USRE48040E1 - Integrated chemical looping air separation in large-scale oxy-fuel plants - Google Patents

Integrated chemical looping air separation in large-scale oxy-fuel plants Download PDF

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USRE48040E1
USRE48040E1 US15/352,554 US201215352554A USRE48040E US RE48040 E1 USRE48040 E1 US RE48040E1 US 201215352554 A US201215352554 A US 201215352554A US RE48040 E USRE48040 E US RE48040E
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flue gas
reactor
reduction reactor
recycled
oxygen
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Behdad Moghtaderi
Terry Fitzgerald Wall
Kalpit Vrajeshkumar Shah
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The University of Newcastle
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/73—After-treatment of removed components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02—Preparation of oxygen
    • C01B13/08—Preparation of oxygen from air with the aid of metal oxides, e.g. barium oxide, manganese oxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01K—STEAM ENGINE PLANTS; STEAM ACCUMULATORS; ENGINE PLANTS NOT OTHERWISE PROVIDED FOR; ENGINES USING SPECIAL WORKING FLUIDS OR CYCLES
    • F01K13/00—General layout or general methods of operation of complete plants
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23C—METHODS OR APPARATUS FOR COMBUSTION USING FLUID FUEL OR SOLID FUEL SUSPENDED IN  A CARRIER GAS OR AIR 
    • F23C9/00—Combustion apparatus characterised by arrangements for returning combustion products or flue gases to the combustion chamber
    • F23C9/003—Combustion apparatus characterised by arrangements for returning combustion products or flue gases to the combustion chamber for pulverulent fuel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J15/00—Arrangements of devices for treating smoke or fumes
    • F23J15/06—Arrangements of devices for treating smoke or fumes of coolers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23L—SUPPLYING AIR OR NON-COMBUSTIBLE LIQUIDS OR GASES TO COMBUSTION APPARATUS IN GENERAL ; VALVES OR DAMPERS SPECIALLY ADAPTED FOR CONTROLLING AIR SUPPLY OR DRAUGHT IN COMBUSTION APPARATUS; INDUCING DRAUGHT IN COMBUSTION APPARATUS; TOPS FOR CHIMNEYS OR VENTILATING SHAFTS; TERMINALS FOR FLUES
    • F23L7/00—Supplying non-combustible liquids or gases, other than air, to the fire, e.g. oxygen, steam
    • F23L7/007—Supplying oxygen or oxygen-enriched air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/45—Gas separation or purification devices adapted for specific applications
    • B01D2259/4516—Gas separation or purification devices adapted for specific applications for fuel vapour recovery systems
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23C—METHODS OR APPARATUS FOR COMBUSTION USING FLUID FUEL OR SOLID FUEL SUSPENDED IN  A CARRIER GAS OR AIR 
    • F23C2900/00—Special features of, or arrangements for combustion apparatus using fluid fuels or solid fuels suspended in air; Combustion processes therefor
    • F23C2900/99008—Unmixed combustion, i.e. without direct mixing of oxygen gas and fuel, but using the oxygen from a metal oxide, e.g. FeO
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J2215/00—Preventing emissions
    • F23J2215/50—Carbon dioxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J2900/00—Special arrangements for conducting or purifying combustion fumes; Treatment of fumes or ashes
    • F23J2900/15061—Deep cooling or freezing of flue gas rich of CO2 to deliver CO2-free emissions, or to deliver liquid CO2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23L—SUPPLYING AIR OR NON-COMBUSTIBLE LIQUIDS OR GASES TO COMBUSTION APPARATUS IN GENERAL ; VALVES OR DAMPERS SPECIALLY ADAPTED FOR CONTROLLING AIR SUPPLY OR DRAUGHT IN COMBUSTION APPARATUS; INDUCING DRAUGHT IN COMBUSTION APPARATUS; TOPS FOR CHIMNEYS OR VENTILATING SHAFTS; TERMINALS FOR FLUES
    • F23L2900/00—Special arrangements for supplying or treating air or oxidant for combustion; Injecting inert gas, water or steam into the combustion chamber
    • F23L2900/07001—Injecting synthetic air, i.e. a combustion supporting mixture made of pure oxygen and an inert gas, e.g. nitrogen or recycled fumes
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E20/00—Combustion technologies with mitigation potential
    • Y02E20/30—Technologies for a more efficient combustion or heat usage
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E20/00—Combustion technologies with mitigation potential
    • Y02E20/32—Direct CO2 mitigation
    • Y02E20/322—
    • Y02E20/326—
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E20/00—Combustion technologies with mitigation potential
    • Y02E20/34—Indirect CO2mitigation, i.e. by acting on non CO2directly related matters of the process, e.g. pre-heating or heat recovery
    • Y02E20/344—
    • Y02E20/346—
    • Y02E20/363—
    • 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
    • Y02P20/124—

Definitions

  • This invention relates to a method and apparatus for integrated chemical looping air separation in large-scale oxy-fuel plants and has been devised particularly though not solely for use in large coal-fired power generating plants.
