WO2018007205A1 - Procédé de production parallèle de gaz de synthèse, de carbone, et de charbon résiduel à faible teneur en polluants à partir de lignite - Google Patents

Procédé de production parallèle de gaz de synthèse, de carbone, et de charbon résiduel à faible teneur en polluants à partir de lignite Download PDF

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WO2018007205A1
WO2018007205A1 PCT/EP2017/065847 EP2017065847W WO2018007205A1 WO 2018007205 A1 WO2018007205 A1 WO 2018007205A1 EP 2017065847 W EP2017065847 W EP 2017065847W WO 2018007205 A1 WO2018007205 A1 WO 2018007205A1
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coal
carbon
stage
gas
mol
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PCT/EP2017/065847
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German (de)
English (en)
Inventor
Hans-Juergen Maass
Otto Machhammer
Andreas Bode
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Basf Se
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Priority to DE112017002937.6T priority Critical patent/DE112017002937A5/de
Publication of WO2018007205A1 publication Critical patent/WO2018007205A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K3/00—Modifying the chemical composition of combustible gases containing carbon monoxide to produce an improved fuel, e.g. one of different calorific value, which may be free from carbon monoxide
    • C10K3/001—Modifying the chemical composition of combustible gases containing carbon monoxide to produce an improved fuel, e.g. one of different calorific value, which may be free from carbon monoxide by thermal treatment
    • C10K3/003—Reducing the tar content
    • C10K3/008—Reducing the tar content by cracking
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B47/00—Destructive distillation of solid carbonaceous materials with indirect heating, e.g. by external combustion
    • C10B47/18—Destructive distillation of solid carbonaceous materials with indirect heating, e.g. by external combustion with moving charge
    • C10B47/22—Destructive distillation of solid carbonaceous materials with indirect heating, e.g. by external combustion with moving charge in dispersed form
    • C10B47/24—Destructive distillation of solid carbonaceous materials with indirect heating, e.g. by external combustion with moving charge in dispersed form according to the "fluidised bed" technique
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10F—DRYING OR WORKING-UP OF PEAT
    • C10F5/00—Drying or de-watering peat
    • C10F5/06—Drying or de-watering peat combined with a carbonisation step for producing turfcoal
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
    • C01B2203/0272—Processes for making hydrogen or synthesis gas containing a decomposition step containing a non-catalytic decomposition step
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042—Purification by adsorption on solids
    • C01B2203/043—Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0805—Methods of heating the process for making hydrogen or synthesis gas
    • C01B2203/085—Methods of heating the process for making hydrogen or synthesis gas by electric heating
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0805—Methods of heating the process for making hydrogen or synthesis gas
    • C01B2203/0866—Methods of heating the process for making hydrogen or synthesis gas by combination of different heating methods
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
    • C01B2203/1205—Composition of the feed
    • C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
    • C01B2203/1235—Hydrocarbons
    • C01B2203/1247—Higher hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
    • C01B2203/1205—Composition of the feed
    • C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
    • C01B2203/1235—Hydrocarbons
    • C01B2203/1252—Cyclic or aromatic hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0913—Carbonaceous raw material
    • C10J2300/095—Exhaust gas from an external process for purification

Definitions

  • the present invention involves chemical utilization of coal, particularly lignite, with a lower carbon footprint than in the prior art.
  • the current processes for the chemical use of lignite e.g.
  • Coal gasification have a high carbon footprint.
  • the production of hydrogen from coal via coal gasification releases about twice as much carbon dioxide as the production of hydrogen from natural gas.
  • the present invention is intended to make it possible, in parallel, to produce so-called inferior coal having a low calorific value, e.g. Brown coal, a
  • Synthesis gas for the production of organic products e.g. methanol
  • Products have a lower carbon footprint than the combination of the known processes for the preparation of the products hydrogen, carbon and carbon, such as e.g. coal gasification and methane steam reforming to produce hydrogen, and oil refining to produce (pet) coke.
  • the inventive method should not be greater than when these products are made from petroleum or natural gas.
  • Coal is a natural product with a very different composition.
  • Lignite composition indicated: carbon of 65-75% by weight, hydrogen of 8-5.5% by weight, oxygen of 30-12% by weight, volatiles of 60-43% by weight and calorific value of 7-13 MJ / kg.
  • the Federal Association brown coal DEBRIV gives in
  • German lignite ash content of 2.5 - 20 wt%, water content of 40 - 60 wt% and sulfur content of 0.15 - 3.5 wt%.
  • lignite is used primarily for electricity generation.
