WO2012034921A1 - Procédé pour la séparation et la capture de co2 à partir de mélanges de gaz utilisant des solutions d'amines dans des alcools anhydres - Google Patents

Procédé pour la séparation et la capture de co2 à partir de mélanges de gaz utilisant des solutions d'amines dans des alcools anhydres Download PDF

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WO2012034921A1
WO2012034921A1 PCT/EP2011/065531 EP2011065531W WO2012034921A1 WO 2012034921 A1 WO2012034921 A1 WO 2012034921A1 EP 2011065531 W EP2011065531 W EP 2011065531W WO 2012034921 A1 WO2012034921 A1 WO 2012034921A1
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solution
amine
process according
absorption
desorption
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Maurizio Peruzzini
Fabrizio Mani
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Consiglio Nazionale Delle Ricerche
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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
    • B01D53/14—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 absorption
    • B01D53/1456—Removing acid components
    • B01D53/1475—Removing 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
    • B01D53/14—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 absorption
    • B01D53/1493—Selection of liquid materials for use as absorbents
    • 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
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/202—Alcohols or their derivatives
    • B01D2252/2021—Methanol
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/202—Alcohols or their derivatives
    • B01D2252/2023—Glycols, diols or their derivatives
    • B01D2252/2025—Ethers or esters of alkylene glycols, e.g. ethylene or propylene carbonate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/202—Alcohols or their derivatives
    • B01D2252/2023—Glycols, diols or their derivatives
    • B01D2252/2026—Polyethylene glycol, ethers or esters thereof, e.g. Selexol
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/204—Amines
    • B01D2252/20478—Alkanolamines
    • B01D2252/20484—Alkanolamines with one hydroxyl group
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/204—Amines
    • B01D2252/20478—Alkanolamines
    • B01D2252/20489—Alkanolamines with two or more hydroxyl groups
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/40—Absorbents explicitly excluding the presence of water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/16—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/22—Carbon dioxide
    • 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
    • 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
    • B01D2258/00—Sources of waste gases
    • B01D2258/05—Biogas
    • 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 relates to a process for the separation and capture of carbon dioxide (C0 2 ) from gaseous mixtures containing several different gases.
  • These gaseous mixtures may be produced by a number of industrial processes, such as, but not exclusively, hydrogen, steel and cement production, combustion of fossil fuels in power plants, as well as plants for waste-to-energy conversion and biomasses combustion.
  • the process according to the invention is particularly suitable for the separation of C0 2 from CH 4 in the production of the so called “natural gas”, and for the separation of C0 2 from H 2 in "steam reforming" and "coal gasification” processes, in which H 2 is obtained from methane, carbon or biomass treatment. I n all these processes, C0 2 is an inevitable waste product that must be separated from H 2 before its possible utilization.
  • C0 2 emitted represents the overall amount of C0 2 released in the atmosphere to produce all energy -electrical, mechanical and thermal- necessary to support the entire process, from the manufacture of the reagents to the C0 2 disposal).
  • C0 2 emitted represents the overall amount of C0 2 released in the atmosphere to produce all energy -electrical, mechanical and thermal- necessary to support the entire process, from the manufacture of the reagents to the C0 2 disposal).
  • 0.3 metric tons of extra C0 2 are emitted (A. Hachiya and S. Frimpong, Environmental Issues and Management of Waste, in Energy and Mineral Production; K.R. Singhal and A.K. Mehrotra Eds, 2000, p. 275; G. Gottlich, VGB Power Tec, 2003, 5, 96; M.
  • Efficient processes for C0 2 capture are those where absorbents are aqueous solutions of inorganic (alkaline carbonates, ammonia) as well as organic (amines) bases. These processes invariably comprise two distinct steps.
  • the gaseous mixture containing C0 2 for example, the gas mixtures from the fossil fuel post-combustion contain, besides water, 4-15% of C0 2 as well as N 2 , 0 2 , S0 2 and, at a much lesser extent, nitrogen oxides and CO
  • the base is thermally regenerated by heating and relatively pure C0 2 is released. At the end of the process pure C0 2 may therefore be used as raw material or properly disposed in geological cavities, oceans or elsewhere.
