US20110203164A1 - method of liquefaction of inflammable minerals - Google Patents

method of liquefaction of inflammable minerals Download PDF

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US20110203164A1
US20110203164A1 US13/125,989 US200913125989A US2011203164A1 US 20110203164 A1 US20110203164 A1 US 20110203164A1 US 200913125989 A US200913125989 A US 200913125989A US 2011203164 A1 US2011203164 A1 US 2011203164A1
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milling
hydrogenation
raw material
inflammable
stage
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US13/125,989
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Chuluun Enkhbold
Brodt Alexander
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Assigned to ENKHBOLD, CHULUUN reassignment ENKHBOLD, CHULUUN ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ALEXSANDER, BRODT
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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
    • C10G1/08—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
    • 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
    • C10G1/06—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by destructive hydrogenation
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/80—Additives
    • C10G2300/802—Diluents

Definitions

  • the invention is related to the technology of producing synthetic liquid fuel and can be applied to the processing of brown and bituminous coals, shale oil and other sapropelites, as well as lignites, peat, bituminous and sub-bituminous coals and other kinds of fossil power-generating minerals into synthetic petroleum products.
  • a method of coal liquefaction in the medium of lower aliphatic alcohols is known (see, for instance, Author's Certificate of the USSR No. 997441. According to this method, the initial dry raw material is milled, mixed with alcohol, the obtained suspension is heated to the necessary temperature, and coal liquefaction is carried out under an elevated pressure with a subsequent separation of the liquid phase from the remaining non-liquefied solid residue.
  • the mentioned method is characterized by a relatively low coal liquefaction efficiency and a significant non-productive alcohol consumption due to a considerable dehydration of the latter at high temperatures and elevated pressures.
  • a method of liquefaction of inflammable minerals which is the closest to the claimed one in its technical idea and the achieved effect, includes preliminary milling of the initial power-generating raw material, its subsequent mixing with paste-forming substance representing a product of petroleum or coal origin, heating of the homogenized paste prepared in this way, and hydrogenation of coaly substance forming a part of the processed inflammable mineral by its interaction with hydrogen under elevated pressure and at a high temperature in the presence of a catalyst. Then the reacted mixture is separated from the inert residue remaining in the solid state, and the obtained artificial petroleum is rectified into fractions, which results in the production of various kinds of liquid fuel and other mineral oil products.
  • the described technology does not ensure, nevertheless, its complex use, because in the course of dry coal milling, methane and other gaseous combustible hydrocarbons saturating the latter are released into the gaseous phase as its new solid surface becomes exposed. They get irreversibly lost volatilizing into the atmosphere and, moreover, destroy the stratospheric ozone.
  • the initial raw material treatment is started with its preliminary milling in two stages realized in mineral salts solution.
  • mineral salts solution Only inorganic compounds catalyzing the hydrogenation process and possessing a high solubility in water can be used as such mineral salts, because the initial raw material milling according to the invention is carried out in a solution saturated to the density exceeding that of inflammable mineral, but inferior to that of waste rock.
  • mineral components of the initial raw material are separated, namely, a light product representing an inflammable mineral floats up from the zone of the impact of milling bodies, whereas a heavy product consisting mainly of waste-rock minerals sinks in such medium.
  • methane discharge from the disintegrated material into the gaseous phase takes place; the former is capped for external consumers and serves as a raw material for producing hydrogen to be used in the process of hydrogenation.
  • a suspension of the light product of the first milling stage is heated before the second milling stage, and a repeated milling of this material is carried out in the hot regime.
  • the light product of the second, hot milling stage is mixed after its dehydration with paste-forming agent, the obtained mixture is diluted with diluent, the solid phase of this paste is levigated to the colloidal size and fed to hydrogenation. After that, non-liquefied solid residue is rinsed with organic diluent, dried and mixed with dehydrated heavy product of the first milling stage.
