular liquid employed, the coal liquefaction solvent, the coal used as starting material and the manner in which the liquefaction is effected. As should be apparent to those skilled in the art, the amount of liquid promoter used should be minimized in order to reduce the overall costs of the process. It has been found that by using the liquid of controlled aromaticity, in accordance with the teachings of the present invention, the desired separation of insoluble material may be effected with modest amounts of liquid promoter.
  • the weight ratio of liquid promoter to coal solution may range from about 0.221 to about 3.0: 1, preferably from about 0.3:1 to about 2.0:] and, most preferably from about 0.311 to about 1.521.
  • promoter liquid of the present invention which is a kerosene fraction having 5 percent and 95 percent volume distillation temperatures of 425 F. and 500 F. respectively
  • promoter liquid to coal solution weight ratios in the order of 0.4:1 to 0.611 have been particularly successful. It is to be understood, however, that greater amounts of liquid promoter may be employed, but the use of such greater amounts is uneconomical. In addition, the use of an excess of liquid promoter may result in the precipitation or separation of an excessive amount of desired coal derived products from the coal extract.
  • liquid promoters of the present invention not only may modest amounts of solvent be employed, but, in addition, ash may be effectively separated from the coal solution; e.g., in amounts greater than 99 percent, without an excessive loss of desired coal derived products.
  • coal such as bituminous coal
  • a moisture ash free basis may contain from about 5 percent to about 10 percent of insoluble material, such as fusain, and accordingly, at a minimum, from about 5 percent to about 10 percent, of the MAF coal, is lost in the process.
  • the potential product loss is measured by the amount of 850 F+ product which is not recovered from the coal in that it is this fraction, which includes insoluble coal material, such as fusain, which can not be recovered from the residual solid product of the coal deashing.
  • product loss of 850 F+ components on an ash free basis
  • product loss of 850 F+ components can be maintained at a value of no greater than about 40 percent, by weight, and preferably no greater than about 25 percent, by weight.
  • the loss of 850 F+ products, on a MAF coal basis is from about 10 percent to about 25 percent, by weight.
  • the net coal product (the extracted carbonaceous matter, excluding promoter liquid, liquefaction solvent and gas make), hereinafter sometimes referred to as coal product, contains less than about 1 percent insoluble material, generally less than 0.1 percent insoluble material and most preferably less than 0.05 percent insoluble material, all by weight.
  • the specific amount of insoluble material which is permitted to be present in the coal product is dependent upon the product standards, and the deashing is controlled in order to provide the required specifications. Based on an Illinois type, the production of a coal product having less than .05 percent, by weight, insoluble material, corresponds to 99+ percent ash removal but as should be apparent to those skilled in the art, the percent ash removal to provide a coal product having the required minimum amount of insoluble material is dependent upon the initial ash content of the coal.
  • the liquid promoter is added to the coal solution in an amount, as hereinabove described, to provide a coal product in which insoluble material is present in an amount of less than about 1 percent, by weight, and most preferably of less than 0.05 percent, by weight, with the loss of 850 F+ product being from about 10 percent to about 40 percent, by weight, preferably from about 10 percent to about 25 percent, by weight, on a MAF coal feed basis; i.e., from about 60 percent to about percent, by weight, of the MAP coal feed is recovered as either gas make or liquid fuel product.
  • the liquid promoter may also be prepared by blending a material having a characterization factor below 9.75 with a material having a characterization factor about 9.75, provided the blend has a characterization factor about 9.75 and the boiling properties, as hereinabove described.
  • the use of blended materials is a convenient manner of regulating the characterization factor.
  • the separation of the insoluble material from the coal extract is generally effected at a temperature from about 300 F. to about 600 F., preferably from about 350 F. to about 500 F., and at a pressure from about 0 psig to about 500 psig, preferably at a pressure from about 0 psig to about 300 psig. It is to be understood that higher pressures could be employed, but as should be apparent to those skilled in the art, lower pressures are preferred.