  • Reaction [3] does not occur with tertiary amines as well as with sterically hindered primary and secondary amines. Reaction [1] is right hand shifted and is the prevailing one, whereas the reactions [2] and [3] contribute to a lesser extent to the C0 2 capture, and the lower is the AMH/C0 2 molar ratio the less they contribute. Moreover, the stability of the amine carbamate AMC0 2 in aqueous solution also determines the relative contribution of reaction [3] to the C0 2 capture.
  • aqueous solutions of blended amines have been investigated, such as AMP-MDEA, AM P-MMEA, AMP- DEA, MEA-MMEA (B.P. Mandal, et al., Chem. Eng. Sci., 2003, 58, 4137; B.P. Mandal, S.S. Bandyopadhyay, Chem. Eng. Sci., 2005, 60, 6438; D. Bonieri, et al., Ind. Eng. Chem. Res., 2005, 44, 3720; R. Idem, et al., Ind. Eng. Chem. Res., 2006, 45, 2414; W.-J.
  • the amines progressively degrade thus loosing their absorption ability and fresh amines must be added.
  • the amines are not completely inert but, especially at high temperature, they may damage the reactors' steel, so that corrosion inhibitors must be added to the absorbent solution too.
  • the C0 2 -loaded absorbent In order to regenerate the free amines for their reuse, the C0 2 -loaded absorbent must be heated at relatively high temperatures (1 10-140°C and pressures up to 4 bar) to force reaction [1] to go on in the opposite sense
  • reaction [4] can be carried out at lower temperatures ( ⁇ 100°C) and at reduced pressure ( ⁇ 1 bar).
  • a number of patented processes are directed to remove acid gases (H 2 S, HCN, S0 2 , besides C0 2 ) by means of aqueous solutions of amines.
  • the employed amines are the same, namely, MEA, MM EA, DEA, M DEA, AM P, DI PA, DGA and their blends.
  • the main differences amongst all of these processes deal with the use of different reaction activators or corrosion inhibitors, and the different experimental conditions used (temperature, pressure, amine concentration comprised between 15 and 70% by weight). Relevant effects may also be ascribed to the technical devices used to increase the gas-to-liquid exchange.
  • MDEA "Ucarsol HS-1 01 ", U nion Carbide (U SA) ; "aM D EA”, BASF AG (Germany); “ADIP-MDEA”, Shell (The Netherland); “Sulfinol-M”, Shell (The Netherland); ELF Aquitaine (France); The Dow Chemical Co. (USA).
  • DIPA "ADIP- DIPA”, “Sulfinol-D”, Shell (The Netherland); DGA: “Diglycolammine", Huntsman Corporation (USA).
  • Alkazid BASF AG (Germany) and “Catacab”, G.F. Versteed et al., (The Netherland) deal with aqueous solutions of alkaline salts of aminoacids.
  • AMISOL (Lurgi Kohle GmbH, Germany) for the C0 2 capture combines the physical absorption of methanol with the chemical absorption of amines by using water-methanol solutions of MEA and DEA at 5-40°C with pressure greater than 10 bar.
  • the overhead vapours of methanol and amines must be condensed by washing them with water or ethylene glycol before being recovered by fractionated distillation.
  • CCS Carbon dioxide Capture and Storage
  • C0 2 BOLs C0 2 BOLs, 0 2 binding organic liquids; RTILs, room temperature ionic liquids; R. Hart et al., Tetrahedron, 2010, 1082; D.J. Heldebrant et al., Energy Procedia, 2008, 1 187; C. L. Lotta et al., Ind. Eng. Chem. Res., 2008, 47, 539; J. E. Bara et al., Ind. Eng. Chem. Res., 2008, 47, 8496; J. H. Davis, Jr. et al., J. Am. Chem. Soc, 2002, 124, 927).
