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WO2010125210A1 - Assisted carbon-dioxide-adsorption method - Google Patents

Assisted carbon-dioxide-adsorption method Download PDF

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Publication number
WO2010125210A1
WO2010125210A1 PCT/ES2010/000171 ES2010000171W WO2010125210A1 WO 2010125210 A1 WO2010125210 A1 WO 2010125210A1 ES 2010000171 W ES2010000171 W ES 2010000171W WO 2010125210 A1 WO2010125210 A1 WO 2010125210A1
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nanoparticles
bed
gas
adsorption
fluidization
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Spanish (es)
French (fr)
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José Manuel VALVERDE MILLÁN
Antonio Castellanos Mata
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Universidad de Sevilla
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Universidad de Sevilla
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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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • 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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • B01D53/06—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 by adsorption, e.g. preparative gas chromatography with moving adsorbents, e.g. rotating beds
    • B01D53/10—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 by adsorption, e.g. preparative gas chromatography with moving adsorbents, e.g. rotating beds with dispersed adsorbents
    • B01D53/12—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 by adsorption, e.g. preparative gas chromatography with moving adsorbents, e.g. rotating beds with dispersed adsorbents according to the "fluidised technique"
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/402—Alkaline earth metal or magnesium compounds of magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/602—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/304—Linear dimensions, e.g. particle shape, diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/10—Noble metals or compounds thereof
    • B01D2255/104—Silver
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20753—Nickel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20761—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • 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
    • B01D53/32—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 by electrical effects other than those provided for in group B01D61/00
    • B01D53/323—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 by electrical effects other than those provided for in group B01D61/00 by electrostatic effects or by high-voltage electric fields
    • 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
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • 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
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the present invention aims at a process of adsorption of CO 2 which consists in passing a gas flow with a determined concentration of CO 2 through a bed of powder arranged on a porous plate in a fluidization chamber, the bed comprising at least one powder selected from ultrafine powders comprising primary particles with a typical size between 1 and 100 nm; and simultaneously subjecting the powder bed to an agitation treatment in combination with an electric field to reduce the effect of cohesion between said particles and destabilize the formation of channels and bubbles.
  • the technical invention corresponds to the general area of chemical engineering. In particular, it would have application in gas filtration processes. It is proposed a procedure that can be used to stimulate the adsorption of CO 2 by means of the assisted fluidization of metal oxide nanoparticles.
  • MO + CO 2 ⁇ MCO 3 This reaction is reversible at high temperatures (calcination), so that these metal oxides are regenerable.
  • metal oxides that have a high adsorption capacity of CO 2 according to the reaction described, among which are CaO, ZnO, MgO, MnO2, NiO, CuO, PbO, Ag 2 O, etc. (Colombo 1973).
  • the adsorption capacity of these metal oxides is very high.
  • Ia of CaO can be 700 g of CO 2 per kg of CaO, which is about an order of magnitude greater than the adsorption capacity of other conventional general purpose filters such as activated carbon filters (Fan and Gupta 2006).
  • metal oxides for the adsorption of CO 2 represents a considerable technological advantage. Since the adsorption process takes place at the surface level, a fundamental parameter that regulates the effectiveness in the practice of the CO 2 adsorption process is the specific area of contact between the gas and the metal oxide in the solid state. Certain adsorbent metal oxides that are obtained from natural precursors are characterized by having a very large amount of micropores (pores smaller than 2 nanometers). However, these micropores are very susceptible to being clogged, thus limiting the effectiveness of the adsorption process.
  • Fan and Gupta describe the fabrication of 3 mesosporous CaCO structures (pore size between 5 and 20 nanometers), which can be regenerated by calcination, giving rise to a CaO adsorbent structure with a considerable specific surface area of 22 m 2 / g (Fan and Gupta 2006).
  • the system is usually heterogeneous (Valverde and Castellanos 2007) due to the great adhesion force of the nanoparticles compared to their weight.
  • the nanoparticle aggregates are practically impervious to gas flow and can have sizes of the order of the millimeter (Jenneson and Gundogdu 2006).
  • the marked aggregation of the nanoparticles favors the formation of very stable channels and bubbles through which the gas preferably flows instead of homogeneously mixing with the solid phase.
  • the surface area of effective contact between the metal oxide nanoparticles and the nanofluidization gas is considerably less than expected.
  • the fluidization of nanoparticles of metal oxides oriented to the adsorption of CO 2 must be carried out primarily with gas previously moistened in order to increase the adsorption capacity of CO 2 by the metal oxide.
  • the condensation of water vapor on the surface of the particles results in the formation of liquid bridges between the particles, which further increases the cohesion of the material and consequently produces a greater aggregation and stabilization of gas channels and bubbles that prevent a optimal contact between the gas and the surface of the nanoparticles. It is therefore necessary to apply a new procedure aimed at the destruction of such aggregates and destabilization of gas channels and bubbles that favor contact between the surface of the nanoparticles and the gas in order to increase the specific surface area effective of the bed of nanoparticles .
  • the object of the present invention is to stimulate the adsorption of CO 2 by nanoparticles of metal oxides in a fluid bed. This procedure applies to the reduction of CO2 emissions resulting from the combustion of fossil fuels.
  • the nanoparticles theoretically offer a relevant adsorption capacity, the surface area of effective contact with the gas in the fluid bed is reduced due to the formation of agglomerates of nanoparticles that are practically impervious to gas flow, as well as to the formation of channels and gas bubbles.
  • the proposed procedure is aimed at homogenizing the fluidization process by means of the combined application of mechanical agitation and an electric field.
  • the process object of the present invention consists in assisting the fluidization with previously humidified gas, and containing a determined amount of CO 2 , of a bed of metal oxide nanoparticles. Said fluidization is assisted by a mechanical method such as the application of vibrations, in combination with the application of an electrostatic field that favors Ia chain formation and destabilize the formation of gas channels and bubbles. This procedure is oriented to increase the contact surface between the solid and gaseous phases and therefore the effectiveness of the adsorption of CO 2
  • the present invention consists in passing a gas flow with a determined concentration of CO 2 through a bed of powder disposed on a porous plate in a fluidization chamber, the bed of powder comprising at least one powder selected from ultrafine powders which they comprise primary particles with a typical size between 1 and 100 nm (nanoparticles); and simultaneously subjecting the powder bed to a stirring treatment to reduce the effect of cohesion between said particles characterized in that the stirring treatment comprises applying at least one vibration on said bed in combination with the application of an electric field by external means.
  • the main characteristic of the primary particles to be used in this procedure is that they are composed of metal oxides such as, for example, CaO, ZnO, MgO, MnO2, NiO, CuO, PbO, Ag 2 O, etc., which have a proven adsorption capacity of CO 2 .
  • the gas with a determined amount of CO 2 is previously humidified in order to increase the adsorption capacity of CO 2 by the surface of the nanoparticles.
  • Figure 1 General scheme of an installation for the adsorption of CO 2 by metal oxide nanoparticles based on a fluidization procedure assisted by the combination of the application of a method of agitation of the bed of nanoparticles with an application of a field electric.
  • Solid plate of porous material that distributes the gas flow to the bed of nanoparticles.
  • Electrodes 9. Electric field acting on the bed of nanoparticles
  • a possible embodiment of the present invention is schematized in Figure 1.
  • the flow of compressed gas, with a determined concentration of CO 2 is controlled by a mass flow controller.
  • This controlled gas flow is humidified using a humidifier.
  • CO 2 and relative humidity analyzers This controlled gas flow is distributed through the bed of nanoparticles located in the cell or fluidization chamber.
  • a solid porous plate is fitted that distributes the gas to the bed of nanoparticles that rests on it.
  • a vibrator By means of a vibrator the bed of nanoparticles is strongly agitated.
  • an external source of electric field and two parallel electrodes placed vertically By means of an external source of electric field and two parallel electrodes placed vertically, the bed of nanoparticles is subjected to an electric field.
  • CO 2 and relative humidity analyzers measure these parameters in order to evaluate the amount of CO 2 adsorbed during the process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The subject matter of the present invention is a CO2-adsorption method that consists in passing a stream of gas with a specific CO2 concentration through a powder bed arranged on a porous plate in a fluidization chamber, the powder bed comprising at least one powder selected from ultrafine powders that comprise primary particles with a typical size of between 1 and 100 nm, and simultaneously subjecting the powder bed to an agitation treatment in combination with an electric field in order to reduce the effect of cohesion between said particles and to destabilize the formation of channels and bubbles. The technical invention relates to the general area of chemical engineering. In particular, the invention would be used in gas-filtration processes. A method is proposed that may be used to stimulate CO2 adsorption by means of the assisted fluidization of metal oxide nanoparticles.