  • the insoluble material is preferably separated by gravity settling with the essentially insolublefree coal extract being recovered as an overflow and the insoluble material as underflow. In such gravity settling, the amount of underflow should be minimized in order to minimize the loss of heavier products in the underflow.
  • the underflow withdrawal rate to obtain desired results is deemed to be within the scope of those skilled in the art. In general, such a rate is from about 20 to about 25 wt. percent of the total feed (liquefaction product and promoter liquid.)
  • the residence time for such settling is generally in the order of from about 0.5 to about 6 hours, and preferably from about 0.5 to 3.0 hours.
  • the coal liquefaction product prior to mixing thereof with the promoter liquid, is treated to separate at least those components boiling up to about the 95 volume percent distillation temperature of the promoter liquid.
  • the coal liquefaction product is free of components which boil within the range of those present in the promoter liquid, thereby facilitating the subsequent recovery of the promoter liquid from the coal liquefaction product.
  • ground or pulverized coal generally bituminous, sub-bituminous or lignite, preferably bituminous coal
  • in line 10 is introduced into a coal solvation and slurrying zone 11 along with a coal liquefaction solvent in line 12.
  • the coal liquefaction solvent may be any one of the wide variety of coal liquefaction solvents used in the art, including both hydrogen donor solvents, non-hydrogen donor solvents and mixtures thereof. These solvents are well known in the art and, accordingly, no detailed description thereof is deemed necessary for a full understanding of the invention.
  • the coal liquefaction solvent is a 600-900 F.
  • solvent which is recovered from the coal liquefaction product and which has not been subjected to hydrogenation subsequent to the recovery thereof.
  • the solvent is added to the coal in an amount sufficient to effect the desired liquefaction, and in general, is added in an amount to provide a solvent to coal weight ratio from about 1:1 to about :1, and preferably from about 1.5:1 to about 5:1.
  • a coal paste is withdrawn from zone 11 through line 13 and introduced into a coal liquefaction zone 14 wherein, as known in the art, the coal is converted to liquid products.
  • the liquefaction zone 14 is operated as known in the art and may be catalytic or non-catalytic and may be effected in the presence or absence of added hydrogen.
  • the hydrogenation may be effected in a fixed catalyst bed, fluidized catalyst bed or in an expanded or ebullating bed.
  • the details of the coal liquefaction step form no part of the present invention and, accordingly, no details thereof are required for a full understanding of the invention.
  • the coal liquefaction is effected in the presence of added hydrogen.
  • the hydrogenation increases the recovery of coal products and also reduces the sulfur and nitrogen content of the recovered liquid coal product.
  • the liquefaction is preferably effected in an upflow ebullated bed, as known in the art; e.g., as described in US. Pat. No. 2,987,465 to Johanson.
  • the coal liquefaction zone includes means for recovering the various gaseous products.
  • a coal liquefaction product comprised of a liquid coal extract of dissolved carbonaceous matter in the coal liquefaction solvent and insoluble material (ash and undissolved coal) is withdrawn from the liquefaction zone 14 through line 15 and introduced into a separation zone 16 to separate from the coal liquefaction product at least those materials boiling up to about the volume percent distillation temperature of the liquid to be used for promoting and enhancing the separation of the insoluble material.
  • the separation zone 16 may include an atmospheric or vacuum flashing chamber or tower, and as particularly described separation zone 16 is designed and operated to separate components boiling up to about 550 F.
  • the promoter liquid is a kero sene fraction which has 5 volume percent and 95 volume percent distillation temperatures which fall within the range from about 425500 1F and is derived from a naphthenic or paraffinic distillate.
  • the combined stream of coal liquefaction product and promoter liquid in line 22 is introduced into a gravity separation zone 23, comprised of a gravity settler which may be any one of those known in the art, wherein an essentially solids free overflow is separated from a solid containing underflow.
  • a gravity settler may be any one of those generally known in the art, the settler is preferably of a special type developed for the present invention as hereinafter described with reference to FIG. 2.