  • the stripping step of the process namely amine regeneration and pure C0 2 release, requires relatively high temperatures (typically, 1 10-140°C and pressure higher than 1 bar) due to the endothermic nature of reaction [4] so that a huge amount of energy is required to heat the aqueous solution due to both the high heat capacity (4.18 kJ kg 1 °C 1 ) and evaporation enthalpy of water (2.44 kJ g 1 ).
  • C0 2 could react with either primary or secondary amines forming the carbamate derivative (see reaction [6])
  • Reaction [5] is responsible for most of the captured C0 2 as the sterically hindered AM P does not form a stable carbamate.
  • the unstable AM P carbamate is formed as an intermediate along the molecular process leading to the alkyl carbonate (reaction [7])
  • Reaction [7] is peculiar of AMP in the absence of water, and does not occur with stable carbamates such as those of M EA, MM EA, DEA, etc. Moreover, both AMP carbamate and alkyl carbonate are unstable species than cannot be obtained in the presence of water.
  • the energy requirements are appreciably reduced not only for the lower decomposition-regeneration temperatures of the carbon contai ni ng species i n solution, but mainly for the lower heat capacity of the alcohols employed (2.5-2.7 kJ kg "1 ) with respect to water, for the lower temperature gap between absorption and desorption steps (30-60°C) with respect to aqueous solutions (80-100°C) and for the reduced solvent evaporation due to the high boiling temperature of the absorbent compared to the desorption temperatures. Moreover, also the thermal decomposition of the amine and the corrosion of the reactor is drastically reduced because of the lower temperatures employed and the absence of water.
  • a gas stream containing C0 2 (in particular between 5 and 12% v/v in air) is brought into contact at 1 bar and at temperatures between 20 and 40°C with an alcoholic solution of either a single amine or a blend of two amines (in the range 1 : 1 - 1 :3 on molar scale). Under these conditions a solution of the corresponding alkyl carbonate and, to a lesser extent, of the carbamate of the amine together with the protonated amine, is produced;
  • the solution obtained in the absorption step (a) is heated at a temperature between 50 and 80°C, and preferably between 65 and 80°C, at atmospheric pressure;
  • both absorption and desorption steps occur at the same time in two distinct reactors set at 20-40°C (the absorber) and 50-80°C, preferably 65-80°C (the desorber), respectively, connected to each other in a closed cycle, wherein the liquid is continuously circulating.
  • a cross heat exchanger cools the hot regenerated amine solution exiting from the desorber before being recycled to the absorber and, at the same time, preheats the carbonated amine solution exiting from the absorber at 20- 40°C, before being transferred to the desorber;
  • the absorption and the desorption steps can be carried out in two separate runs using either two different reactors or a single reactor acting as the absorber at 20-40°C in the first step and, once the C0 2 capture is completed, as the desorber at temperatures comprised between 50 and 80°C, preferably 65-80°C.
  • AMP 2- amino-2-methyl-1-propanol
  • DGA 2-(2-aminoethoxy)ethanol
  • mixtures of AMP with a different amine that are, but not limited to, AMP and, respectively, 2,2'-iminodiethanol (DEA), A/-methyl-2,2'-iminodiethanol (MDEA), 3,3'-imino-di-2-methylpropanol (DIPA) and A/-methyl-2-aminoethanol (MMEA), preferably mixtures of AMP with another of the above said amines in molar ratios second amine:AMP comprised between 1 : 1 and 1 :3.
  • DEA 2,2'-iminodiethanol
  • MDEA A/-methyl-2,2'-iminodiethanol
  • DIPA 3,3'-imino-di-2-methylpropanol
  • MMEA A/-methyl-2-aminoethanol
  • the solvents employed are either simple alcohols or polyhydroxylated aliphatic alcohols. Typical examples are 1- propanol, 2-propanol, 1-butanol, 2-butanol, mono methyl, mono ethyl and mono butyl ethers of ethylene glycol, mono methyl and mono ethyl ethers of diethylene glycol, mixtures of ethylene glycol, 1 ,2-propandiol, diethylene glycol and diethyl ether of diethylene glycol with, respectively, methanol, ethanol, and 1-propanol.