  • the obtained mixture of inert minerals is rinsed with water and removed from the production cycle. Washing water left after rinsing this production waste is evaporated to the original density, and the regenerated aqueous solution is returned to the first milling stage. The heavy product of the second milling stage is squeezed from excessive liquid phase, cooled down and also returned to the process starting point.
  • Both individual mineral salts with a sufficiently high water solubility such as zinc or tin chlorides, ammonium molybdates or iron sulfates, and their various mixtures can be used as water-soluble compounds catalyzing the hydrogenation process.
  • Water solubility of these hydrogenation catalysts is sufficient for preparation on their basis aqueous solutions with the density sufficient for floating of inflammable components of the initial raw material.
  • compositions consisting of products of oil-refining, by-product-coking industry or fine organic synthesis containing organic substances of aromatic series capable of acting at their heating as atomic hydrogen donors (for instance, a mixture of tetraline with anthracene oil diluted with isopropyl alcohol) can be used as a paste-formative substance for realizing the method of the present invention.
  • the realization of the method of the invention ensures an essential decrease in power consumption of this industrial process.
  • the invention possesses not only novelty, but also essential distinctive features imparting a number of obvious technical and economical advantages to the method of the invention, which favorably distinguish the latter from known engineering solutions in the area of synthetic liquid fuel production.
  • Freshly-mined (or delivered to the processing site by hydrotransport) initial lump coal is charged into tumbling ball mill 1 flooded with aqueous solution of hydrogenation catalyst representing a 40% aqueous solution of zinc chloride with the density 1.417 g/cm 3 .
  • aqueous solution of hydrogenation catalyst representing a 40% aqueous solution of zinc chloride with the density 1.417 g/cm 3 .
  • the finest particles of the combustible mineral which are not contaminated by waste rock and not conjoined with it, do not sink and remain afloat on the surface of such liquid medium, while the rest of the initial raw material components submerge into the zone of milling bodies impact.
  • mill 1 The discharge of mill 1 is fed to sump 3 equipped with a stirrer, wherefrom it is fed by pump 4 to hydrocyclone 5 , where a more intense separation of coal (after milling in mill 1 ) from contaminating mineral impurities representing heavier components of the initial power-generating raw material takes place.
  • the light product of the first milling stage discharged from the cylindrical part of hydrocyclone 5 is fed to container 6 with an agitator heated by steam. As a result of heating, the density of the liquid phase of such suspension drops from 1.417 g/cm 3 (at 20° C.) to 1.344 g/cm 3 (at 100° C.).
  • this hot technological flow is fed to the second milling stage, which is realized in a heated (but not reaching the boiling temperature) solution of zinc chloride in water, in tumbling ball mill 8 , which is also connected by its end face to methane manifold 2 and covered with a thick layer of thermal insulation.
  • the heavy product of the first milling stage discharged from the conical part of hydrocyclone 5 is squeezed from the excessive liquid phase on centrifugal filter 7 and fed to mixer 35 for mixing with the remaining solid phase extracted out of the heavy hydrogenate in the end of the flow chart.
  • the fugate of centrifuge 7 is returned to the first milling cycle for mixing with the initial as-received coal fed to mill 1 .
  • the flow discharged from mill 8 similarly to the discharge of mill 1 , is also fed to separation.
  • the latter is realized in sedimentation centrifuge 9 (and not in a hydrocyclone), which is thermally insulated, just as mill 8 , in order to prevent the return of the liquid phase density to its initial value, at which the first stage of milling was carried out.
  • a high-purity coaly material representing the light product of the second milling stage which is wholly free from visible mechanical impurities, is carried out together with the fugate of sedimentation centrifuge 9 .
  • the discharged cake representing the heavy product of the second milling stage and containing residues of the combustible substance is returned to mill 1 for regrinding in a cold aqueous salt solution of the initial density by means of elevator 10 equipped with a cooling jacket and blown by a fan for cooling the transported material to the ambient temperature.