Description

TÍTULO TITLE

Procedimiento asistido de adsorción de dióxido de carbonoAssisted carbon dioxide adsorption procedure

OBJETO DE LA INVENCIÓNOBJECT OF THE INVENTION

La presente invención tiene por objeto un procedimiento de adsorción de CO2 que consiste en hacer pasar un flujo de gas con una concentración determinada de CO2 a través de un lecho de polvo dispuesto sobre una placa porosa en una cámara de fluidización, comprendiendo el lecho de polvo al menos un polvo seleccionado entre polvos ultrafinos que comprenden partículas primarias con un tamaño típico entre 1 y 100 nm; y simultáneamente someter el lecho de polvo a un tratamiento de agitación en combinación con una campo eléctrico para reducir el efecto de Ia cohesión entre dichas partículas y desestabilizar Ia formación de canales y burbujas.The present invention aims at a process of adsorption of CO 2 which consists in passing a gas flow with a determined concentration of CO 2 through a bed of powder arranged on a porous plate in a fluidization chamber, the bed comprising at least one powder selected from ultrafine powders comprising primary particles with a typical size between 1 and 100 nm; and simultaneously subjecting the powder bed to an agitation treatment in combination with an electric field to reduce the effect of cohesion between said particles and destabilize the formation of channels and bubbles.