  • the increased capital cost due to the use of alcohols could be compensated, at least in part, by the lesser amount of amines employed (about 50% with respect to the aqueous solutions) that maintain unaltered their reaction capacity for a longer time.
  • the alcohols employed are inexpensive, thermally stable and are entirely recycled.
  • the formation of a precipitate allows to further decrease the desorption temperature to 50- 70°C, that is at lower temperature than it occurs when the precipitate is absent.
  • Figure 1 is a schematic illustration of the reactor for C0 2 absorption process (absorber);
  • Figure 2 shows a flowchart of the absorption/desorption/regeneration continuous cycle used in experimental tests of the present process.
  • the reaction of C0 2 capture takes place into the reactor 1 - schematically reproduced in Figure 1 - charged with the absorbent solution.
  • a sintered glass diffuser 2 is placed at the bottom of the reactor 1 and three polyethylene disks 3 are placed at regular intervals and fully immersed i n the l iquid .
  • I n Figure 1 the liquid level is indicated with L.
  • three polyethylene disks have been used, so that the gas mixture, while flowing through the diffuser 2, is split into micro-bubbles in such a way that the liquid-gas contact surface is greatly enhanced.
  • the three disks 3 spaced within the solution increase the liquid turbulence therefore providing the reacting liquid-gas mixture with a sufficient residence time.
  • the gas way out is placed at the top of the reactor. In such a device the C0 2 capture is very fast -even at room temperature and atmospheric pressure- without the need of any catalyst or reaction activators.
  • the absorbent solution contained into the absorber is an amine such as, but not limited to, AMP (2-amino-2-methyl-1-propanol) and DGA [2-(2-aminoethoxy)ethanol], or a mixture of two different amines such as, but not limited to, AMP mixed with DEA (2,2'-iminodiethanol), MDEA (A/-methyl-2,2'-iminodiethanol) , DI PA (3,3'-imino-di-2- methylpropanol), or MMEA (A/-methyl-2-aminoethanol), dissolved into either a single alcohol solution or a mixture of two different alcohols.
  • AMP 2,2'-iminodiethanol
  • MDEA A/-methyl-2,2'-iminodiethanol
  • DI PA 3,3'-imino-di-2- methylpropanol
  • MMEA A/-methyl-2-aminoethanol
  • the AMP/second amine molar ratios are comprised between 1 : 1 and 3: 1 .
  • the volume ratio of the two alcohols is comprised between 1 : 1 and 1 :2.
  • the absorbent temperature is kept between 20°C and 40°C, preferably at 20°C.
  • the absorber is fed with the gas mixture (C0 2 content in the gas flow may vary in the range 5 -12%) through the porous diffuser.
  • the outlet C0 2 concentration is analyzed by a gas chromatograph 4.
  • the carbonated amine solution exiting from the absorber (or the heterogeneous slurry, if the C0 2 absorption forms solid compounds) is continuously transferred to the desorbing reactor 5 ( Figure 2) by means of the pump 7 and connecting tubes.
  • the thermal decomposition of the products derived from the reaction of C0 2 with the absorbent takes place in the desorber unit 5, thus regenerating the ammine and producing pure C0 2 .
  • the desorber is heated up at temperatures between 50 and 80°C, preferably between 65 and 80°C.
  • thermocouple monitors the solution temperature during the desorption run. In order to sustain the decomposition kinetic, the solution is maintained under stirring.
  • a condenser 6 cooled by water at room temperature is placed on the top of the desorber for the condensation of the overhead vapor that is refluxed to the desorber.
  • the pure C0 2 produced by the desorption-regeneration process can be sequestered in standard ways or directly used.
  • the regenerated solution produced in the desorber unit 5 is continuously transferred into the absorber unit 1 by means of the pump 8 and connecting tubes.
  • a cross heat exchanger 9 is placed between the two reactors. The heat exchanger preheats the solution exiting from the absorber before being transferred to the desorber. At the same time, it cools down the solution exiting from the desorber before being recycled to the absorber.
  • the absorption and desorption processes take place continuously, at the same time, in a closed loop.