  • ASU air separation unit
  • Oxygen is commonly produced at industrial scales by air separation using cryogenic distillation and adsorption based technologies. Advanced technologies such as membrane separation (e.g. ion-transport membrane, ITM) and in-situ air separation are also being developed for small-volume point-of-use oxygen generation.
  • membrane separation e.g. ion-transport membrane, ITM
  • in-situ air separation are also being developed for small-volume point-of-use oxygen generation.
  • cryogenic systems are employed in large-scale production of high-purity oxygen while adsorption systems are employed at the lower end of the production scale and for lower oxygen purities.
  • cryogenic separation air is liquefied at very low temperatures and, hence, oxygen is selectively removed from the air by distillation.
  • Cryogenic air separation involves a number of key steps, including: (i) air compression; (ii) air liquefaction, and (iii) distillation to separate oxygen from other gases.
  • Membranes rely on a barrier film to separate O 2 from air.
  • the film allows selective permeation of O 2 and can be made from a host of different materials including polysulphone and acetate.
  • More advanced membrane systems, such as ITMs, allow the rapid transfer of oxygen ions, achieving fluxes which are orders of magnitude higher than polymeric membranes.
  • Perovskite membranes e.g. La1-xAxCol1-yFeyO3-I La 1-x A x Co 1-y Fe y O 3-I
  • Oxygen in this process though fully reacts with a fuel leaving no excess oxygen for collection as a product.
  • Membranes are generally modular and can be replicated to satisfy the throughput requirements.
  • thermo-chemical cycles for water splitting have been also studied for hydrogen and oxygen production. Over 250 thermo-chemical cycles have been reported in the literature although only a few have proven to be economically feasible. This is not surprising given that the water splitting reaction is thermodynamically feasible at temperatures in excess of 1600° C., requiring a complex and expensive reactor system driven by solar energy. Electrolysis of water is energy intensive too.
  • cryogenic air separation systems appear to be the only practical option for oxy-fuel applications.
  • a cryogenic air separation unit with a typical specific power consumption of about 0.4 kWh/[m 3 O 2 ] may consume between 10% and 40% of the gross power output of the oxy-fuel plant.
  • Cryogenic ASUs also typically constitute 40% of the total equipment cost or about 14% of the total plant cost.
  • the present invention uses a chemical looping air separation process fully integrated with the processes of a large-scale oxy-fuel power generation plant to achieve this outcome.
  • the present invention provides a method of air separation in large-scale oxy-fuel power generation plants of the type having a boiler to generate steam, said method including the steps of recycling flue gas from the boiler through a reduction reactor that is connected in a chemical looping process with an oxidation reactor such that the reduction reactor produces a mixture of oxygen and recycled flue gas, and feeding said mixture back into the boiler.
  • a controlled proportion of the recycled flue gas from the boiler is fed through the reduction reactor, with the remaining recycled flue gas being fed directly to the boiler.