  • the lignite is burned, creating the climate-damaging carbon dioxide.
  • Chemically, the Lignite via gasification and hydrogenation for the production of fuels, via charring and extraction as raw material for the chemistry, via coking for the
  • the product range from gasoline to waxes and tars to tar coke is more cost-effective since, for example, the handling of liquids is easier than that of
  • the generated gas mixture contains carbon monoxide, carbon dioxide, hydrogen and water as well as methane, which is thermally decomposed in a second stage into hydrogen and carbon.
  • the generated carbon is returned to the gasification.
  • the generated gas can be used after purification as a synthesis gas for methanol production or Fischer-Tropsch synthesis.
  • a disadvantage of this method is the need for a catalyst and high pressures in the gasification reaction, which usually entail high investment costs. There is a risk that the generated
  • Fluidized bed at about 600 ° C is manwelt. Part of the resulting carbonization gas is withdrawn from the process, freed from the entrained coke dust, to a
  • Gas treatment plant performed in which the tar condensation and gas purification are performed.
  • the discharged carbonization gas is used as heating gas.
  • the other Part of the resulting carbonization is used for heating an exhaust gas stream, which serves for preheating the coal used, and then returned to the fluidized bed.
  • the coke is in an Enderhitzer on a over the
  • the exhaust gas produced during the final heating is used to pre-heat the coal to be smoldered.
  • the produced tar oil can be used in the production of naphthalene, anthracene or phenanthrene. In this single-stage
  • DE 2 825 691 A1 discloses a process for the production of shaped coke in which a mixture of fine coal, grass and non-coke agglomerates is moved downwards in an oven and the mixture in one
  • Preheating section is heated to a temperature of 370 to 540 ° C to form Grus and initiate the release of the volatiles of the coal.
  • the temperature of the preheated coal mixture is further increased within a devolatilizer furnace section to 650-1300 ° C to form discrete coke agglomerates of plastic consistency.
  • the coke agglomerates are then cooled with carbon dioxide gases to a range of 315 to 40 ° C to cure the coke agglomerates. Then they are removed together with the grus from the oven, the coke agglomerates and the grus separated by sieves and the Grus in the oven cycle
  • the released in the heating of the coal or coke gases comprise at its discharge point, the volatile carbon constituents, carbon dioxide and different proportions of hydrogen and carbon monoxide depending on the gas temperature. Chemical use of the volatile carbon components is not disclosed. The parallel production of high-purity carbon is not possible with this one-step process.
  • EP 80 549 A2 discloses a process for obtaining pyrolysis gas from combustible materials, e.g. Plastic waste, crushed and subsequently in one
  • the resulting carbonization gases are passed through a arranged in the heating of the Verschwelungsreaktors cracker and the larger gas molecules cracked in this without partial combustion at temperatures of 1000 to 1200 ° C, i. cleaved into smaller gas molecules without cleaving methane and thus without precipitating solid.
  • the resulting cracking gases are then cooled and fed into a wet scrubber, where the impurities are deposited. These cracked gases are then energetically utilized, e.g. in a power plant. In this one-step process, the simultaneous production of syngas and high purity carbon is not possible.
  • Coke oven part of the volatile hydrocarbons in the coal by heating to a temperature of 900 to 1400 ° C pyrolyzed. The remainder of the volatile components are released and filtered off with suction. This is essentially made of carbon existing coke and a coke oven gas.
  • the coke oven gas contains hydrogen, methane,
  • Granules e.g. Coal thermally decomposed into carbon and hydrogen.
  • coal is used as an inert material for the deposition of thermally produced carbon.
  • a utilization of coal as a chemical raw material is not described. There is no indication that the gas to be used would be coal carbonization or coal vaporization gas.
  • EP 2 987 769 describes a process for the production of synthesis gas in which carbon and hydrogen are obtained from hydrocarbon by thermal decomposition, wherein at least a part of the carbon obtained in a coal power plant for electricity production oxidizes and at least part of the hydrogen obtained with
  • Carbon dioxide is converted to carbon monoxide and water. Again, one will be
  • Hydrogen-containing dome gases such as or blast furnace gas from a blast furnace, converter gas from the crude steel production and / or coke oven gas from the pyrolysis of hard coal,
  • WO 2013/2691 describes a combination of gasification and pyrolysis of
  • Substance mixture resulting raw gas is introduced into a cracking reactor.
  • the raw gas is reacted in the presence of pyrolysis coke and the ash from the gasification with the aid of steam in synthesis gas.
  • the pyrolysis coke is burned in a third step with air. Accordingly, no pyrolysis coke is discharged.