  • the final deep squeezing of the light product of the second milling stage is realized by feeding the fugate of sedimentation centrifuge 9 to centrifugal filter 11 .
  • the obtained hot transparent water-mineral medium is returned by pump 13 from sump 12 to mill 8 , while wet coal cake impregnated with aqueous zinc chloride solution is fed to screw mixer 14 heated with indirect steam in order to mix with hot paste-forming agent.
  • the latter represents tetraline (1,2,3,4-tetra hydronaphthaline C 10 H 12 ) with an admixture of anthracene oil (coal-tar resin fraction boiling within the limits from 270 to 360° C.).
  • mixer 14 operates in rarefaction conditions. Water vapors released in the course of said process are diverted for condensation, and the uniform paste-like mass obtained in screw mixer 14 is further diluted in screw mixer 15 (equipped with a cooling jacket) with a diluent representing isopropyl alcohol (isopropanol CH 3 CHOHCH 3 ) and fed to disperser 16 . In the latter, the solid phase of such diluted paste is levigated to the colloidal size in a strong centrifugal field.
  • the coal deeply purified from mineral impurities and levigated in disperser 16 to ultrafine state is fed, as a liquid homogenized paste, into recuperative heat exchanger 18 by plunger pump 17 equipped with a hydraulic drive.
  • hydrogen preheated in heater 20 is added to the paste fed into said heat exchanger for heating.
  • Heated reaction mixture is fed for final heating to 400° C. into high-pressure pipe furnace 21 heated by gas burners.
  • the mixture leaving hydrogenation reactor 22 passes through hot separator 23 , where vapor/gaseous phase is separated from liquid reaction products carrying out solid phase residues. Vapor/gaseous mixture is removed from hot separator 23 from above and then is fed for heat recuperation into heat exchangers 18 and 20 . After that, it is fed to condenser 24 for cooling and to cold separator 25 —for subsequent separation, with a release of circulation gas returned into the process and light condensed hydrogenate. Meanwhile, a mixture of high-boiling liquid hydrogenation products contaminated with solid particles residues is carried out from the lower part of hot separator 23 into refrigerator 28 , throttled in valve 29 and, after the final pressure release in expander 30 , is accumulated in thickener 31 .
  • Thickened sludge is fed from the latter to a batch centrifugal filter 32 for deep squeezing from the infiltrating liquid phase.
  • the cake squeezed on centrifuge 32 is cleaned on it from the impregnating residues of heavy hydrogenate with an organic solvent, for instance, light petroleum (a mixture of light hydrocarbons, predominantly paraffin hydrocarbons with 5 and 6 carbon atoms), passes through drier 33 and is reloaded to belt conveyor 34 transporting this industrial waste into mixer 35 for mixing with wet heavy product removed from the initial power-generating raw material already at the first stage of its milling. Meanwhile, the discharge of thickener 31 is combined with the fugate of centrifuge 32 , and the resulting heavy hydrogenate, which is completely free from solid particles, is fed to further processing realized within the system of synthetic petroleum processing.
  • an organic solvent for instance, light petroleum (a mixture of light hydrocarbons, predominantly paraffin hydrocarbons with 5 and 6 carbon atoms)
  • the wet mixture of solid industrial wastes obtained in mixer 35 is cleaned with hot water from zinc chloride residues carried out of the technological process by means of countercurrent multi-stage washing on band vacuum filter 37 and withdrawn from the production cycle to storage or utilization.
  • Washing water resulting from the countercurrent washing process which represents a dilute aqueous solution of zinc chloride, is fed from sump 38 by pump 39 into evaporator system 40 for evaporation.
  • Water steam lost by such solution in the course of evaporation is condensed in condenser 41 , and the obtained fresh condensate is returned to the first step of countercurrent washing of solid industrial waste on band vacuum filter 37 .
  • Aqueous solution of zinc chloride in water recovered, in this way, to the required initial density of 1.417 g/cm 3 is continuously discharged from its internal circulation circuit into the starting point of the process by pump 41 with its simultaneous cooling in heat exchanger 42 , and fed to the input of ball mill 1 .
  • Freshly-mined coarse coal (ash level 8.9%, volatile substances content 45.2%, sulfur content 0.8%) is charged into a steel mortar vessel filled with 40% aqueous zinc chloride solution with the density 1.417 g/cm 3 . Then the cleanest coal particles in the initial raw material, which are not contaminated with waste rock, remain afloat in such liquid medium, while the remaining rock mass sinks to the bottom of said vessel. The sunk material is manually ground into smaller fragments using a steel tamper.