La invención técnica corresponde al área general de Ia ingeniería química. En particular, tendría aplicación en procesos de filtración de gases. Se propone un procedimiento que puede ser empleado para estimular Ia adsorción de CO2 mediante Ia fluidización asistida de nanopartículas de óxidos metálicos.The technical invention corresponds to the general area of chemical engineering. In particular, it would have application in gas filtration processes. It is proposed a procedure that can be used to stimulate the adsorption of CO 2 by means of the assisted fluidization of metal oxide nanoparticles.

ESTADO DE LA TÉCNICASTATE OF THE TECHNIQUE

En los últimos años Ia concentración de gases de efecto invernadero en Ia atmósfera ha presentado un considerable incremento, Io cual contribuye, según expertos sobre el cambio climático, al calentamiento global de nuestro planeta de manera significativa y prácticamente irreversible (Friedlingstein y Solomon 2005). El dióxido de carbono (CO2) es el gas más importante de efecto invernadero, cuyo incremento en Ia atmósfera es debido principalmente al creciente uso de combustibles fósiles (Halman y Steinberg 1999). Aunque una solución definitiva a este grave problema se encuentra en Ia potenciación del uso de fuentes de energía renovables y no emisoras de CO2, el desarrollo de nuevas tecnologías orientadas a Ia reducción de emisiones de este gas de efecto invernadero es actualmente una actividad altamente prioritaria. Por tanto, cualquier aportación que pueda suponer una optimización de los procesos de eliminación de emisiones de gases de efecto invernadero puede suponer un relevante avance tecnológico.In recent years the concentration of greenhouse gases in the atmosphere has presented a considerable increase, which contributes, according to experts on climate change, to the global warming of our planet in a significant and almost irreversible way (Friedlingstein and Solomon 2005). Carbon dioxide (CO 2 ) is the most important greenhouse gas, whose increase in the atmosphere is mainly due to the increasing use of fossil fuels (Halman and Steinberg 1999). Although a definitive solution to this serious problem is the synergistic use of renewable energy sources and do not emit CO2, the development of new technologies aimed at the reduction of emissions of this greenhouse gas is currently a high priority activity . Therefore, any contribution that may involve an optimization of the elimination processes of Greenhouse gas emissions can be a significant technological advance.

Entre las técnicas que en Ia actualidad se emplean al objeto de reducir Ia emisión de CO2 a Ia atmósfera (Halman y Steinberg 1999) encontramos Ia adsorción de CO2 por Ia superficie de óxidos metálicos (Colombo 1973, Fan y Gupta 2006). Los óxidos de ciertos metales (representados por MO) reaccionan con el CO2 para formar carbonatos metálicos (MCO3) de acuerdo con Ia reacción:Among the techniques currently used in order to reduce the emission of CO 2 into the atmosphere (Halman and Steinberg 1999) we find the adsorption of CO 2 by the surface of metal oxides (Colombo 1973, Fan and Gupta 2006). The oxides of certain metals (represented by MO) react with CO 2 to form metal carbonates (MCO 3 ) according to the reaction:

MO+CO2→MCO3 Esta reacción es reversible a altas temperaturas (calcinación), de manera que estos óxidos metálicos son regenerables. Existen numerosos óxidos metálicos que presentan gran capacidad de adsorción de CO2 según Ia reacción descrita, entre los que se encuentran el CaO, ZnO, MgO, MnO2, NiO, CuO, PbO, Ag2O, etc. (Colombo 1973). La capacidad de adsorción de estos óxidos metálicos es muy elevada. Por ejemplo, Ia del CaO puede llegar a ser de 700 g de CO2 por kg de CaO, que es alrededor de un orden de magnitud superior a Ia capacidad de adsorción de otros filtros convencionales de uso general como los filtros de carbón activado (Fan y Gupta 2006). Por tanto, el uso de óxidos metálicos para Ia adsorción de CO2 representa una ventaja tecnológica considerable. Puesto que el proceso de adsorción tiene lugar a nivel superficial, un parámetro fundamental que regula Ia efectividad en Ia práctica del proceso de adsorción de CO2 es el área específica de contacto entre el gas y el óxido metálico en estado sólido. Ciertos óxidos metálicos adsorbentes que se obtienen a partir de precursores naturales se caracterizan por poseer una cantidad muy grande de microporos (poros menores de 2 nanómetros). No obstante, estos microporos son muy susceptibles a ser obstruidos, limitando así Ia eficacia del proceso de adsorción. Fan y Gupta describen Ia fabricación de estructuras de CaCO3 meso- porosas (tamaño de poro entre 5 y 20 nanómetros), que pueden ser regeneradas mediante calcinación, dando lugar a una estructura adsorbente de CaO con un área superficial específica considerable de 22 m2/g (Fan y Gupta 2006).MO + CO 2 → MCO 3 This reaction is reversible at high temperatures (calcination), so that these metal oxides are regenerable. There are numerous metal oxides that have a high adsorption capacity of CO 2 according to the reaction described, among which are CaO, ZnO, MgO, MnO2, NiO, CuO, PbO, Ag 2 O, etc. (Colombo 1973). The adsorption capacity of these metal oxides is very high. For example, Ia of CaO can be 700 g of CO 2 per kg of CaO, which is about an order of magnitude greater than the adsorption capacity of other conventional general purpose filters such as activated carbon filters (Fan and Gupta 2006). Therefore, the use of metal oxides for the adsorption of CO 2 represents a considerable technological advantage. Since the adsorption process takes place at the surface level, a fundamental parameter that regulates the effectiveness in the practice of the CO 2 adsorption process is the specific area of contact between the gas and the metal oxide in the solid state. Certain adsorbent metal oxides that are obtained from natural precursors are characterized by having a very large amount of micropores (pores smaller than 2 nanometers). However, these micropores are very susceptible to being clogged, thus limiting the effectiveness of the adsorption process. Fan and Gupta describe the fabrication of 3 mesosporous CaCO structures (pore size between 5 and 20 nanometers), which can be regenerated by calcination, giving rise to a CaO adsorbent structure with a considerable specific surface area of 22 m 2 / g (Fan and Gupta 2006).

Por otra parte, el desarrollo en los últimos años de técnicas de producción masiva de nanopartículas ha hecho posible el uso de éstas en aplicaciones de filtrado que se ven enormemente favorecidas por el gran área superficial específica de contacto que proporcionan, del orden de 100 m2/g (Espin et al. 2004). Una aplicación de especial relevancia para Ia presente invención es Ia adsorción estimulada de CO2 por nanopartículas de óxidos metálicos (Espin et al. 2004, Bakardjieva et al. 2004, Lu et al. 2005). Hay que tener en cuenta que Ia mayor reactividad de estas nanopartículas no es únicamente debida al su gran área superficial específica, si no también en gran medida a las particularidades morfológicas y defectos de su superficie (Klabunde et al. 1996, Stark et al. 1996). Por ello, el uso de nanopartículas adsorbentes de CO2 representa una ventaja añadida.On the other hand, the development in recent years of nanoparticle mass production techniques has made it possible to use them in filtering applications that are greatly favored by the large specific surface area of contact they provide, of the order of 100 m 2 / g (Espin et al. 2004). An application of special relevance for the present invention is the stimulated adsorption of CO 2 by metal oxide nanoparticles (Espin et al. 2004, Bakardjieva et al. 2004, Lu et al. 2005). It should be taken into account that the greater reactivity of these nanoparticles is not only due to their large specific surface area, but also to a large extent due to morphological particularities and surface defects (Klabunde et al. 1996, Stark et al. 1996 ). Therefore, the use of CO 2 adsorbent nanoparticles represents an added advantage.

No obstante, al hacer pasar el gas a través de un lecho de nanopartículas (nanofluidización) el sistema es usualmente heterogéneo (Valverde y Castellanos 2007) debido a Ia gran fuerza de adhesión de las nanopartículas en comparación con su peso. Esto hace que las nanopartículas se agreguen con gran facilidad. Los agregados de nanopartículas son prácticamente impermeables al flujo de gas y pueden llegar a tener tamaños del orden del milímetro (Jenneson and Gundogdu 2006). Adicionalmente, Ia marcada agregación de las nanopartículas favorece Ia formación de canales muy estables y burbujas a través de los cuales el gas fluye preferentemente en lugar de mezclarse homogéneamente con Ia fase sólida. Así, el área superficial de contacto efectiva entre las nanopartículas de óxido metálico y el gas en nanofluidización es considerablemente menor de Io esperado. En concreto, estos efectos han sido mostrados recientemente por Jenneson and Gundogdu (Jenneson and Gundogdu 2006) mediante visualización in-situ de un lecho fluidizado de nanopartículas de un óxidos metálico (ZnO) usando tomografía de Rayos X. Por tanto, en el proceso de fluidización convencional de nanopartículas no se llega a conseguir una óptima mezcla entre las fases gaseosa y sólida, Io cual compromete seriamente Ia efectividad de Ia adsorción de CO2 en Ia superficie de las nanopartículas a pesar de su potencialmente elevada reactividad.However, by passing the gas through a bed of nanoparticles (nanofluidization) the system is usually heterogeneous (Valverde and Castellanos 2007) due to the great adhesion force of the nanoparticles compared to their weight. This makes the nanoparticles aggregate with great ease. The nanoparticle aggregates are practically impervious to gas flow and can have sizes of the order of the millimeter (Jenneson and Gundogdu 2006). Additionally, the marked aggregation of the nanoparticles favors the formation of very stable channels and bubbles through which the gas preferably flows instead of homogeneously mixing with the solid phase. Thus, the surface area of effective contact between the metal oxide nanoparticles and the nanofluidization gas is considerably less than expected. Specifically, these effects have been recently shown by Jenneson and Gundogdu (Jenneson and Gundogdu 2006) by in-situ visualization of a fluidized bed of nanoparticles of a metal oxides (ZnO) using X-ray tomography. Therefore, in the process of Conventional fluidization of nanoparticles does not achieve an optimal mixture between the gas and solid phases, which seriously compromises the effectiveness of the adsorption of CO 2 on the surface of the nanoparticles despite their potentially high reactivity.