  • the invention is based on the object to develop a method that makes it possible from the large incidence of low-rank coal with low Kohlenohlungsgrad, especially with a molar H to C ratio in the water and ash-free coal greater than 0.6 , eg Brown coal, three high quality, separately available products such as
  • the synthesis gas can be used for example for the production of organic products, such as methanol, dimethyl ether, gasoline or diesel.
  • the high-purity carbon can replace, for example, refinery petroleum coke.
  • the degree of coalification characterizes the chemical and physical properties of the coals such as water content, carbon content, volatile content, calorific value and vitreous reflection (Maceral).
  • High purity carbon in this context means that the carbon content is greater than 99.9 mol%, preferably greater than 99.95 mol%.
  • the object is achieved according to the invention with a process for the parallel production of synthesis gas, carbon and a residual coal from a charcoal with a molar H to C ratio in the water and ash-free coal of greater than 0.5, achieved in that a first stage at least a portion of the volatile constituents of the feed coal are thermally expelled from the feed coal at temperatures of 500 to 1000 ° C and at least a portion of these volatile constituents in a second stage thermally at temperatures of 1000 to 1800 ° C to synthesis gas and carbon reacted and both reaction products of the second stage are discharged from the reactor, wherein the reaction of the second stage as
  • the temperatures in the first stage may be between 400 and 1200 ° C, advantageously between 600 and 900 ° C, preferably between 600 and 800 ° C, more preferably between 700 and 800 ° C, in particular about 750 ° C.
  • the pressure in the first stage is preferably 1 to 25 bar, preferably 1 to 5 bar, in particular 1 to 2 bar.
  • the content of volatiles to be driven can be adjusted by the temperature and pressure range, as well as the size of the
  • the feed coal has a molar H to C ratio in the water- and ash-free coal of greater than 0.55, preferably greater than 0.6.
  • the economic optimum is advantageous a mean "x - 2y" value.
  • the residual coal has a molar H: C ratio of 0.3 to 0.8, preferably from 0.4 to 0.8, in particular from 0.5 to 0.7.
  • the "x-2y" value of the residual carbon is likewise advantageously 0.1 to 0.8, preferably from 0.2 to 0.7, in particular from 0.3 to 0.6. Reduces the value of the residual coal by 10 to 60%, preferably by 30 to 60% and in particular by 40 to 50% with respect to the "x - 2y" value of the feed coal.
  • volatile constituents also called carbonization gases, in particular hydrogen, methane, heavy hydrocarbons such as e.g. Brown coal smolder, carbon monoxide and carbon dioxide.
  • gasoline, yellow oil, creosote oil, gas oil, paraffin oil, hard paraffin, soft paraffin, tar pitch and tar coke can be obtained from lignite smelters.
  • Lignite CHl, 20o, 28 40,9 47,3 1 1, 4
  • the carbonization gas after the first stage has the following composition: hydrogen in the range from 30 to 50 mol% with respect to the total amount of carbonization gas, preferably from 30 to 45 mol%, in particular from 40 to 45 mol%; Methane in the range from 25 to 15 mol%, preferably from 20 to 25 mol%, heavy hydrocarbons in the range from 4 to 1 mol%, preferably from 3 to 4 mol%, carbon monoxide in the range from 10 to 20 mol%, preferably from 10 to 15 mol%, carbon dioxide in the range from 5 to 15 mol%, preferably in the range from 5 to 10 mol%.
  • the oxygen content of the carbonization gas is advantageously from 1 to 25 mol .-%, preferably from 2 to 20 mol .-%, in particular from 5 to 15 mol .-%.
  • less than 25 mol% of steam is preferably fed in relation to the optionally predried charge coal, preferably less than 10 mol%, particularly preferably less than 5 mol%; In particular, no water vapor is added in the first stage.
  • the first stage less than 10 mol% of oxygen, with respect to the optionally pre-dried feed coal, is fed, preferably less than 5 mol%; In particular, no oxygen is added in the first stage.
  • the feed coal used in the first stage consists of predried lignite whose water content after drying is preferably between 0 and 25% by weight, more preferably between 1 and 15% by weight, most preferably between 2 and 12% by weight, in particular between 5 and 10% by weight.
  • Pre-drying is advantageously carried out with the aid of a vapor compression, as in the
  • the smoldering in the first stage advantageously converts the char to a low-emission residual coal that has a calorific value between 22 and 28 MJ / kg ashless, typically 24 to 26 MJ / kg.
  • the low-emission residual coal is advantageously discharged from the Verschwelungsreaktor or the reactor region of the carbonization.