  • the overflow essentially free of insoluble mateial is withdrawn from separation zone 23 through line 24 and introduced into a recovery zone 25 for recovering promoter liquid and various fractions of the coal extract.
  • the recovery zone 25 may be comprised of one or more fractionators to distill various fractions from the product. As particularly described, the recovery zone is operated to recover a first fraction having 5 percent and 95 percent volume distillation temperatures of from 425 to 500 F.
  • the promoter liquid recovered in the: recovery zone is admixed with the liquefaction product in line 17 and makeup may be provided through line 26.
  • the underflow containing dispersed insoluble material withdrawn from separation zone 23 through line 31 is introduced into a stripping zone 32 wherein material boiling, below about 900 F is stripped therefrom and introduced into the recovery zone 25 through line 33.
  • the ash rich stripper bottoms in line 34 may then be subjected to calcination or coking. Alternatively, part of the stripper bottoms may be used as feedstock to a partial oxidation process for producing hydrogen. As a further alternative a portion of the stripper bottoms may be used for plant fuel.
  • the stripper bottoms in line 34 contains from about percent to about percent, by weight, of the MAF coal.
  • the coal product (the product recovered from zones 16 and 25, excluding liquefaction solvent and promoter liquid contains less than 1 percent and preferably less than 0.05 percent, by weight, of insoluble material.
  • the gravity settler of the present invention which is preferably used in the embodiment of FIG. 1 is described with reference to FIG. 2.
  • the preferred settler 100 of the present invention comprised of a cylindrical main body portion 101 and dished upper and lower heads 102 and 103, respectively.
  • the main body portion 101 is provided with a feed inlet 104 which is positioned perpendicularly to the main axis of the vessel 100 at a central point thereof.
  • the upper head 102 is provided with an inclined overflow outlet 105 and the lower head 103 is provided with an inclined underflow outlet 106, both of which are inclined at an angle of approximately
  • the settler 100 is slanted at an angle with respect to horizonatal with the preferred angle being from about 45 to about
  • the mixture of coal liquefaction prodnet and promoter liquid is introduced into the settler through inlet 104, with the essentially solid free overflow being withdrawn through overflow outlet 105 and the solid containing underflow being withdrawn without accumulation of ash and bitumens.
  • the settler of the present invention is particularly suited for use with the deashing technique of the present invention, such a settler may also be used 5 for gravity settling deashing by techniques other than those of the present invention.
  • This ash-rich liquid receiver product will hereinafter be referred to as either a coal solution, ash-rich coal solution, or hydrogenated coal solution.
  • Table 1 is a summary of analytical inspection 30 data obtained for the ash-rich coal solutions used in the solvent deashing examples, which will be cited subsequently.
  • Table 2 is a compilation of Characterization Factors on liquids used in the subsequent deashing examples. This index is a measure of aromaticity and/or parafinicity.
  • the use of a tank in a vertical position prevents the accumulation of such materials, but it provides less settling cross sectional area than that provided in a horizontal tank.
  • the use of the inclined settler of the present invention provides efficient use of a given diameter vessel for settling 300 grams of ash-rich coal solution number 1 and 1,200 grams of liquid A were charged to a 2 liter cylindrical stainless steel electrically heated rocking bomb. Bomb in measurements was 4.26 inches l.D. X 18 inches long on the straight side, and it was equipped with a A inch bottom drawoff valve. The contents of the bomb were rocked and heated to 500 F. over about a 30 minute period. Bomb contents were then allowed to settle vertically for about 4 hours at 500 F. without any rocking.
  • EXAMPLE 2 300 grams of ash-rich coal solution number 11, and a blend of 300 grams of liquid D and 900 grams of liquid B, were added to the 2 liter rocking bomb described in example 1. The contents of the bomb were heated with rocking to 500 F. over about a 30 minute period. Bomb contents were then allowed to settle vertically for about 4 hours at 500 F. without any rocking.