Recientemente se han investigado métodos dirigidos a homogenizar Ia nanofluidización que tienen como objetivo lograr una mayor superficie de contacto efectiva de las nanopartículas con Ia fase gaseosa. Los métodos que han sido empleados con éxito son hasta el momento Ia aplicación de vibraciones al lecho fluido, aplicación de pulsos acústicos, centrifugación, aplicación de un campo magnético externo variable que agita bolas magnéticas emplazadas en el interior del lecho de nanopartículas (Pfeffer et al, 2005) y aplicación de un campo eléctrico oscilantes (Espin et al. 2009). Estas técnicas provocan una agitación intensa de los agregados de nanopartículas, ya sea mediante una fuerza mecánica (Pfeffer et al, 2005) o a través de una fuerza eléctrica oscilante (Espin et al. 2009). Principalmente se ha demostrado que dichas técnicas son eficaces en Ia mejora de Ia fluidización de nanopartículas de SiO2 con gases secos. Al disminuir Ia heterogeneidad de Ia fluidización se favorece un mayor contacto sólido-gas, Io cual debe contribuir a incrementar Ia efectividad de cualquier reacción que se produzca en base a dicho contacto. No obstante, aún no se ha explorado Ia aplicación directa de estos métodos a Ia fluidización de nanopartículas de óxidos metálicos, que es altamente heterogénea (Jenneson and Gundogdu 2006), ni se ha probado su efecto sobre Ia adsorción asistida de CO2 mediante nanofluidización.Recently, methods aimed at homogenizing the nanofluidization have been investigated which aim to achieve a greater effective contact surface of the nanoparticles with the gas phase. The methods that have been used successfully are so far the application of vibrations to the fluid bed, application of acoustic pulses, centrifugation, application of a variable external magnetic field that agitates magnetic balls located inside the bed of nanoparticles (Pfeffer et al. , 2005) and application of a oscillating electric field (Espin et al. 2009). These techniques cause intense agitation of nanoparticle aggregates, either by a mechanical force (Pfeffer et al, 2005) or by an oscillating electric force (Espin et al. 2009). Mainly it has been shown that said techniques are effective in improving the fluidization of SiO 2 nanoparticles with dry gases. By decreasing the heterogeneity of the fluidization, a greater solid-gas contact is favored, which should contribute to increasing the effectiveness of any reaction that occurs based on said contact. However, the direct application of these methods to the fluidization of metal oxide nanoparticles, which is highly heterogeneous (Jenneson and Gundogdu 2006), has not yet been explored, nor has its effect on the assisted adsorption of CO 2 by nanofluidization been tested.