  • Low-pollutant in this context means that the residual carbon based on the initial amount of pollutants contains at least 10% less pollutants, preferably at least 30% less, especially at least 50% less than the feed coal.
  • the first stage, the smoldering, can advantageously be carried out in a rotary kiln, shaft furnace fluidized bed or moving bed reactor.
  • the production bed of the first stage is advantageously a packed bed of the coal used.
  • fixed bed is understood to mean when the solid reactor contents are not fluidized and at rest, the term “moving bed” when the solid reactor contents are not fluidized but move through the reactor, and the term “fluidized bed” the solid reactor contents are at least partially fluidized at least in the reaction zone and move through the reactor
  • Reactor contents are moving, but no longer fluidized.
  • this circulation stream consists of the volatile constituents of the feed coal and, when starting the carbonization, has methane as the base gas, superheated steam and / or carbon dioxide, preferably methane and / or superheated steam, in particular methane.
  • this circulatory stream Before leaving the coal bed, this circulatory stream, which at this point with the volatile
  • the cooling of the recycle stream enriched with the volatile components is expediently carried out only to the extent that no appreciable amounts of volatile components condense, the temperature to be selected depending on the gas composition and the pressure.
  • This enriched circulation stream advantageously with a ratio of cycle gas to gas, which is introduced into the second stage, from 0.1 to 10, preferably 0.5 to 5, more preferably 0.75 to 2.5, in particular 1 to 2, is then advantageously separated into the recycle stream, which is recycled back into the lower end of the coal bed and into a stream which is advantageously fed without further treatment of the second stage.
  • the recycle stream is advantageously further cooled to a temperature of advantageously 20 to 80 ° C. This condense water and the condensable organic components.
  • the thus cooled and dried recycle stream occurs as a circulating stream at the lower end of the coal bed back into this and cools there the exiting residual coal.
  • the condensate from the recycle stream is advantageously separated in a phase separator into a water phase and an organic phase, wherein the organic phase is fed to the second stage in a suitable manner.
  • the first stage energy supply can be both direct and indirect.
  • the type of energy supply can be both electrical and thermal.
  • the endothermic charring in the first stage is maintained by thermal energy.
  • part of the carbonization gases is advantageously oxidized.
  • Fill in the first stage is also oxidized. Serves as an oxidizing agent
  • pure oxygen or oxygen-enriched air having an O 2 content of greater than 80% mol% wherein pure oxygen is understood as meaning strongly enriched air having an O 2 content greater than 99 mol%.
  • a favorable embodiment is the following process: Gas is withdrawn from the hot area of the bed, burned in a combustion chamber with the oxygen and the hot flue gases back into the hot area of the bed
  • the heat of the carbonization is advantageously provided.
  • Heat exchangers installed. These heat exchangers may advantageously have both a plate shape and tubes.
  • the beds can flow both in the pipes and around the pipes.
  • a hot flue gas which gives off its heat through the tube wall to the beds and thereby cools when flowing through the tubes.
  • the heat required in the first stage to drive off the volatiles from the coal may be supplied by electric current. This can be done by electromagnetic induction or by passing electrical current through the bed of the feed coal, which serves as a resistor and thereby heated. Furthermore, the energy input can be effected by indirect electrical heating.
  • a preferred variant of the method according to the invention consists in that the heat required in the first stage for expelling the volatile constituents from the coal is effected by indirect thermal heat supply by combustion of the feed coal or of the residual coal with air.
  • hot flue gases flow through heat exchanger tubes, which are lapped by the charcoal on the outside.
  • the carbonization gases formed in the first stage are advantageously carried out without further cooling outside the reactor of the carbonization or the reactor region of the carbonization and advantageously without further work-up in the second stage.
  • the sulfur compounds and other pollutants contained in the carbonization gases are also advantageously carried to the second stage, in which the thermal reaction takes place.
  • the volatiles cooled by the feed coal bed are removed at the top of the carbonization reactor.
  • An alternative advantageous process control is to remove the volatile constituents from the hot region of the feed coal bed.
  • the volatile constituents in particular the methane and the higher hydrocarbons, advantageously thermally reacted at temperatures preferably between 1000 to 1600 ° C and at pressures between 1 and 25 bar, in synthesis gas and carbon (see, for example, WO 2013/004398) ,
  • the temperatures in the second stage are advantageously between 1000 and 1600 ° C, in particular between 1 100 and 1300 ° C.
  • the pressure in the second stage is preferably 1 to 10 bar, in particular 1 to 5 bar.
