CA2697355A1 - Catalyst-loaded coal compositions, methods of making and use - Google Patents

Catalyst-loaded coal compositions, methods of making and use Download PDF

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Publication number
CA2697355A1
CA2697355A1 CA2697355A CA2697355A CA2697355A1 CA 2697355 A1 CA2697355 A1 CA 2697355A1 CA 2697355 A CA2697355 A CA 2697355A CA 2697355 A CA2697355 A CA 2697355A CA 2697355 A1 CA2697355 A1 CA 2697355A1
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Prior art keywords
catalyst
coal
fraction
loaded
amount
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Granted
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CA2697355A
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French (fr)
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CA2697355C (en
Inventor
Alkis S. Rappas
George Frederick Salem
Edwin J. Hippo
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Greatpoint Energy Inc
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Greatpoint Energy, Inc.
Alkis S. Rappas
George Frederick Salem
Edwin J. Hippo
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Publication of CA2697355A1 publication Critical patent/CA2697355A1/en
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Publication of CA2697355C publication Critical patent/CA2697355C/en
Expired - Fee Related legal-status Critical Current
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • 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
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • 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
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/46—Gasification of granular or pulverulent flues in suspension
    • C10J3/48—Apparatus; Plants
    • C10J3/482—Gasifiers with stationary fluidised bed
    • 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
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/46—Gasification of granular or pulverulent flues in suspension
    • C10J3/54—Gasification of granular or pulverulent fuels by the Winkler technique, i.e. by fluidisation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L9/00—Treating solid fuels to improve their combustion
    • C10L9/08—Treating solid fuels to improve their combustion by heat treatments, e.g. calcining
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L9/00—Treating solid fuels to improve their combustion
    • C10L9/10—Treating solid fuels to improve their combustion by using additives
    • 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
    • C10J2300/0903—Feed preparation
    • C10J2300/0906—Physical processes, e.g. shredding, comminuting, chopping, sorting
    • 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
    • C10J2300/0903—Feed preparation
    • C10J2300/0909—Drying
    • 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
    • C10J2300/093—Coal
    • 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
    • C10J2300/0953—Gasifying agents
    • C10J2300/0973—Water
    • 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
    • C10J2300/0983—Additives
    • 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
    • C10J2300/18—Details of the gasification process, e.g. loops, autothermal operation
    • C10J2300/1807—Recycle loops, e.g. gas, solids, heating medium, water
    • 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
    • C10J2300/18—Details of the gasification process, e.g. loops, autothermal operation
    • C10J2300/1807—Recycle loops, e.g. gas, solids, heating medium, water
    • C10J2300/1823—Recycle loops, e.g. gas, solids, heating medium, water for synthesis gas
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/582—Recycling of unreacted starting or intermediate materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)

Abstract

The present invention relates to catalyst-loaded coal compositions having a moisture content of less than about 6 wt%, a process for the preparation of catalyst-loaded coal compositions, and an integrated process for the gasification of the catalyst-loaded coal compositions. The catalyst-loaded coal compositions can be prepared by a diffusive catalyst loading process that provides for a highly dispersed catalyst that is predominantly associated with the coal matrix, such as by ion-exchange.

Claims (20)

1. A catalyst-loaded coal composition comprising a coal and a gasification catalyst, wherein (i) the coal comprises a matrix containing ion exchange sites comprising acidic functional groups; (ii) the composition has a moisture content of less than about 6 wt%;
(iii) the gasification catalyst is an alkali metal cation or mixtures thereof;
and (iv) the gasification catalyst is present in an amount such that a ratio of catalyst atoms to carbon atoms is in the range of about 0.01 to about 0.1; and characterized in that (v) greater than about 50% of the total amount of the catalyst loaded is associated with the coal matrix by ion exchange on the acidic functional groups of the coal.
2. The composition according to claim 1, characterized in that the composition has a particle size ranging from about 25 microns to about 2500 microns.
3. The composition according to claim 1 or claim 2, wherein the coal is sub-bituminous, bituminous, lignite, anthracite or mixtures thereof.
4. The composition according to any of claims 1-3, characterized in that the coal is sub-bituminous, the gasification catalyst is potassium cation, and wherein the gasification catalyst is present in an amount such that a ratio of catalyst atoms to carbon atoms is in the range of about 0.03 to about 0.05.
5. The composition according to any of claims 1-4, characterized in that the catalyst is highly dispersed throughout the coal matrix.
6. The composition according to any of claims 1-5, characterized in that greater than about 70% of the total amount of catalyst loaded is associated with the coal matrix.
7. A method of preparing a catalyst-loaded coal composition comprising the steps of:
(a) grinding a raw coal;

(b) soaking the ground coal in an excess of aqueous solution comprising a salt of a catalyst to form a slurry, wherein the slurry is at a density within the range from about 5 wt% to about 40 wt% solids;

(c) holding the slurry at a contact temperature and for a contact time so as to provide ample opportunity to achieve substantial and uniform catalyst loading;