  • the hot suspension of finely ground coal poured out of the thermally insulated ball mill is separated on a fast (4000 rpm) sedimentation centrifuge. Sediment pressed to the internal surface of the rotating rotor by centrifugal forces, which is discharged from the centrifuge by means of a rotating screw, is cooled and returned to the steel mortar vessel for mixing with the next batch of the initial rock mass. Meanwhile, the fugate representing a suspension of coal finely cleaned from mineral impurities in aqueous solution of zinc chloride is separated on a centrifugal filter.
  • the paste diluted with isopropyl alcohol is fed to a centrifugal disperser, where the solid phase of this system is additionally disintegrated to a colloidal size.
  • the disperser content is reloaded into a steel autoclave installed afterwards in a muffle furnace with a tangential input of compressed hydrogen (for more efficient mixing), and coal hydrogenation is realized in this medium.
  • the mixture in the autoclave is gradually heated from 80° C. and initial hydrogen pressure of 2 MPa to the temperature 405° C. and the pressure of 11 MPa.
  • the autoclave is taken out of the muffle furnace, cooled, depressurized, and the synthetic oil formed therein is separated from solid particles in a centrifugal filter.
  • Solid sediment extracted from said liquid is cleaned from synthetic oil residues by light petroleum, dried with hot air and then rinsed with plenty of warm distilled water, dried and weighed.
  • the obtained dry residue weighs 2.74 gram.
  • This material is mixed with cake obtained by squeezing the heavy product of the first milling stage on a nutsch filter.
  • the obtained waste mixture of solid minerals is washed on the nutsch filter with hot fresh water and withdrawn from the process as waste.
  • the remaining washing water is mixed with the discharge of washing the solid residue extracted from the synthetic oil and evaporated to the density of aqueous zinc chloride solution equal to its initial value 1.417 g/cm 3 .
  • the weight of dry clean residue extracted from the synthetic oil obtained in the autoclave is 1.39 gram.
  • the efficiency of liquefaction of raw material impregnated before its hydrogenation in the autoclave with a mixture of iron sulfate and ammonium molybdate reaches 98.61%.
  • a mixed water-mineral medium is prepared by dissolving a dry mixture of ammonium tetramolybdate (NH 4 ) 2 .4MoO 3 .2H 2 O with iron vitriol FeSO 4 .7H 2 O taken in the weight ratio 84:16 in water.
  • the solution density is brought to 1.296 g/cm 3 by water saturation with said composition of mineral salts at room temperature. After that, freshly-mined coal with the composition as in example 1 is charged into this solution, and liquefaction is performed according to the method described above in example 1.
  • the initial raw material for liquefaction and experimental conditions are the same as in Example 1. However, 40% solution of ferric iron sulfate Fe 2 (SO 4 ) 3 with the density of 1.448 g/cm 3 is used for coal milling. Here the dry clean residue output that has not transformed into synthetic oil amounts to 3.12 grams. Hence, the efficiency of coal processing in this case equals 96.88%.
  • the initial raw material for liquefaction and experimental conditions are the same as in Example 1. However, 40% solution of divalent tin chloride SnCl 2 with the density of 1.414 g/cm 3 is used as a medium for wet coal milling. As a result of such processing, dry residue remaining non-liquefied is 2.89 grams. Hence, the efficiency of coal liquefaction in this case equals 97.11%.
  • Raw material for liquefaction and experimental conditions are the same as in Example 1.
  • the solution for wet coal grinding with the density 1.392 g/cm 3 is prepared by dissolving a mixture of nine-water ferric iron sulfate Fe 2 (SO 4 ) 3 .9H 2 O with five-water quadrivalent tin chloride SnCl 4 .5H 2 O taken in the weight ratio 75:25 in water.
  • the weight of the residue remaining non-liquefied is 2.41 grams; hence, the efficiency of coal liquefaction in this case equals 97.59%.
  • the use of the method of the invention for the production of synthetic liquid fuel undoubtedly, contributes to an essential increase in the technico-economical efficiency of the processing of fossil power-generating raw material, especially that with elevated mineral impurities content, and, at the same time, ensures its complex utilization and increase in liquefaction efficiency, and considerably weakens the harmful impact of the synthetic liquid fuel production on the natural environment.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Extraction Or Liquid Replacement (AREA)
US13/125,989 2008-10-27 2009-02-09 method of liquefaction of inflammable minerals Abandoned US20110203164A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
MN420808 2008-10-27
MN4208 2008-10-27
PCT/IB2009/050517 WO2010049821A2 (en) 2008-10-27 2009-02-09 A method of liquefaction of inflammable minerals