  • the pressure in the second stage is 0.01 to 2 bar, preferably 0.01 to 1 bar, preferably 0.01 to 0.5 bar lower than the pressure in the first stage.
  • the first and second stages are thus carried out at a similar pressure level.
  • Support materials preferably heat transfer materials carried out, on which the carbon formed in the cleavage reaction of the hydrocarbons primarily, in particular greater than 90% with respect to the maximum pyrolyzable
  • Carbon content of the carbonization gas adsorbs. These solid supports can be used for regenerative heat integration.
  • the production bed is advantageously a packed bed of solid support materials.
  • the second stage, the thermal decomposition can advantageously be carried out in a fixed bed, fluidized bed or moving bed reactor, wherein the term "fluidized bed” also includes a Production bed is understood when the solid reactor content in the reaction zone is at least partially fluidized and above and / or below the reaction zone of the solid reactor contents moves, but no longer fluidized.
  • the support materials of the production bed are advantageously temperature-resistant in the range from 1000 to 1800 ° C., preferably from 1300 to 1800 ° C., more preferably from 1500 to 1800 ° C., in particular from 1600 to 1800 ° C.
  • temperature-resistant carrier materials advantageously come e.g. ceramic
  • Carrier particles in particular materials according to DIN EN 60 672-3 such.
  • non-standard high performance ceramic materials such as e.g. Quartz glass, silicon carbide, boron carbide and / or nitrides serve as a temperature-resistant support materials. These heat transfer materials can be compared to the deposited thereon
  • a carbonaceous granulate is to be understood as meaning a material which advantageously consists of solid grains which are at least 50% by weight, preferably at least 80% by weight, more preferably at least 90% by weight of carbon, more preferably at least 95 wt .-%, in particular at least 98 wt .-% carbon.
  • the carbonaceous granules are advantageously spherical.
  • a multiplicity of different carbonaceous granules can be used.
  • such granules may consist predominantly of coal, coke, coke breeze and / or mixtures thereof.
  • the carbonaceous granules 0 to 15 wt .-% based on the total mass of the granules, preferably 0 to 5 wt .-%, metal, metal oxide and / or ceramic.
  • the ammonia contained in the carbonization gases is advantageously decomposed in the second stage into nitrogen and hydrogen.
  • the methane and the higher hydrocarbons are largely reacted in an endothermic reaction, advantageously greater than 90% in synthesis gas and carbon due to the high temperatures.
  • Hydrocarbons include, but are not limited to, crude tar, naphthalene and BTX (mixture of benzene, toluene and xylenes). These products are preferably reacted in a thermal conversion to methane.
  • the area in which the methane conversion is to be adjusted depends primarily on the nature of the subsequent processes.
  • the methane conversion can be controlled by the selected pressure and Setting the temperature. It may be advantageous, for example, to not react methane in pyrolysis above 95% and then to discharge the unreacted methane in the subsequent process step. This may be advantageous, for example, if the subsequent process requires a cycle gas process, such as the methanol synthesis or the Fischer-Tropsch process, or the separation of the methane from the pyrolysis in the subsequent process, for example by a pressure swing absorption or a temperature swing absorption, with a lower Effort is possible, as in pyrolysis.
  • sub-stoichiometric reforming means that the O content of the process gas, including the carbonization gases (volatile constituents of the feed coal) and optionally oxygen for autothermal heating, is not in the second stage
  • the molar C: O ratio is greater than 1: 1.
  • the choice of the concrete substoichiometric ratio depends on the desired synthesis gas product stream Synthesis gas (consisting of H2, CO, C02, H20) always also a solid carbon-containing phase
  • Reaction products are discharged from the reactor or the reaction zone of the thermal reaction.
  • x may advantageously be between 1 and 30 and y advantageously between 2 and 60.
  • the ammonia is decomposed during the thermal reaction at least partially, depending on the selected temperature and the pressure in nitrogen and hydrogen.
  • the balance of the Boudouard reaction is on the side of carbon monoxide.
  • the hot product gas of the second stage is advantageously cooled as quickly as possible; this cooling can be carried out particularly preferably by a direct heat transfer from the hot product gas to the cold bed of support materials.
  • the hydrogen to carbon ratio can be adjusted by the pressure chosen due to the reforming reactions to the requirements of the subsequent processes.
  • the carbon formed in the pyrolysis forms in the gas phase or on the support materials and settles on these and is discharged from the pyrolysis reactor.
  • the carbon is now in a high purity state and may be e.g. Replace refinery petroleum coke.