Es importante resaltar que trabajos previos han mostrado que Ia capacidad de adsorción de CO2 por un óxido metálico se ve notablemente incrementada en un ambiente de alta humedad relativa (Colombo y Mills 1966). Por ello sería deseable que las nanopartículas tengan una naturaleza hidrófila y, además, el gas sea previamente humedecido. Es de esperar entonces que Ia condensación del vapor de agua en Ia superficie de las nanopartículas de lugar Ia formación de puentes líquidos entre ellas (Schubert 1984). Ello provocaría un notable incremento de Ia fuerza de cohesión entre aglomerados de partículas que induciría una mayor agregación y que por tanto perjudicaría, aún en mayor medida, Ia efectividad del proceso de fluidización sobre Ia adsorción de CO2 en presencia de vapor de agua. Existe, sin embargo, un método mediante el cual se logra homogeneizar Ia fluidización de granos gruesos no cohesivos (tamaño mayor de 100 mieras) e hidrófilos con gas humedecido consistente en Ia aplicación de un campo eléctrico estático (Johnson y Melcher 1975). La polarización eléctrica inducida por un campo eléctrico estático sobre los granos húmedos provoca Ia formación de cadenas. Estas cadenas contribuyen igualmente a desestabilizar Ia formación de canales y burbujas. La aplicación directa de esta técnica a Ia fluidización de nanopartículas hidrófitas altamente cohesivas con gases humedecidos no tiene una efectividad probada.It is important to highlight that previous works have shown that the adsorption capacity of CO 2 by a metal oxide is significantly increased in an environment of high relative humidity (Colombo and Mills 1966). Therefore, it would be desirable for the nanoparticles to have a hydrophilic nature and, in addition, the gas to be previously moistened. It is to be expected that the condensation of water vapor on the surface of the nanoparticles will place the formation of liquid bridges between them (Schubert 1984). This would cause a notable increase in the cohesion force between particle agglomerates that would induce greater aggregation and that would therefore, to a greater extent, impair the effectiveness of the fluidization process on the adsorption of CO 2 in the presence of water vapor. There is, however, a method by which it is possible to homogenize the fluidization of non-cohesive coarse grains (size greater than 100 microns) and hydrophilic with moistened gas consisting of the application of a static electric field (Johnson and Melcher 1975). The electrical polarization induced by a static electric field on the wet grains causes the formation of chains. These chains also contribute to destabilizing the formation of channels and bubbles. The direct application of this technique to the fluidization of highly cohesive hydrophilic nanoparticles with moistened gases does not have proven effectiveness.

Es necesaria Ia aplicación de nuevos procedimientos que den lugar a Ia homogeneización de Ia fluidización de nanopartículas de óxidos metálicos en presencia de humedad. Estos procedimientos tendrían como consecuencia un incremento del área de Ia superficie efectiva de contacto entre el óxido metálico y el CO2 y por tanto una optimización del proceso de adsorción de CO2.It is necessary to apply new procedures that give rise to the homogenization of the fluidization of nanoparticles of metal oxides in the presence of moisture. These procedures would result in a increase in the area of the effective contact surface between the metal oxide and the CO 2 and therefore an optimization of the CO 2 adsorption process.

DESCRIPCIÓN DE LA INVENCIÓNDESCRIPTION OF THE INVENTION

La fluidización de nanopartículas de óxidos metálicos orientada a Ia adsorción de CO2 ha de realizarse primordialmente con gas previamente humedecido con el objetivo de incrementar Ia capacidad de adsorción de CO2 por parte del óxido metálico. La condensación del vapor de agua sobre Ia superficie de las partículas da lugar a Ia formación de puentes líquidos entre las partículas, Io cual incrementa aún más Ia cohesión del material y consecuentemente produce una mayor agregación y estabilización de canales y burbujas de gas que impiden una contacto óptimo entre el gas y Ia superficie de las nanopartículas. Es pues necesaria Ia aplicación de un nuevo procedimiento dirigido a Ia destrucción de tales agregados y desestabilización de canales y burbujas de gas que favorezca el contacto entre Ia superficie de las nanopartículas y el gas al objeto de incrementar el área superficial específica efectiva del lecho de nanopartículas.The fluidization of nanoparticles of metal oxides oriented to the adsorption of CO 2 must be carried out primarily with gas previously moistened in order to increase the adsorption capacity of CO 2 by the metal oxide. The condensation of water vapor on the surface of the particles results in the formation of liquid bridges between the particles, which further increases the cohesion of the material and consequently produces a greater aggregation and stabilization of gas channels and bubbles that prevent a optimal contact between the gas and the surface of the nanoparticles. It is therefore necessary to apply a new procedure aimed at the destruction of such aggregates and destabilization of gas channels and bubbles that favor contact between the surface of the nanoparticles and the gas in order to increase the specific surface area effective of the bed of nanoparticles .