  • an alternative batch process can be adopted consisting in a complete absorption run and a complete desorption run occurring in the two distinct reactors 1 and 5 or, alternatively, in the same reactor 1 , which works in the first stage as an absorption reactor (at 20°C) and in the second stage, after the C0 2 absorption is completed, as a desorption reactor (at 50-70°C).
  • the present absorbent solution is preferably either an alcohol solution of single AMP (2-amino-2-methyl-1-propanol) or mixtures of AMP with a second amine selected from DEA (2,2'-iminodiethanol), MDEA (N-methyl-2,2'-iminodiethanol), DI PA (3,3'- imino-di-2-methylprpopanol), and MMEA (N-methyl-2-aminoethanol).
  • a further individual amine solution of preferred use according to the invention is an alcohol solution of DGA [2-(2-aminoethoxy)ethanol].
  • Preferred alcohols according to the invention are selected from the group consisting of 1-propanol, 2-propanol, 1-butanol, 2-butanol, mono methyl, mono ethyl and mono butyl ethers of ethylene glycol, mono methyl and mono ethyl ethers of diethylene glycol, mixtures of ethylene glycol and 1 ,2-propandiol, of either diethylene glycol, or diethyl ether of diethylene glycol, respectively, with methanol, ethanol and 1 - propanol.
  • the adopted experimental conditions are set to get the most efficient results when the gas mixtures contains 12% C0 2 by volume in air (gas mixture flux 12-16 dm 3 /h at room conditions).
  • the starting conditions are: the absorber 1 contains 0,300 dm 3 of the 2.0 M individual amine solution, or of the solution of a mixture of two amines.
  • the absorber temperature is kept constant at 20°C (by means of a thermostated bath not illustrated in the Figure 1). Pores' size of the diffuser 2 is in the range16-40 ⁇ .
  • a thermocouple (not illustrated in Figure 1) monitors the absorbent temperature.
  • the inlet and outlet C0 2 percentages in the flue gas m ixtu re are measured every 5 m i nutes usi ng a properly calibrated gas chromatograph (indicated as 4 in Figure 2).
  • the desorber unit 5 contains 0.300 dm 3 of the 2.0 M of the partially carbonated amine-alcohol solution (C0 2 absorbed in correspondence of 50% of its maximum solubility).
  • the reactor is kept at a constant temperature using a paraffin oil bath (not illustrated in Figure 2).
  • the desorption runs have been performed at temperatures of 65, 70, 75, and 80°C.
  • thermocouple monitors the solution temperature during the desorption process.
  • the desorber In order to sustain the desorption kinetic, the desorber is equipped with a magnetic stirrer. A condenser cooled by water at room temperature 6 is placed on the top of the desorber 5 in order to reflux the overhead vapors to the stripper. Actually, the amount of the vapors leaving the solution is low, as a consequence of the desorption temperature which is much lower than the solution boiling point.
  • the liquids, the carbonated and the regenerated ones, are continuously circulating in the closed loop, by means of the pumps 7 and 8. Altogether, the fluxes are comprised between 0.500 and 0.700 dm 3 /h.
  • the maximum absorption efficiency - calculated for 16 dm 3 h "1 flux with 12% C0 2 mixture - is obtained in correspondence of a constant liquid flux of 0.600 dm 3 h "1 .
  • a cross heat exchanger 9 placed between the two reactors, preheats carbonated liquid moving from the absorber 1 (at 20°C) to the desorber 5, and at the same time, cools the regenerated liquid moving from the desorber 5 (at 65-80°C) to the absorber 1 .
  • Each experiment - performed at a constant desorption temperature - lasts between 4 and 6 hours and it is stopped when the absorption efficiency value remains constant; it means that the amount of C0 2 absorbed is equal to the amount of C0 2 desorbed, that means that the amount of absorbent solution used in the absorption step is equal to the amount of absorbent solution regenerated in the desorption step.
  • the C0 2 absorption efficiency (percentage ratio of absorbed C0 2 compared to the C0 2 flowing in the absorbent) calculated for the different absorbent solutions and for each different desorption temperature; and the maximum absorption capacity of the amine alcohol solutions (the ratio between absorbed C0 2 and amount of amine, calculated as both weight % and in molar scale or "loading").