  • This example illustrates the effectiveness of a liquid blend at a promoter to coal solution ratio of about 1:1.
  • EXAMPLE 3 A 1,500 ml. dimpled glass resin flask was used in the experiment. The resin flask was outfitted with a four bladed turbine agitator, thermometer, a heating mantle, reflux condenser, and a dropping funnel.
  • This example illustrates the effectiveness of a liquid promoter of the present invention, in the absence of diluent, at a promoter liquid to coal solution ratio of 1.3:1.
  • This example illustrates the effectiveness of a liquid promoter of the present invention, in the absence of diluent, at a promoter liquid to coal solution ratio of about 0.54:1.
  • This example illustrates the effectiveness of a liquid blend at a liquid to coal solution ratio of about 1.4:1.
  • EXAMPLE 6 The settler apparatus described with reference to FIG. 2 is used to deash ash-rich coal solution No. 21.
  • EXAMPLE 7 The apparatus described with reference to FIG. 2 is used to deash coal solution No. 92 using promoter liquid D. The conditions and results are reported in the following Table.
  • EXAMPLE 9 In accordance with the present invention, in a typical run, based on 40 lbs. of coal feed in line 10 and 1.4 lbs. of hydrogen feed to the liquefaction zone, the net liquified coal product recovered in zone 16 and recovery zone is about 20 lbs; the gas make in the liquefaction zone is about 11 lbs; and the coal residual product in line 34 is about 10 lbs., with about 4 lbs thereof being ash. This represents about 99+ percent, by weight, ash removal, with MAF coal product loss based on MAF coal feed, being about 18 percent, by weight.
  • the present invention is particularly advantageous in that insoluble materials can be separated from a coal liquefaction product without requiring filtration.
  • ash and insoluble material separation can be maximized with minimum loss of desired coal derived products and with modest amounts of promoter liquid.
  • the present invention is also distinguishable from an extraction process in that the promoter liquid is not employed to extract a fraction of the liquid coal extract, but instead is employed to promote settling of insoluble material.
  • a process for separating insoluble material from a coal liquefaction product produced from a coal feed and comprised of insoluble material and carbonaceous matter dissolved in a coal liquefaction solvent comprising:
  • liquid promoter introducing said liquefaction product and a liquid promoter into a gravity settling zone to separate insoluble material by gravity settling, said liquid promoter having a 5 volume percent distillation tem' perature of at least about 250 F. and a 95 volume percent distillation temperature of at least about 350 F. and no greater than about 750 F., said liquid having a characterization factor (K) of at least 9.75;
  • said liquid having a characterization factor greater than said coal liquefaction solvent
  • promoter liquid being added in an amount sufficient to promote and enhance gravity settling of insoluble material to produce an overflow essentially free of insoluble material
  • liquid promoter is at least one member selected from the group consisting of kerosene, kerosene fractions, middle distillates, light gas oils, gas oil fractions, heavy naphthas, white oils and white oil fractions from crude oils.
  • the promoter liquid is a fraction having a volume percent distillation temperature of at least about 425 F. and a 95 volume percent distillation temperature of no greater than about 500 F.
  • liquid promoter is a kerosene fraction having a characterization factor of about 1 1.9 and a 5 volume percent distillation temperature of no less than 425 F. and a 95 volume distillation temperature of no greater than about 500 F.
  • a process for separating insoluble material from a coal liquefaction product produced from a coal feed and comprised of insoluble material and carbonaceous matter dissolved in a coal liquefaction, solvent comprising:
  • liquid promoter of a hydrocarbon mixture
  • said liquid promoter having a 5 volume percent distillation temperature of at least about 250 F and a 95 volume percent distillation temperature of at least about 350 F and no greater than about 750 F
  • said liquid promoter being at least one member selected from the group consisting of kerosene, kerosene fractions, middle distillates, light gas oils, gas oil fractions, heavy naphthas, white oils and white oil fractions from crude oils,
  • the liquid promoter to coal liquefaction product weight ratio being from about 0.2:1 to about 3.0:1, said ratio being an amount which produces an essentially insoluble material free overflow from said gravity settling zone and a net coal product from said coal feed containing less than about 0.05 percent, by weight, insoluble material and an underflow which contains the insoluble material, said underflow containing no greater than about 40 percent, by weight, of the moisture ash free coal as an ash free 850 F+ fraction.