  • the chemical looping process includes the steps of passing oxidized metal oxide and heat from the oxidation reactor to the reduction reactor, and passing reduced metal oxide from the reduction reactor to the oxidation reactor.
  • the present invention provides apparatus for generating oxygen to be fed into a boiler in a large-scale oxy-fuel power generation plant, said apparatus including a reduction reactor, a flue gas recycling conduit arranged to transfer some of the flue gas emitted in use from the boiler to the reduction reactor, an oxidation reactor connected to the reduction reactor by transfer means arranged to transfer solid particulate material between the reduction reactor and the oxidation reactor, and an outlet conduit arranged to transfer oxygen and recycled flue gas mixture from the reduction reactor back into the boiler.
  • FIG. 1 is a schematic representation of the known chemical looping concept
  • FIG. 2 is a schematic view of a chemical looping air separation process (CLAS) for standalone production of high purity oxygen;
  • CLAS chemical looping air separation process
  • FIG. 3 is a schematic drawing of a typical oxy-fuel coal-fired power plant
  • FIG. 4 is a schematic drawing of a chemical looping air separation process adapted to be integrated into a large-scale oxy-fuel coal-fired power plant according to the invention
  • FIG. 5 is a schematic view of an oxy-fuel coal-fired power plant fitted with an integrated chemical looping air separation process according to the invention
  • FIG. 6 is a graph showing the link between actual partial pressures and equilibrium partial pressures in the process shown in FIG. 4 ;
  • FIG. 7 is a graph showing the results of the chemical equilibrium calculations for the process shown schematically in FIG. 4 ;
  • FIG. 8 is a graph showing the determination of the actual partial pressure in the oxidation and reduction reactor outlets of the process shown schematically in FIG. 4 ;
  • FIG. 9 is a schematic view of alternative recycled flue gas stream locations for CLAS integration with oxy-fuel
  • FIG. 10 is a graph showing a comparison of the operating cost for different oxygen carriers
  • FIG. 11 is a schematic view of oxygen production using steam (CLAS integration with solar or electric heaters);
  • FIG. 12 is a schematic view of oxygen production using recycled CO 2 (CLAS integration with solar or electric heaters);
  • FIG. 13 is a schematic view of oxygen production using steam (CLAS integration with gasifier or boiler systems);
  • FIG. 14 is a schematic view of oxygen production using recycled CO 2 (CLAS integration with gasifier or boiler systems);
  • FIG. 15 is a schematic view of oxygen production using recycled CO 2 (CLAS integration with oxy-fuel furnace);
  • FIG. 16 is a schematic view of oxygen production using recycled CO 2 at high temperatures (CLAS integration with oxy-fuel furnace at high temperature);
  • FIG. 17 is a schematic view of a temperature swing CLAS process
  • FIG. 18 is a graph showing the effect of different integration modes on the operating cost for CLAS.
  • FIG. 19 is a graph showing the O 2 % in the recycled product gas streams
  • FIG. 20 is a schematic view of a hybrid CLAS/Cryogenic Air Separation Unit (CASU) system for oxy-fuel thermal power plant;
  • CASU CLAS/Cryogenic Air Separation Unit
  • FIG. 21 is a schematic view of a CLAS hybrid steam/recycled CO 2 system for oxy-fuel thermal power plant
  • FIG. 22 is a schematic view of a double pipe reactor design for isothermal ICLAS
  • FIG. 23 is a schematic drawing of the process in the reactor shown in FIG. 22 ;
  • FIG. 24 is a similar reactor design to that shown in FIG. 22 with oxygen supplied by a chemical looping based combustor.
  • FIGS. 25A and B show embodiments of a loop seal.
  • the present invention uses the known chemical looping process in a unique manner to integrate that process into large-scale oxy-fuel type power plants running on organic or fossil based (e.g. coal, gas, oil) fuels.