El objeto de Ia presente invención es estimular Ia adsorción de CO2 por nanopartículas de óxidos metálicos en un lecho fluido. Este procedimiento es aplicable a Ia reducción de emisiones de CO2 derivada de Ia combustión de combustibles fósiles. Si bien las nanopartículas ofrecen en teoría una relevante capacidad de adsorción, el área superficial de contacto efectiva con el gas en el lecho fluido es reducida debido a Ia formación de aglomerados de nanopartículas que son prácticamente impermeables al flujo de gas, así como a Ia formación de canales y burbujas de gas. El procedimiento propuesto está dirigido a homogeneizar el proceso de fluidización mediante Ia aplicación combinada de agitación mecánica y un campo eléctrico. De esta manera se prevé incrementar el área de contacto efectiva entre las fases gaseosa y sólida en el lecho fluido, Io cual redundará en una mayor capacidad de adsorción de CO2. El procedimiento objeto de Ia presente invención consiste en asistir Ia fluidización con gas previamente humidificado, y que contiene una cantidad determinada de CO2, de un lecho de nanopartículas de óxido metálico. Dicha fluidización es asistida por un método mecánico como por ejemplo Ia aplicación de vibraciones, en combinación con Ia aplicación de un campo electrostático que favorezca Ia formación de cadenas y desestabilice Ia formación de canales y burbujas de gas. Este procedimiento está orientado a incrementar Ia superficie de contacto entre las fases sólida y gaseosa y por tanto Ia efectividad de Ia adsorción de CO2 The object of the present invention is to stimulate the adsorption of CO 2 by nanoparticles of metal oxides in a fluid bed. This procedure applies to the reduction of CO2 emissions resulting from the combustion of fossil fuels. Although the nanoparticles theoretically offer a relevant adsorption capacity, the surface area of effective contact with the gas in the fluid bed is reduced due to the formation of agglomerates of nanoparticles that are practically impervious to gas flow, as well as to the formation of channels and gas bubbles. The proposed procedure is aimed at homogenizing the fluidization process by means of the combined application of mechanical agitation and an electric field. In this way, it is expected to increase the effective contact area between the gaseous and solid phases in the fluid bed, which will result in a greater adsorption capacity of CO 2 . The process object of the present invention consists in assisting the fluidization with previously humidified gas, and containing a determined amount of CO 2 , of a bed of metal oxide nanoparticles. Said fluidization is assisted by a mechanical method such as the application of vibrations, in combination with the application of an electrostatic field that favors Ia chain formation and destabilize the formation of gas channels and bubbles. This procedure is oriented to increase the contact surface between the solid and gaseous phases and therefore the effectiveness of the adsorption of CO 2

La presente invención consiste en hacer pasar un flujo de gas con una concentración determinada de CO2 a través de un lecho de polvo dispuesto sobre una placa porosa en una cámara de fluidización, comprendiendo el lecho de polvo al menos un polvo seleccionado entre polvos ultrafinos que comprenden partículas primarias con un tamaño típico entre 1 y 100 nm (nanopartículas); y simultáneamente someter el lecho de polvo a un tratamiento de agitación para reducir el efecto de Ia cohesión entre dichas partículas caracterizado porque el tratamiento de agitación comprende aplicar sobre dicho lecho al menos vibración en combinación con Ia aplicación de un campo eléctrico por medios externos. La principal característica de las partículas primarias a usar en este procedimiento es que se encuentren estén compuestas por óxidos metálicos como, por ejemplo, CaO, ZnO, MgO, MnO2, NiO, CuO, PbO, Ag2O, etc., que poseen una probada capacidad de adsorción de CO2. En este procedimiento el gas con una cantidad determinada de CO2 es previamente humidificado al objeto de incrementar Ia capacidad de adsorción de CO2 por parte de Ia superficie de las nanopartículas.The present invention consists in passing a gas flow with a determined concentration of CO 2 through a bed of powder disposed on a porous plate in a fluidization chamber, the bed of powder comprising at least one powder selected from ultrafine powders which they comprise primary particles with a typical size between 1 and 100 nm (nanoparticles); and simultaneously subjecting the powder bed to a stirring treatment to reduce the effect of cohesion between said particles characterized in that the stirring treatment comprises applying at least one vibration on said bed in combination with the application of an electric field by external means. The main characteristic of the primary particles to be used in this procedure is that they are composed of metal oxides such as, for example, CaO, ZnO, MgO, MnO2, NiO, CuO, PbO, Ag 2 O, etc., which have a proven adsorption capacity of CO 2 . In this process the gas with a determined amount of CO 2 is previously humidified in order to increase the adsorption capacity of CO 2 by the surface of the nanoparticles.

DESCRIPCIÓN DE LAS FIGURASDESCRIPTION OF THE FIGURES

Figura 1.- Esquema general de una instalación para Ia adsorción de CO2 por nanopartículas de óxidos metálicas en base a un procedimiento de fluidización asistida por Ia combinación de Ia aplicación de un método de agitación del lecho de nanopartículas con un Ia aplicación de un campo eléctrico.Figure 1.- General scheme of an installation for the adsorption of CO 2 by metal oxide nanoparticles based on a fluidization procedure assisted by the combination of the application of a method of agitation of the bed of nanoparticles with an application of a field electric.

1. Fuente de gas comprimido con una concentración indeterminada de CO2 1. Source of compressed gas with an undetermined concentration of CO 2

2. Controlador del flujo de gas2. Gas flow controller

3. Humidificador 4. Flujo de gas controlado3. Humidifier 4. Controlled gas flow

5. Placa sólida de material poroso que distribuye el flujo de gas hacia el lecho de nanopartículas.5. Solid plate of porous material that distributes the gas flow to the bed of nanoparticles.