  • said promoter liquid is a kerosene fraction having a characterization factor of about 11.9, a 5 volume percent distillation temperature of at least about 4250 F., and a 95 volume percent distillation temperature of no greater than about 500 F.
  • underflow is withdrawn from said settling zone at a rate of from about 20 to about 25 wt. percent of the total of liquefaction product and promoter liquid introduced into the settling zone.
  • liquid promoter has a characterization factor of at least about 11.0.
  • a process for separating insoluble material from a coal liquefaction product produced from a coal feed and comprised of insoluble material and carbonaceous matter dissolved in a coal liquefaction solvent comprising:
  • step (b) separating from the coal liquefaction product at least those components boiling up to about the 95 volume percent distillation temperature of the liquid promoter hereinafter defined in step (b);
  • step (b) introducing the coal liquefaction product from step (a) and a liquid promoter into a gravity settling zone, said liquid promoter having a 5 volume percent distillation temperature of at least about 250 F. and a 95 volume percent distillation temperature of at least about 350 F.
  • said liquid having a characterization factor (K) of at least about 9.75, said liquid having a characterization factor K greater than said coal liquefaction solvent and being present in an amount sufficient to promote and enhance gravity settling of insoluble material to produce a net coal product from said coal feed containing less than about 0.1 percent, by weight, insoluble material and a coal residue con taining no greater than about 40 percent, by weight, of the MAP coal feed as an ash free +850 F. fraction;
  • step (b) e. passing separated promoter liquid from step (d) to step (b).
  • liquid promoter has a characterization factor of at least about 1 1.0.

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  • Chemical & Material Sciences (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
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US00304319A 1972-11-07 1972-11-07 Coal liquefaction Expired - Lifetime US3856675A (en)

Priority Applications (17)

Application Number Priority Date Filing Date Title
US00304319A US3856675A (en) 1972-11-07 1972-11-07 Coal liquefaction
ZA738417*A ZA738417B (en) 1972-11-07 1973-10-30 Process for solvent deashing of hydrofined coal solution
LU68727A LU68727A1 (nl) 1972-11-07 1973-10-31
BE137296A BE806789A (fr) 1972-11-07 1973-10-31 Procede pour eliminer les cendres de produits de liquefaction du charbon
AU62148/73A AU469767B2 (en) 1972-11-07 1973-11-02 Process for solvent leashing of hydrofined coal solution
FR7339068A FR2205564B1 (nl) 1972-11-07 1973-11-02
JP48124890A JPS521922B2 (nl) 1972-11-07 1973-11-06
IT70257/73A IT996915B (it) 1972-11-07 1973-11-06 Procedimento per la rimozione delle ceneri dal solvente di solu zioni di carbone idrosuddiviso
CA185,185A CA1004618A (en) 1972-11-07 1973-11-06 Process for solvent deashing of hydrofined coal solution
GB5155273A GB1452297A (en) 1972-11-07 1973-11-06 Process for solvent de-ashing of hydrofined coal solution
DE2355606A DE2355606C2 (de) 1972-11-07 1973-11-07 Abtrennung von unlöslichem Material aus einem Kohleverflüssigungsprodukt
NLAANVRAGE7315260,A NL174064C (nl) 1972-11-07 1973-11-07 Werkwijze voor het afscheiden van onoplosbaar materiaal uit een bij het vloeibaar maken van kool verkregen produkt.