  • organic or fossil based fuels e.g. coal, gas, oil
  • a given chemical reaction e.g. A+B ⁇ C+D
  • a chemical reaction is divided into multiple sub-reactions using solid intermediates (SI) such as metal oxides (MeO) and carbon dioxide scavengers (e.g. CaO).
  • SI solid intermediates
  • MeO metal oxides
  • CaO carbon dioxide scavengers
  • These intermediates are reduced and regenerated in a cyclic fashion through the progress of the sub-reactions.
  • the process is typically carried out by circulation of SI particles via a system of two interconnected reactors (typically fluidised beds) where sub-reactions are executed.
  • A+SI 1 ⁇ C+SI 2 B+SI 2 ⁇ D+SI 1 Overall: A+B ⁇ C+D
  • Chemical looping schemes can be designed in such a manner that the energy and exergy losses of the overall process are minimised while allowing the separation of the undesired products (e.g. CO 2 ) generated from the reactions to be accomplished with ease, yielding an overall efficient and economical process. It is this inherent ability for separation of undesired products, such as CO 2 , which makes the chemical looping process an invaluable tool in low CO 2 emission technologies (e.g. clean coal technologies). Furthermore, the ability to incorporate a diverse range of intermediates (e.g. metal oxides, CO 2 scavengers, etc) provides the chemical looping concept with an unprecedented versatility, enabling it to be used in a wide range of applications.
  • a diverse range of intermediates e.g. metal oxides, CO 2 scavengers, etc
  • This process is shown schematically in FIG. 1 .
  • the chemical looping process has been used to develop a chemical looping air separation process (CLAS) for standalone production of high purity oxygen.
  • CLAS chemical looping air separation process
  • the CLAS process relies on a chemical principle similar to that used in the chemical looping combustion (CLC) which is commonly carried out in a two-step redox reaction. However, by incorporating the concept of oxygen decoupling into the two-step redox reaction, CLAS is able to separate oxygen from normal air. As FIG. 2 illustrates, the CLAS process works in a cyclic fashion by continuous recirculation of metal oxide particles between a set of two interconnected reactors, where oxidation (O 2 coupling, see Eq 1) takes place in an oxidation reactor 1 and reduction (O 2 decoupling, see Eq 2) of carrier particles, takes place in a reduction reactor 2 .
  • oxidation O 2 coupling, see Eq 1
  • reduction O 2 decoupling
  • the system therefore consists of two reactors linked together through a transfer means in the form of a loop-seal 3 , such as that shown in FIGS. 25A and 25B, to prevent gas leakage from one reactor to another.
  • Air is fed into the oxidation reactor so that the incoming reduced carrier particles can be regenerated to a higher oxidation state.
  • the regenerated carrier particles are transported back to the reduction reactor by the transfer means 3 where oxygen decoupling occurs in the presence of steam.
  • the mixture of steam and oxygen exiting from the reduction reactor is passed through a condenser 4 so that steam can be fully separated from O 2 .
  • the product oxygen can be then compressed for storage and delivery or directly fed to another process for on-site use.
  • Table 1 summarises the results of the heat and mass balance analysis for the CuO/Cu 2 O metal oxide system. Since much of the heat required for the CLAS process is provided through waste heat recovery from various parts of the flow-sheet, the net input power (Q net ) is relatively small. It is evident from Table 1 that Q net consistently decreases as the reaction temperature is increased. The volume of product oxygen also diminishes as the reaction temperature is increased. This can be assigned to the fact that equilibrium constrains impose lower oxygen molar flows through the system as the reaction temperature is increased. It is interesting to note that for the present case the specific power varies between 0.041 and 0.053 kWh/m 3 n with an average value of 0.045 kWh/m 3 n .
  • the present invention uses the principles of the CLAS process described above and uses recycled flue gas from a large-scale oxy-fuel power generation plant rather than steam to allow the process to be integrated into oxy-fuel type power plants running on organic (e.g. biomass) or fossil-based (e.g. coal, gas, oil, etc) fuels.