  • the process of the second stage is advantageously carried out without the presence of a technical catalyst, wherein a technical catalyst is characterized in that it is produced and used in a targeted manner.
  • the energy supply to the second stage, the thermal conversion, can also be done both directly and indirectly.
  • the type of energy input can be both electrical and thermal.
  • the direct electrical energy supply can be done both inductively and ohmic.
  • the respective carbonaceous beds represent a corresponding resistance.
  • the ohmic variant since in this case all electrical losses that arise from the end of the external power supply, directly benefit the heating of the beds.
  • the beds can be designed both as a fluidized bed, moving bed or as a fixed bed, in the case of direct electrical heating, the fixed bed variant is preferable.
  • two electrodes are installed in the beds, between which the beds act as an electrical resistance and heat up as the current passes through the electrical feedthrough losses.
  • electric heating elements are lapped by the respective beds. These electric heating elements heat up when electricity flows through them and release this heat to the surrounding beds.
  • oxidizing agent used is, for example, pure oxygen or oxygen-enriched air having an O 2 content of greater than 80 mol%, where pure oxygen is understood as meaning strongly enriched air having an O 2 content greater than 99 mol%.
  • the heat of combustion of the above-mentioned endothermic reactions is advantageously provided by the heat of combustion released during the oxidation.
  • a favorable embodiment is the following process: Gas is withdrawn from the hot area of the respective bed, burned in a combustion chamber with the oxygen and the hot flue gases are redistributed into the hot area of the bed.
  • Heat exchanger installed. These heat exchangers may advantageously have both a plate shape and tubes. In the case of pipes, the beds can flow both in the pipes and around the pipes.
  • a hot flue gas which gives off its heat through the tube wall to the beds and thereby cools when flowing through the tubes.
  • the heat required in the second stage for thermal conversion of the components expelled from the coal is supplied by electric current and / or oxygen addition for an oxidation process.
  • the heat supply can be done by electromagnetic induction or by
  • a further embodiment of the method according to the invention provides that in the second stage, the thermal conversion of methane and the higher
  • Hydrocarbons, used heat transfer material advantageously from a
  • the bed of carbonaceous granules is designed as a moving or fluidized bed.
  • This bed is called carbon bed in the following.
  • a further variant of the process according to the invention provides that the conversion of the volatiles expelled from the coal into synthesis gas and high-purity carbon takes place in the presence of a bed of carbon-rich granules moving from top to bottom, which at least partially recirculates becomes.
  • volatile components are passed whose gaseous reaction products after pyrolysis and gasification or reforming at the upper end of the carbon bed through the
  • Carbon at the lower end is discharged more or less hot.
  • the hot carbon emerging at the lower end of the second stage is cooled by an inert gas stream which flows to the
  • the hot inert gas stream for cooling the exiting hot carbon can also be used to generate steam.
  • This steam can be used on the one hand in the workup process of the process for the conversion of the synthesis gas to methanol or dimethyl ether or for the production of electricity.
  • a further embodiment of the method according to the invention provides that the synthesis gas leaving the second stage is desulfurized and purified (in "Chemischetechnik, Rothe und Kunststoff, Volume 4, Winnacker-Kuchler, 5th edition, Wiley-VCH, p. 353 et seq. ).
  • Gas mixture present pollutants, such as mercury, from the
  • the present after the desulfurization and purification gas consists mainly of hydrogen and carbon monoxide and possibly partially back-reacted
  • Carbon dioxide preferably greater than 80 mol%, more preferably greater than 90 mol%, in particular greater than mol 95% of hydrogen and carbon monoxide or
  • Carbon dioxide wherein the content of re-reacted carbon dioxide is less than 5%
  • An improvement of the method according to the invention is that the process is operated by controlling, inter alia, water content of the feed coal, temperature and pressure of the respective stages such that the gas present after desulfurization and purification has a hydrogen-carbon monoxide ratio corresponding to the requirement of greater than 2.
  • this gas is additionally supplied with carbon dioxide when used for the synthesis of, for example, methanol, dimethyl ether, gasoline or Fischer / T ropsch condensate, so that this process represents a carbon dioxide sink.
  • the products of the synthesis gas e.g., fuels
  • the products of the residual coal e.g., electricity
  • the inventive method allows new opportunities for the use of lignite.
  • lignite Due to the low carbon footprint, the inventive method allows new opportunities for the use of lignite.
  • carbon dioxide is released than in the known processes of coal gasification (see Figure 6).
  • a further advantage of the method according to the invention is the possibility of producing, on the one hand, highly pure carbon and, on the other hand, low-emission residual coal with a relatively high calorific value (about 26 GJ / t ashless).