CS7300007641A CS186778B2 (en) 1972-11-07 1973-11-07 Method for the separation of insoluble parts from coal solutions in liquefying agent
GB35427/75A GB1516145A (en) 1972-11-07 1975-08-27 Liquefaction of coal
DE19752539054 DE2539054A1 (de) 1972-11-07 1975-09-03 Kohleverfluessigung
NLAANVRAGE7510521,A NL176791C (nl) 1972-11-07 1975-09-05 Verbetering van de werkwijze voor het afscheiden van onoplosbaar materiaal uit een vloeibaar koolprodukt onder toepassing van een vloeibare promotor met een bepaalde karakteriseringsfactor.
FR7527287A FR2283944A2 (fr) 1972-11-07 1975-09-05 Procede pour eliminer les cendres de produits de liquefaction du charbon

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US00304319A US3856675A (en) 1972-11-07 1972-11-07 Coal liquefaction

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US3856675A true US3856675A (en) 1974-12-24

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Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3932266A (en) * 1973-12-12 1976-01-13 The Lummus Company Synthetic crude from coal
US3954595A (en) * 1974-03-18 1976-05-04 The Lummus Company Coal liquefaction
US3974073A (en) * 1974-09-06 1976-08-10 The Lummus Company Coal liquefaction
US3997425A (en) * 1974-12-26 1976-12-14 Universal Oil Products Company Process for the liquefaction of coal
US4040957A (en) * 1976-02-20 1977-08-09 The Lummus Company Separation of insoluble material from coal liquefaction product by use of a diluent
DE2725020A1 (de) * 1976-06-01 1977-12-22 Kerr Mc Gee Chem Corp Verfahren zur kohle-entaschung
JPS5316705A (en) * 1976-06-01 1978-02-16 Kerr Mc Gee Corp Method of removing ash from coal
US4075080A (en) * 1976-02-18 1978-02-21 Continental Oil Company Coal liquefaction process with removal of agglomerated insolubles
US4077866A (en) * 1976-10-01 1978-03-07 Mobil Oil Corporation Process for producing low-sulfur liquid and solid fuels from coal
US4077881A (en) * 1976-07-08 1978-03-07 The Lummus Company Separation of insoluble material from coal liquefaction product by gravity settling
US4090958A (en) * 1976-02-23 1978-05-23 Kerr-Mcgee Corporation Coal processing system for producing a stream of flowable insoluble coal products
US4102775A (en) * 1977-08-15 1978-07-25 The Dow Chemical Company Conversion process for solid, hydrocarbonaceous materials
DE2834475A1 (de) * 1977-08-18 1979-03-01 Lummus Co Verfahren zur behandlung eines pyrolyse-heizoels
US4148716A (en) * 1977-10-21 1979-04-10 Gulf Research & Development Company Process for separating tar and solids from coal liquefaction products using a halogenated aliphatic solvent
US4162956A (en) * 1978-03-20 1979-07-31 Kerr-Mcgee Corporation Coal deashing process having improved solvent recovery techniques
US4172024A (en) * 1978-06-15 1979-10-23 The Lummus Company Catalyst withdrawal and addition in a coal liquefaction process
US4207168A (en) * 1977-08-18 1980-06-10 The Lummus Company Treatment of pyrolysis fuel oil
US4216074A (en) * 1978-08-30 1980-08-05 The Lummus Company Dual delayed coking of coal liquefaction product
US4292170A (en) * 1977-07-28 1981-09-29 The Lummus Company Removal of quinoline insolubles from coal derived fractions
US4310422A (en) * 1980-02-13 1982-01-12 Bergwerksverband Gmbh Method of processing and recirculating filtration residues
US4402821A (en) * 1981-11-13 1983-09-06 Mobil Oil Corporation Process for liquefaction of coal