  • organic e.g. biomass
  • fossil-based e.g. coal, gas, oil, etc
  • FIG. 3 For example consider the conventional oxy-fuel coal-fired power plant shown schematically in FIG. 3 . As shown, coal, oxygen (from the ASU) and recycled flue gas are co-fed into the boiler where the mixture is combusted at high temperatures. The heat generated from the combustion process runs a steam cycle which in turn converts the thermal energy into electricity.
  • recycled flue gas here is an important and integral part of the oxy-fuel combustion process because firing pure oxygen in a boiler would result in excessively high flame temperatures which may damage the boiler. Therefore, the mixture must be diluted by mixing with recycled flue gas before it can be fed into the boiler.
  • the present invention employs recycled flue gas rather than steam to provide an Integrated Chemical Looping Air Separation (ICLAS) process during the reduction phase (see FIGS. 4 and 5 ).
  • ICLAS Integrated Chemical Looping Air Separation
  • ICLAS process The working principle of the ICLAS process is similar to that of the CLAS process but the ICLAS process is executed in a distinctly different way.
  • CLAS and ICLAS processes work in a cyclic fashion by continuous recirculation of metal oxide particles between a set of two interconnected rectors, where oxidation (Eq 1, O 2 coupling) and reduction (Eq 2, O 2 decoupling—see FIG. 2 ) of carrier particles take place, respectively.
  • Eq 1, O 2 coupling oxidation
  • reduction Eq 2, O 2 decoupling—see FIG. 2
  • air is first fed into the oxidation reactor for separation of oxygen from air through the oxygen coupling process (i.e. regeneration of reduced carrier particles) and then the oxidised (i.e. regenerated) particles are reduced in a reduction reactor to release oxygen via the oxygen decoupling reaction.
  • the ICLAS unit shown schematically at 5 takes a portion of the recycled flue gas at 6 and passes that portion through a flue gas recycling conduit 7 through a heater exchanger 8 forming part of the ICLAS unit 5 so that the hot recycled flue gas is fed into the reduction reactor 9 .
  • solid particulate material is used to transfer Me x O y (oxidised metal oxide) and heat from the oxidation reactor 11 via transfer means 10 to the reduction reactor 9 and then to return Me x O y-2 (reduced metal oxide) from the reduction reactor 9 to the oxidation reactor 11 .
  • the process taking place in the reduction reactor 9 as previously described results in a mixture of oxygen and flue gas which is transmitted through an inlet conduit 12 back into the boiler 13 .
  • the oxygen and recycled flue gas mixture may be combined with the fresh coal feed at 14 before being fed into the boiler.
  • the successful execution of the ICLAS process largely depends on the ability to exploit the reversible nature of the reactions occurring in both reactors. This can be best accomplished by manipulating the balance between the equilibrium and actual partial pressures (PP) of oxygen over the metal oxide. According to Le Chatelier's principle if a chemical system in equilibrium is disturbed, it will adjust itself to restore equilibrium. In a system with the equilibrium constant K p and reaction quotient Q p (this quantity is calculated by the same expression as K p but using actual conditions) the reaction will shift from products to reactants if Q p >K r . Conversely, if Q p ⁇ K r , the reaction will proceed from reactants to products. This simple principle is employed here to assure the successful operation of the CLAS process.
  • the actual PP in the reduction reactor can be easily adjusted by controlling the flow rates of the incoming steam and outgoing steam/O 2 mixture.
  • the steam therefore, is not merely a carrier gas but most importantly a means of controlling the partial pressure of O 2 in the reduction reactor. Steam is ideally suited for this task since unlike other carrier gases (e.g. He, CO 2 ) it can be easily separated from O 2 by condensation.
  • the approach outlined above faces a number of challenges. Among these perhaps the most important challenge is the development of effective and robust metal oxide oxygen carriers. Very much like CLC type oxygen carriers, the carriers suitable for the ICLAS process should have a number of desirable properties including:
  • the oxygen carriers for the ICLAS process should be able to react reversibly with gaseous oxygen at high temperatures.