  • Pollutants in the pyrolysis in the gas phase can be separated in the following from this by known methods.
  • the process according to the invention offers a long-term perspective for low carbon dioxide production of chemical products, liquid fuels, pure carbon as
  • the value of the invention is not the highest
  • Input materials carbon and hydrogen.
  • the carbon may e.g. by CO2 to
  • Lignite has approximately twice as high hydrogen content as hard coal in terms of carbon content.
  • lignite typically have a molar ratio of H to C-1, 2 (hence the formula CH1 2) and coal of only 0.6 (hence the formula CH 0, 6). If the brown coal is withdrawn half of its hydrogen, a residual carbon remains (bottom right in the figure), which has about a molar H to C ratio as hard coal.
  • the carbon footprint basically makes no difference whether the pure carbon and the low-emission residual coal are ultimately re-sequestered or whether they can replace other fossil raw materials in other processes and that these fossil raw materials can remain in the earth.
  • the pure carbon and the low-emission residual coal are ultimately re-sequestered or whether they can replace other fossil raw materials in other processes and that these fossil raw materials can remain in the earth.
  • the high purity carbon could be the high purity carbon
  • Imported coal can be used. For this, the not yet subsidized import coal could be left in the earth. Because only in the promotion and transport of
  • FIG. 2a This is illustrated by a comparison (FIG. 2a).
  • the principle should be clarified, so that no losses and no conversion energies are taken into account, but only the atomic balance.
  • Fuel such as diesel, consists mainly of molecules with the chemical formula (CH2) n.
  • CH2 chemical formula
  • 1 mol of CH 2 should now be prepared from CH 2 O, 0.3, in comparison once by the process according to the invention and once by coal gasification:
  • Atmosphere be withdrawn.
  • the carbon footprint value for electric current corresponds to 0.30 t C02 / MWh e i the expected value, which was calculated by the Federal Ministry for the Environment, Nature Conservation and Nuclear Safety, Berlin 2007 (J. Nitsch, Renewable Energy Saving Strategy - Leistudie 2007)
  • 20.48 tons of wet brown coal are used, from which 1.00 tons of gasoline are produced in a methanol to gasoline (MTG) process, 0.57 tons of pyrolysis coke and 5.94 tons of residual coal.
  • MTG methanol to gasoline
  • the pyrolysis coke and the residual coal correspond to 4.30 t hard coal units. This produces 1, 23 t of carbon dioxide.
  • refinery of 1, 09 t of crude oil produces 1, 00 t of gasoline. This fall with the comparative provision of 4.30 t
  • the process according to the invention also opens up the possibility of excess current
  • the carbonization reactor 5 In the carbonization reactor 5 is a coal bed, which moves due to gravity from top to bottom. Since the migrating coal is simultaneously fluidized by flowing gas, the carbon bed is a fluidized bed. Countercurrent to the downwardly moving coal, it flows against a recycle gas. This enters the carbonization reactor 5 at its lower part, heats up in the flow, wherein it cools the exiting residual carbon. At the upper part of the carbonization reactor 5, the hot recycle gas, which now also contains the volatile components, heats the incoming charge coal, cooling itself to such an extent (see FIG. 4b, 239 ° C.) that no appreciable amounts of volatile components condense out.
  • a carbonization process which can also be referred to as a distillation process, instead.
  • a carbonization process which can also be referred to as a distillation process, instead.
  • 59 kWh of electrical energy are supplied to the smoldering process.
  • the volatiles are expelled from the coal. This produces 290.2 kg low-emission
  • This residual coal is removed via the residual coal discharge 6 from the carbonization reactor 5.
  • the residual coal can be used for the substitution of hard coal or dried lignite.
  • the smoldering process takes place in the carbonization reactor 5 under exclusion of air and without
  • the smoldering process produces 151, 9 kg of carbonization gas.
  • This consists of hydrogen, methane, higher hydrocarbons such as BTX (mixture of benzene, toluene and xylenes), carbon monoxide, carbon dioxide, oxygen, nitrogen,
  • the carbonization gas is removed together with the recycle gas (349.7 kg) via the carbonization line 7. Of these, 215.8 kg are diverted and after drying to give 46.8 kg of carbon monoxide, recycled as recycle gas (168.9 kg) back into the lower part of the carbonization reactor 5. 133.9 kg of carbonization are passed directly into the pyrolysis reactor 8 at a pressure of 5 bar without cooling or other treatment.