(d) dewatering the slurry to form a catalyst-loaded wet coal cake; and (e) thermally-treating the catalyst-loaded wet coal cake under a flow of inert dry gas at a temperature and for a time sufficient to reduce the moisture content to less than about 6 wt%.
8. The method according to claim 7, characterized in that the catalyst is potassium, sodium, lithium or mixtures thereof.
9. The method according to claim 7, characterized in that the solution further comprises a phosphorous- and boron-free wetting agent.
10. The method according to claim 7, characterized in that (i) the ground coal prior to step (b) is separated into a first fraction and a second fraction, wherein the first fraction is larger than the second fraction, and wherein the first and second fractions are in a ratio ranging from greater than 50:50 to 90:10, and wherein the first fraction is used in steps (b)-(d), and the second fraction is thoroughly mixed with said first fraction after steps (b)-(d) before step (e); or (ii) the coal prior to step (a) is separated into a first fraction and a second fraction, wherein the first fraction is larger than the second fraction, and wherein the first and second fractions are in a ratio ranging from greater than 50:50 to 90:10, and wherein the first fraction is used in steps (a)-(d), and the second fraction is ground, and the ground second fraction is thoroughly mixed with said first fraction after steps (a)-(d) before step (e).
11. The method according to claim 7, characterized in that the slurry is held at a contact temperature ranging from about 20°C to about 95°C for a contact time ranging from about 1 hours to about 48 hours.
12. The method according to claim 7, characterized in that the thermally-treating step is performed at a temperature ranging from about 90°C to about 250°C.
13. The method according to claim 7, characterized in that the aqueous solution comprises an amount of the catalyst salt sufficient to provide the catalyst-loaded coal composition having a ratio of catalyst atoms to carbon atoms in the range of about 0.01 to about 0.1.
14. The method according to one or more of claims 7-13, wherein the aqueous solution comprises an amount of said catalyst salt equal to or greater than the amount to achieve saturation ion-exchange loading of the coal.
15. An integrated process for the steady-state gasification of an optimized reactor feed catalyst-loaded coal composition, comprising the steps of:

(a) providing a ground raw coal solid stream into a diffuse catalyst loading contactor;
(b) introducing an influent stream comprising a salt of a catalyst into the diffuse catalyst loading contactor to create a slurry, wherein the influent stream is comprised of a raffinate stream, a recycle stream and a makeup stream;

(c) controlling the amount of catalyst in the influent stream;

(d) holding the slurry at a contact temperature and for a contact time so as to provide ample opportunity to achieve substantial and uniform catalyst loading;

(e) dewatering the slurry by filtration to form a catalyst-loaded wet coal cake and the raffinate solution;

(f) recycling the raffinate solution into the influent stream;

(g) thermally-treating the catalyst-loaded wet coal cake under a flow of inert dry gas to reduce the moisture content to less than about 6 wt%;

(h) gasifying the catalyst-loaded thermally-treated coal composition in a fluidized bed reactor in the presence of steam and a recycled gas at a temperature ranging from about 450°C to about 750°C and a pressure ranging from about 50 psig and about 1000 psig, to produce a char and a raw gas stream comprising methane ;

(i) withdrawing the raw gas stream from the fluidized bed reactor;
(j) withdrawing the char from the fluidized bed reactor;

(k) extracting catalyst from the char; and (l) recycling extracted catalyst into the influent stream as the recycle stream.
16. The integrated process according to claim 15, characterized in that the amount of catalyst in the influent stream is controlled by a method comprising the steps of:

(a) monitoring the amount of catalyst in the raffinate stream;
(b) monitoring the amount of catalyst in the recycle stream; and (c) adjusting the amount of catalyst in the makeup stream.
17. The integrated process according to claim 15 or claim 16, characterized in that the concentration of catalyst in the influent stream is sufficient to provide the catalyst-loaded coal composition having a ratio of catalyst atoms to carbon atoms in the range of about 0.01 to about 0.1.
18. The integrated process according to any of claims 15-17, characterized in that the amount of catalyst in the influent stream ranges from about 0.3 mol/kg to about 3.0 mol/kg.
19. The integrated process according to any of claims 15-18, characterized in that the amount of catalyst in the influent stream is equal to or greater than the amount to achieve saturation ion-exchange loading of the coal.
20. The integrated process according to any of claims 15-19, characterized in that the catalyst-loaded thermally-treated coal composition is as set forth in any of claims 1-6.
CA2697355A 2007-08-02 2008-07-23 Catalyst-loaded coal compositions, methods of making and use Expired - Fee Related CA2697355C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US6613007P 2007-08-02 2007-08-02
US61/066,130 2007-08-02
PCT/US2008/070888 WO2009018053A1 (en) 2007-08-02 2008-07-23 Catalyst-loaded coal compositions, methods of making and use

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CA2697355A1 true CA2697355A1 (en) 2009-02-05
CA2697355C CA2697355C (en) 2012-10-02

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US (1) US8163048B2 (en)
KR (1) KR101138096B1 (en)
CN (2) CN101795761A (en)
AU (1) AU2008282518B2 (en)
CA (1) CA2697355C (en)
WO (1) WO2009018053A1 (en)

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