  • This additional thermodynamic constraint is a means of differentiating oxygen carriers feasible for the ICLAS process from those only suitable for common redox applications.
  • Numerous studies have been carried out on oxides of transitional metals, such as Fe, Cu, Co, Mn and Ni as potential candidates for redox applications. Thermodynamically, oxides of Cu, Mn and Co are more promising for oxygen decoupling (i.e. ICLAS process) because of their ability to reversibly react with oxygen. But any other metal oxide, solid oxides, or their mixtures with reversible oxygen decoupling properties can be also employed in the ICLAS process.
  • thermodynamic chemical-equilibrium calculations were carried out on oxides of Cu (CuO/Cu 2 O), Mn (Mn 2 O 3 /Mn 3 O 4 ) and Co (i.e. Co 3 O 4 /CoO) as well as a 1:1 physically mixed Mn/Co oxide system to ascertain their feasibility for the ICLAS process.
  • the specific objective was to determine the equilibrium partial pressure (EPP) of oxygen for each metal oxide system.
  • EPP equilibrium partial pressure
  • the approach adopted here was to minimise the Gibbs free energy of the heterogeneous system under consideration. For a given set of pressure and temperature this was achieved by adjusting species mole numbers so that the Gibbs function (G) defined by Eq (3) is minimised:
  • g i 0 is the molar based Gibbs free energy of species i at the reference state
  • I the total number of species in the heterogeneous mixture of metal oxide and gaseous species
  • n i is the mole number of species i
  • P is pressure
  • P o is the pressure at the reference state
  • R is the universal gas constant
  • T is the temperature of the mixture
  • X i is the mole fraction of species i.
  • a ji is the number of j-element in species i
  • ⁇ j is the element mole number of j-element in the system (i.e. 6.023 ⁇ 10 23 multiplied by the number of atoms of type/present in the system).
  • FIG. 7 The results of chemical-equilibrium calculations for the metal oxide systems listed in Table 2 are illustrated in FIG. 7 where the equilibrium partial pressure of oxygen (EPP) has been plotted against temperature. As shown in FIG. 7 , all three oxide systems exhibit similar and promising trends.
  • the Co system has the added advantage of featuring a narrow range of equilibrium temperatures between 750-900° C. Note that narrow range of equilibrium temperature implies that the full range of partial pressures can be covered by limited amount of heating and/or cooling.
  • the minimum equilibrium temperature for the Co system is relatively high and as such it cannot be employed at temperatures below 750° C.
  • the Mn system can be used at temperatures as low as 650° C. but its range of equilibrium temperature is quite wide (650-1000° C.) demanding sizable heating and/or cooling load to cover the full range of partial pressures of interest.
  • the separate set of calculations carried out for the 1:1 physically mixed mixture of Mn/Co metal oxide system showed that the drawbacks of the Mn and Co systems can be notably minimised when pure oxides are mixed.
  • the Mn/Co mixture can be used at temperatures around 650° C. it does not possess a temperature range as wide as that of the Mn which is its main advantage.
  • the actual partial pressure in the reduction reactor can be easily adjusted by controlling the flow rates of the incoming recycled flue gas and outgoing O 2 /flue gas mixture.
  • the flue gas therefore, is not merely a carrier gas but most importantly a means of controlling the partial pressure of O 2 in the reduction reactor.
  • the heat transported by the incoming carrier particles into the reduction reactor is sufficient to support the endothermic oxygen decoupling process.
  • some heat must be supplied to the reduction reactor to compensate for heat losses to the surrounding.
  • no additional heat is also required for generation of superheated steam in the ICLAS process.
  • much of the required heat duty is offset by utilising the flue gas stream which is already hot.
  • Our preliminary calculations suggest that the heat demand for the ICLAS process is ⁇ 0.03 kWh per cubic meters of oxygen produced (i.e. 0.03 kWh/m 3 n ) which is about 30% and 90% less than those of the equivalent CLAS and cryogenic type process, respectively.