  • the carbon black condensate is separated in a phase separator into 28.8 kg of condensate water containing carbon dioxide and ammonia and 18.0 kg of organic condensate consisting of higher hydrocarbons.
  • the organic condensate is fed into the pyrolysis reactor 8 together with the carbonization gas.
  • the pyrolysis reactor 8 is a heat transfer material, which consists in a variant of the method of ceramic balls and is used for heat integration.
  • the supplied carbonization gases are thermally at a temperature of 1400 ° C and a pressure of 5 bar in a second stage of the process
  • the methane and the higher hydrocarbons such as BTX (mixture of benzene, toluene and xylenes) and tar, are decomposed into hydrogen and carbon.
  • Ammonia contained in carbonization gas is also decomposed into nitrogen and hydrogen. Since the carbonization gas also contains oxygen-containing components such as H 2 0 and CO 2 , gasification and reforming reactions take place in the pyrolysis reactor.
  • This carbon is now in a highly purified form as a pyrolysis coke. It is a high-quality product that can replace refinery petroleum coke and be used, for example, for electrode production. It is removed via the carbon line 1 1 from the pyrolysis reactor 8.
  • the heat transfer material moves by gravity from top to bottom. It is being circulated.
  • the carbonization gas coming from the carbonization reactor 5 is passed into the lower part of the pyrolysis reactor 8 and flows upwards in this in countercurrent to the heat transfer material. Since that in the upper part of the
  • Pyrolysis reactor 8 abandoned heat transfer material is relatively cold, the present after the pyrolysis gas mixture cools and thereby heats the heat exchange
  • Pyrolysis reactor 8 exits through the carbon line 9, still hot. He has one
  • Possibility of heat supply is to burn a part of the reactants with pure oxygen.
  • the heat transfer material used in the pyrolysis consists not of ceramic balls, but of a carbon-rich granules, e.g. consists of pyrolysis and is recycled. This 235 kg pyrolysis are recycled.
  • This pyrolysis coke forms in the pyrolysis reactor 8 a coke bed, which is designed as a moving or fluidized bed. The pyrolysis coke is charged at the top of the pyrolysis reactor 8 and moves downwards during pyrolysis due to gravity. The carbonization gas, which at the lower part of the
  • Pyrolysis reactor 8 is abandoned, flows upwards. It will be up to
  • Decomposition temperature of the hydrocarbons heated. After reaching the
  • the pyrolysis coke consists of a pure and high-quality carbon. It is removed via the carbon line 9 from the pyrolysis reactor 8. This will be 28.1 kg
  • the heat of the hot pyrolysis coke is used to dry the feed coal in the dryer 2.
  • the present in the second stage after the pyrolysis gas mixture contains mainly hydrogen, carbon monoxide, ammonia, water vapor, hydrogen sulfide, residual methane and other pollutants, such as mercury u. Like. 137.8 kg of this gas mixture are compressed to about 71 bar and then with a temperature of 190 ° C over the
  • Synthesis gas is the starting material for syntheses for the production of various organic products, such as methanol, dimethyl ether, gasoline and diesel via Fischer / Tschopsch synthesis.
  • Carbon dioxide are passed a total of 150.8 kg of synthesis gas in the synthesis reactor 14.
  • the synthesis products such as methanol, dimethyl ether, gasoline and diesel, are led away from the synthesis reactor 14 through the product line 16.

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Abstract

L'invention concerne un procédé de production parallèle de gaz de synthèse, de carbone et d'un charbon résiduel à partir d'une pâte à coke présentant dans le charbon exempt d'eau et de cendres un rapport H/C supérieur à 0,6, le procédé étant caractérisé en ce que dans une première étape, au moins une partie des composants volatils de la pâte à coke est expulsée thermiquement de la pâte à coke à des température de 500 à 1 000° C et, dans une seconde étape, ces composants volatils sont ensuite convertis thermiquement en gaz de synthèse et en carbone à des températures de 1 000 à 1 800° C et les deux produits de réaction de la seconde étape sont extraits du réacteur, la conversion de la seconde étape étant effectuée sous la forme d'un reformage sous-stœchiométrique et d'une décomposition thermique.
PCT/EP2017/065847 2016-07-06 2017-06-27 Procédé de production parallèle de gaz de synthèse, de carbone, et de charbon résiduel à faible teneur en polluants à partir de lignite WO2018007205A1 (fr)

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Publication number Priority date Publication date Assignee Title
DE102019000803A1 (de) 2019-02-05 2020-08-06 Hans-Jürgen Maaß Verfahren zur Erzeugung von Synthesegas

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