6. Lecho de nanopartículas adsorbentes de CO2 6. Bed of CO 2 adsorbent nanoparticles

7. Fuente de generación de un campo eléctrico 8. Electrodos 9. Campo eléctrico que actúa sobre el lecho de nanopartículas7. Source of generation of an electric field 8. Electrodes 9. Electric field acting on the bed of nanoparticles

10. Celda o cámara de fluidización en Ia que se aloja el lecho de nanopartículas10. Cell or fluidization chamber in which the bed of nanoparticles is housed

11. Dispositivo generador de vibraciones11. Vibration generating device

12. Analizadores de CO2 13. Analizadores de humedad12. CO 2 analyzers 13. Moisture analyzers

MODO DE REALIZACIÓN DE LA INVENCIÓNEMBODIMENT OF THE INVENTION

Una posible realización de Ia presente invención se encuentra esquematizada en Ia figura 1. El flujo de gas comprimido, con una concentración determinada de CO2, es controlado mediante un controlador de flujo másico. Este flujo de gas controlado es humidificado usando un humidificador.A possible embodiment of the present invention is schematized in Figure 1. The flow of compressed gas, with a determined concentration of CO 2 , is controlled by a mass flow controller. This controlled gas flow is humidified using a humidifier.

Posteriormente, se analiza su concentración de CO2 y humedad relativa mediante analizadores de CO2 y humedad relativa. Este flujo de gas controlado es distribuido a través del lecho de nanopartículas emplazado en Ia celda o cámara de fluidización. En Ia base de Ia celda de fluidización se ajusta un una placa porosa sólida que distribuye el gas al lecho de nanopartículas que reposa sobre ésta. Por medio de un vibrador el lecho de nanopartículas es fuertemente agitado. Mediante una fuente externa de campo eléctrico y dos electrodos paralelos emplazados verticalmente, el lecho de nanopartículas es sometido a un campo eléctrico. A Ia salida del gas, analizadores de CO2 y de humedad relativa miden estos parámetros al objeto de evaluar Ia cantidad de CO2 adsorbido durante el proceso. Subsequently, its concentration of CO 2 and relative humidity is analyzed using CO 2 and relative humidity analyzers. This controlled gas flow is distributed through the bed of nanoparticles located in the cell or fluidization chamber. At the base of the fluidization cell, a solid porous plate is fitted that distributes the gas to the bed of nanoparticles that rests on it. By means of a vibrator the bed of nanoparticles is strongly agitated. By means of an external source of electric field and two parallel electrodes placed vertically, the bed of nanoparticles is subjected to an electric field. At the exit of the gas, CO 2 and relative humidity analyzers measure these parameters in order to evaluate the amount of CO 2 adsorbed during the process.

Claims

REIVINDICACIONES 1. Procedimiento asistido de adsorción de CO2 caracterizado porque consiste en hacer pasar un flujo de gas con una concentración determinada de CO2 a través de un lecho de polvo dispuesto sobre una placa porosa en una cámara de fluidización, comprendiendo el lecho de polvo al menos un polvo seleccionado entre polvos ultrafinos que comprenden partículas primarias con un tamaño típico entre 1 y 100 nm; y, simultáneamente someter el lecho de polvo a un tratamiento de agitación en combinación con una campo eléctrico para reducir el efecto de Ia cohesión entre dichas partículas y desestabilizar Ia formación de canales y burbujas.1. Assisted process of adsorption of CO 2 characterized in that it consists in passing a gas flow with a determined concentration of CO 2 through a bed of powder arranged on a porous plate in a fluidization chamber, the bed of dust comprising the less a powder selected from ultrafine powders comprising primary particles with a typical size between 1 and 100 nm; and, simultaneously subjecting the powder bed to a stirring treatment in combination with an electric field to reduce the effect of cohesion between said particles and destabilize the formation of channels and bubbles. 2. Procedimiento según Ia reivindicación 1 , caracterizado porque las partículas primarias están formadas por óxidos metálicos.2. Method according to claim 1, characterized in that the primary particles are formed by metal oxides. 3. Procedimiento según Ia reivindicación 1 , caracterizado porque el flujo de gas es previamente humidificado con agua.3. Method according to claim 1, characterized in that the gas flow is previously humidified with water. 4. Procedimiento según Ia reivindicación 1 , caracterizado porque el tratamiento de agitación comprende aplicar sobre el lecho de polvo al menos vibración.4. Method according to claim 1, characterized in that the stirring treatment comprises applying at least one vibration on the powder bed. 5. Procedimiento según Ia reivindicación 1 , caracterizado porque el campo eléctrico aplicado es estático, pulsado y/o alterno. 5. Method according to claim 1, characterized in that the applied electric field is static, pulsed and / or alternate.
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