  • recycled CO 2 is used extensively. In the description above, location of the recycled CO 2 stream is shown very generally. Recycled CO 2 (i.e. flue gas) can be recycled from oxy-fuel thermal power plant from various locations.
  • FIG. 9 shows the simplified block diagram of CLAS integration concept with oxy-fuel.
  • flue gas CO 2 —rich
  • they can be termed as (1) hot (2) warm (3) wet and (4) dry recycling.
  • concentration of impurities in flue gas will reduce by moving down from option 1 to 4 but at the same time, inlet flue gas temperature to CLAS reduction reactor will decrease due to heat losses which will increase the operating costs for oxygen production.
  • Hot (1) recycling stream will have temperature ranging from 800-1200° C. while the others (2), (3) and (4) will have a temperature of 380° C. after reheating.
  • the detailed schemes are not shown in the following examples to avoid complexity.
  • mixed metal oxides can also be done according to Ellingham diagram which may fulfill the part of the thermal energy required.
  • iron oxides mixed with manganese oxides may be good for the CLAS process. Iron oxide being lower on the Ellingham diagram is difficult to reduce while easy to oxidize in the oxidation/reduction reactor of the CLAS. Oxidation of iron oxide is an exothermic reaction which will consume part of the oxygen available from the air during oxidation or released from the metal oxides during reduction. Oxidation of iron oxide being an exothermic reaction will generate extra thermal energy which can fulfill the partial requirement of the heating of air and recycled steam/CO 2 .
  • preparation of mixed metal oxides, life cycle, mechanical strength, reaction kinetics and inventory are limiting factors for the use of this novel idea.
  • the CLAS process is integrated with steam generated from an oxy-fuel thermal power plant.
  • the steam generated from the oxy-fuel thermal power plant is directly sent to the reduction reactor for the reduction of the oxidized metal oxides coming from the air reactor.
  • the extra heat needed will be supplied using solar or electric heaters.
  • FIG. 12 shows use of recycled CO 2 at 380° C. instead of steam for the reduction of metal oxide.
  • One of the advantages is that the oxy-fuel technology needs CO 2 to be recycled in the furnace to mainly avoid the high flame temperatures. This recycled CO 2 on its way back to the furnace will help reducing metal oxides for oxygen production.
  • FIG. 13 shows the use of steam as proposed in example 2 with the difference of the use of integrated boiler (IBS) or gasifier (IGS) systems instead of solar/electric heaters for accomplishing the extra thermal energy requirement.
  • IBS integrated boiler
  • IGS gasifier
  • the heat generated by conventional fuels such as coal or NG will suffice the extra thermal energy required for heating up air and steam after the major heat recovery from CLAS outlet streams.
  • IGS/IBS are integrated to cater the extra thermal energy needed after possible heat recovery.
  • This example shown in FIG. 15 is similar to example 3 and recycled CO 2 at 380° C./steam for the reduction of metal oxides in reduction reactor. To avoid complexity, the steam line is not shown in the FIG. 15 .
  • This example will have higher efficiency and lower capital investment as no extra system (Solar/Electric heaters or IGS/IBS) is needed.
  • this option eliminates the recycling of CO 2 at lower temperature (380° C.) instead it recommends the use of crude flue gas at high temperatures (1200° C.) directly for reduction of the metal oxides. It also suggests the use of polishing unit for capturing the sulfur which may degrade the metal oxides. However, the polishing unit requirement and sizing can only be recommended after systematic investigations on the effect of SO x on the metal oxides used as oxygen carriers in the CLAS process. Effect of NO x and moisture also needs to be studied in detail.
  • TSCLAS fixed/fluidized bed temperature swing chemical looping air separation
  • FIG. 18 clearly indicates that TSCLAS with IOFFH integration mode will be parked at the bottom in the costing chart.
  • issues related to fixed beds such as chemical conversion, channeling and maintenance are still to be assessed further.
  • temperature swing may not be suitable due to short reaction times in the reactors as well as heat recovery problems.