EP0087965A2 (en) * 1982-02-27 1983-09-07 SANDWELL & COMPANY LIMITED Process for separation of solids from liquid hydrocarbons
US4410414A (en) * 1980-01-18 1983-10-18 Hybrid Energy Systems, Inc. Method for hydroconversion of solid carbonaceous materials
US4420404A (en) * 1981-01-21 1983-12-13 Dravo Corporation Process for dewatering fine granular materials
US4470900A (en) * 1978-10-31 1984-09-11 Hri, Inc. Solids precipitation and polymerization of asphaltenes in coal-derived liquids
US4487682A (en) * 1979-07-17 1984-12-11 Coal Industry (Patents) Limited Coal extraction
DE3508897A1 (de) * 1984-03-16 1985-09-19 Lummus Crest Inc., Bloomfield, N.J. Verfahren zur verfluessigung von sub-bituminoeser kohle
US4863586A (en) * 1987-05-07 1989-09-05 Veba Oel Entwicklungs-Gesellschaft Mbh Process for recovery of low-temperature carbonization oil

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1516145A (en) * 1972-11-07 1978-06-28 Lummus Co Liquefaction of coal
DE2504488C2 (de) * 1975-02-04 1985-06-13 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zum Abtrennen der Feststoffe aus staubhaltigen hochsiedenden Kohlenwasserstoffen
DE2654635B2 (de) * 1976-12-02 1979-07-12 Ludwig Dr. 6703 Limburgerhof Raichle Verfahren zur kontinuierlichen Herstellung von Kohlenwasserstoffölen aus Kohle durch spaltende Druckhydrierung
JPH0819418B2 (ja) * 1990-10-24 1996-02-28 日本褐炭液化株式会社 石炭の液化方法

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US3519553A (en) * 1968-04-08 1970-07-07 Hydrocarbon Research Inc Coal conversion process
US3687837A (en) * 1970-08-27 1972-08-29 Exxon Research Engineering Co Coal liquefaction solids removal
US3791956A (en) * 1973-02-16 1974-02-12 Consolidation Coal Co Conversion of coal to clean fuel

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FR840583A (fr) * 1937-07-15 1939-04-27 Int Hydrogeneeringsoctrooien Procédé pour éliminer mécaniquement les substances solides des résidus d'huile
US3535224A (en) * 1968-06-25 1970-10-20 Universal Oil Prod Co Coal liquefaction process
US3598718A (en) * 1969-08-18 1971-08-10 Universal Oil Prod Co Solvent extraction of coal
US3607716A (en) * 1970-01-09 1971-09-21 Kerr Mc Gee Chem Corp Fractionation of coal liquefaction products in a mixture of heavy and light organic solvents

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3519553A (en) * 1968-04-08 1970-07-07 Hydrocarbon Research Inc Coal conversion process
US3687837A (en) * 1970-08-27 1972-08-29 Exxon Research Engineering Co Coal liquefaction solids removal
US3791956A (en) * 1973-02-16 1974-02-12 Consolidation Coal Co Conversion of coal to clean fuel

Cited By (32)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3932266A (en) * 1973-12-12 1976-01-13 The Lummus Company Synthetic crude from coal
US3954595A (en) * 1974-03-18 1976-05-04 The Lummus Company Coal liquefaction
US3974073A (en) * 1974-09-06 1976-08-10 The Lummus Company Coal liquefaction
US3997425A (en) * 1974-12-26 1976-12-14 Universal Oil Products Company Process for the liquefaction of coal
US4075080A (en) * 1976-02-18 1978-02-21 Continental Oil Company Coal liquefaction process with removal of agglomerated insolubles
US4040957A (en) * 1976-02-20 1977-08-09 The Lummus Company Separation of insoluble material from coal liquefaction product by use of a diluent
FR2341640A1 (fr) * 1976-02-20 1977-09-16 Lummus Co Procede pour separer une matiere insoluble d'un produit de liquefaction de la houille
US4090958A (en) * 1976-02-23 1978-05-23 Kerr-Mcgee Corporation Coal processing system for producing a stream of flowable insoluble coal products