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US (1) US20110203164A1 (ru)
CN (1) CN102203216A (ru)
EA (1) EA019190B1 (ru)
WO (1) WO2010049821A2 (ru)
ZA (1) ZA201102667B (ru)

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IL227549A (en) 2013-07-18 2016-04-21 S G B D Technologies Ltd Methods and systems for compressing and underwater gas
WO2015008274A1 (en) * 2013-07-18 2015-01-22 S.G.B.D. Technologies Ltd. Underwater gas liquefaction, gas field development and processing combustible materials
US9664019B2 (en) 2013-07-18 2017-05-30 S.G.B.D. Technologies Ltd. Underwater gas field development methods and systems
KR102385590B1 (ko) 2014-07-17 2022-04-11 사빅 글로벌 테크놀러지스 비.브이. 수소열분해 공정에서 수소 도너 스트림을 사용한 수소 결핍 스트림의 업그레이드

Citations (3)

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US3536608A (en) * 1968-08-20 1970-10-27 Universal Oil Prod Co Coal liquefaction process
US4460376A (en) * 1979-04-11 1984-07-17 Boliden Aktiebolag Method of recovering high-grade fuel from solid mineral-fuel raw material
US20030160500A1 (en) * 2002-01-09 2003-08-28 Drake Ronald D. Method and means for processing oil sands while excavating

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US4333815A (en) * 1979-03-05 1982-06-08 The United States Of America As Represented By The United States Department Of Energy Coal liquefaction in an inorganic-organic medium
SE8202879L (sv) * 1982-05-07 1983-11-08 Carbogel Ab Vattenuppslamning av ett fast brensle samt sett och medel for framstellning derav
US4617105A (en) * 1985-09-26 1986-10-14 Air Products And Chemicals, Inc. Coal liquefaction process using pretreatment with a binary solvent mixture
US5151173A (en) * 1989-12-21 1992-09-29 Exxon Research And Engineering Company Conversion of coal with promoted carbon monoxide pretreatment
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Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US3536608A (en) * 1968-08-20 1970-10-27 Universal Oil Prod Co Coal liquefaction process
US4460376A (en) * 1979-04-11 1984-07-17 Boliden Aktiebolag Method of recovering high-grade fuel from solid mineral-fuel raw material
US20030160500A1 (en) * 2002-01-09 2003-08-28 Drake Ronald D. Method and means for processing oil sands while excavating

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EA019190B1 (ru) 2014-01-30
ZA201102667B (en) 2011-12-28
WO2010049821A2 (en) 2010-05-06
WO2010049821A3 (en) 2010-08-26
EA201170614A1 (ru) 2012-03-30
CN102203216A (zh) 2011-09-28

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