  • the CLAS designed with only recycled CO 2 may have limitations in producing the desired product streams (30% O 2 in the recycled flue gas) for oxy-fuel furnace. As shown in FIG. 19 , the cost for producing 16% O 2 in the recycled product gas stream will be nearly as same as the operating cost for CASU (2020). Two final examples are therefore suggested to overcome this limitation.
  • steam is used in the reduction reactor along with CO 2 to dilute the O 2 /CO 2 ratio in the product stream as shown in FIG. 21 .
  • One particularly effective manner of providing the ICLAS unit shown at 5 in FIG. 5 is to utilise a double pipe reactor design for isothermal ICLAS (IICLAS) as shown in FIG. 22 (also shown schematically in FIG. 23, showing various reduced air (RA) streams, distinguished from one another with superscript “x”, “**” and without superscript and recycled flue gas streams (RC), distinguished from one another with superscript “*” and no superscript, and the arrangement of heat exchangers 1-3, designated HE1, HE2 and HE3, respectively.)
  • the oxygen reactor (OR) 15 is an inner pipe within the reduction reactor (RR) 16 as an outer pipe allowing efficient heat transfer as shown at 17 .
  • Air introduced at 18 passes upwardly where it is heated by the combustors 31 to a desired temperature and then passes through the inner pipe oxidation reactor 15 where it oxidises the oxygen carrier particles.
  • the oxidised carrier particles are transported upwardly along path 32 into cyclone 19 where reduced air exits the cyclone at 20 .
  • the oxidised carrier particles are then transferred to the reduction reactor 15 as shown at 33 .
  • Recycled flue gas (RC) introduced at 22 along with added combustion gases from the combustors 31 will reduce the oxidized oxygen carrier particles.
  • the reduced oxygen carrier particles are then transported through conduit 21 through cyclone 34 back to the oxidation reactor 15 .
  • Two combustors 31 are designed to provide the necessary heat to the process and also to maintain uniform temperature throughout the reactor beds.
  • the part of the product stream containing oxygen with CO 2 at 23 is also sent to the combustor 31 for combustion purpose.
  • the horizontal combustor can be divided into different zones as shown at 24 to optimise the energy requirements.
  • the tentative temperature profiles of the oxidation and reduction reactors can be seen in the graph 25 located alongside the schematic drawing of the reactor with corresponding heights in the graph.
  • the bed temperature in the oxidation reactor 15 will increase with height as oxidation is an exothermic process.
  • bed temperature in the reduction reactor 16 will decrease with height, as seen in graph 25 .
  • lower bed height will have lower temperature in opposite to high temperature in the reduction reactor. This will be completely opposite when at higher bed height.
  • the design therefore provides scope for effective heat transfer as shown at 17 between the oxidation and reduction reactors across the full bed height.
  • the isothermal ICLAS reactor design as shown in FIG. 22 is designed to achieve the following important objectives:
  • Constant temperature profiles and oxygen partial pressures in the reactor are expected to improve the overall conversion as well as to increase the oxygen production compared to conventional dual circulating fluidised bed chemical looping systems.
  • the oxygen is supplied by a chemical looping based combustor generally shown by the apparatus within the zone 26 . All other features in the reactor design shown in FIG. 24 are similar to those shown in FIG. 22 .
  • the main difference is in supplying oxygen to the combustors.
  • a chemical looping based combustor is provided as represented by the apparatus shown within zone 26 .
  • the chemical looping based combustor can use a number of oxygen carriers such as oxides of Cu, Mn, Co, Ni, Fe, Illuminite etc. In the particular example shown in FIG. 24 , the use of Ni-oxide is illustrated.
  • the oxidation of Ni is carried out in the combustor oxidation reactor 28 with air.
  • the oxidised nickel i.e. NiO
  • the reduced oxides by CH 4 in the reduction reactor are then transported back to the combustor oxidation reactor 28 using conduit 27 .
  • IICLAS isothermal ICLAS

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