JPS5614709B2 (nl) * 1976-06-01 1981-04-06
JPS5316705A (en) * 1976-06-01 1978-02-16 Kerr Mc Gee Corp Method of removing ash from coal
DE2725020A1 (de) * 1976-06-01 1977-12-22 Kerr Mc Gee Chem Corp Verfahren zur kohle-entaschung
US4077881A (en) * 1976-07-08 1978-03-07 The Lummus Company Separation of insoluble material from coal liquefaction product by gravity settling
US4077866A (en) * 1976-10-01 1978-03-07 Mobil Oil Corporation Process for producing low-sulfur liquid and solid fuels from coal
US4292170A (en) * 1977-07-28 1981-09-29 The Lummus Company Removal of quinoline insolubles from coal derived fractions
US4102775A (en) * 1977-08-15 1978-07-25 The Dow Chemical Company Conversion process for solid, hydrocarbonaceous materials
FR2400548A1 (fr) * 1977-08-18 1979-03-16 Lummus Co Procede de traitement de fuels de pyrolyse contenant des asphaltenes
DE2834475A1 (de) * 1977-08-18 1979-03-01 Lummus Co Verfahren zur behandlung eines pyrolyse-heizoels
US4207168A (en) * 1977-08-18 1980-06-10 The Lummus Company Treatment of pyrolysis fuel oil
US4148716A (en) * 1977-10-21 1979-04-10 Gulf Research & Development Company Process for separating tar and solids from coal liquefaction products using a halogenated aliphatic solvent
US4162956A (en) * 1978-03-20 1979-07-31 Kerr-Mcgee Corporation Coal deashing process having improved solvent recovery techniques
US4172024A (en) * 1978-06-15 1979-10-23 The Lummus Company Catalyst withdrawal and addition in a coal liquefaction process
US4216074A (en) * 1978-08-30 1980-08-05 The Lummus Company Dual delayed coking of coal liquefaction product
US4470900A (en) * 1978-10-31 1984-09-11 Hri, Inc. Solids precipitation and polymerization of asphaltenes in coal-derived liquids
US4487682A (en) * 1979-07-17 1984-12-11 Coal Industry (Patents) Limited Coal extraction
US4410414A (en) * 1980-01-18 1983-10-18 Hybrid Energy Systems, Inc. Method for hydroconversion of solid carbonaceous materials
US4310422A (en) * 1980-02-13 1982-01-12 Bergwerksverband Gmbh Method of processing and recirculating filtration residues
US4420404A (en) * 1981-01-21 1983-12-13 Dravo Corporation Process for dewatering fine granular materials
US4402821A (en) * 1981-11-13 1983-09-06 Mobil Oil Corporation Process for liquefaction of coal
EP0087965A2 (en) * 1982-02-27 1983-09-07 SANDWELL & COMPANY LIMITED Process for separation of solids from liquid hydrocarbons
EP0087965A3 (en) * 1982-02-27 1984-01-11 Sandwell & Company Limited Process for separation of solids from liquid hydrocarbons
DE3508897A1 (de) * 1984-03-16 1985-09-19 Lummus Crest Inc., Bloomfield, N.J. Verfahren zur verfluessigung von sub-bituminoeser kohle
US4863586A (en) * 1987-05-07 1989-09-05 Veba Oel Entwicklungs-Gesellschaft Mbh Process for recovery of low-temperature carbonization oil

Also Published As

Publication number Publication date
DE2355606C2 (de) 1981-10-15
AU6214873A (en) 1975-05-08
ZA738417B (en) 1974-09-25
FR2205564A1 (nl) 1974-05-31
BE806789A (fr) 1974-02-15
GB1452297A (en) 1976-10-13
DE2355606A1 (de) 1974-05-16
CS186778B2 (en) 1978-12-29
JPS521922B2 (nl) 1977-01-19
NL7315260A (nl) 1974-05-09
NL174064B (nl) 1983-11-16
JPS4997802A (nl) 1974-09-17
AU469767B2 (en) 1976-02-26
IT996915B (it) 1975-12-10
CA1004618A (en) 1977-02-01
LU68727A1 (nl) 1974-01-08
NL174064C (nl) 1984-04-16
FR2205564B1 (nl) 1978-10-27

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