  • the starting concentration of the single amine used, or of the mixture of amines, is 2.0 M, and the weight percentage of the amine solutions is between 16.8 and 22.6.
  • the C0 2 absorption efficiency (average value) of the solutions of the single amine, and of their mixtures, increases as a consequence of the increased desorption temperature, and, at a given temperature, it decreases as the solvent viscosity increases. For this reason, it is preferable not to use pure ethylene glycol, but to use it diluted with methyl, ethyl or n-propyl alcohol to provide a lower viscosity of the solution.
  • Methanol based solutions are the most efficient, for a given amine and at a given regeneration temperature.
  • the desorption efficiency (percentage ratio between desorbed and absorbed C0 2 ) which is equal to the amine regeneration efficiency, was measured in function of desorption temperatures. The desorption process starts at 50°C and its rate increases as a function of the temperature: in most cases a desorption-regeneration efficiency greater than 90% was obtained at temperatures below than 70°C.
  • EXAMPLE 1 A solution of AMP 2.0 mol dm "3 (18.5% by weight) is prepared by dissolving 107 g of AMP in a 1 : 1 mixture (volume by volume) of ethylene glycol and ethanol to the overall volume of 0.600 dm 3 .
  • the absorber ( Figure 1) is charged with 0.300 dm 3 of the so obtained solution, and the temperature of the device is kept constant to 20°C by means of a thermostatic bath.
  • the remaining part of the solution is pre-carbonated with pure C0 2 up to 50% of its maximum solubility and afterwards it is transferred into the desorber unit.
  • Said reactor equi pped with a mag netic sti rrer and with a water-cooled condenser, is placed into a thermostatic oil-bath.
  • the temperature in the desorber unit is brought to 65°C.
  • the mixture of C0 2 and air (12% of C0 2 in volume) is continuously fed into the absorber through a diffuser at the bottom of the absorbent solution.
  • This absorber setup allows to reduce the size of the C0 2 bubbles therefore maximizing the exchange surface between the two reacting phases.
  • the mixture C0 2 /air has an average flow of 16 dm 3 h "1 , approximately.
  • Two peristaltic pumps allow the liquid mixtures to circulate continuously in a closed loop between the absorber and the desorber units through a cross heat exchanger.
  • the absorbed liquid, enriched in C0 2 is moved from the absorber to the desorber and, at the same time, the regenerated liquid is moved from the desorber to the absorber through the heat exchanger.
  • the flow of these two liquids is kept constant at the value of 0.600 dm 3 h "1 .
  • the process was stopped when the efficiency of C0 2 absorption remains constant and the equilibrium is reached.
  • the process is repeated with desorption temperature gradually brought to 70, 75 and 80°C.
  • the maximum loading capacity and the absorption efficiency at the above said four values of temperature of desorption-regeneration runs, are shown in the Table 1 above reported.
  • a solution of AMP 2.0 mol dm "3 (19.2% by weight) is prepared by dissolving 107 g of AMP in a 1 :2 mixture (v/v) of ethylene glycol and 1-propanol to the overall volume of 0.600 dm 3 .
  • the absorber unit ( Figure 1) is charged with part of said solution (0.300 dm 3 ) and the temperature of the device is kept constant to 20°C by means of a thermostatic bath.
  • the remaining part of the solution 0.300 dm 3 , is pre-carbonated with pure C0 2 up to 50% of its maximum solubility and afterwards it is transferred into the desorber unit.
  • the absorption-desorption process is carried out as described above in Example 1 .
  • the 13 C-NMR analysis of reaction mixtures shows that most of C0 2 is stored in solution as mono carbonate derivative of ethylene glycol (HOCH 2 CH 2 OC0 2 " ).
  • a solution of AMP 2,0 mol dm "3 (17.4% by weight) is prepared by dissolving 107 g of AMP in the monomethyl ether of diethylene glycol to the overall volume of 0.600 dm 3 .
  • the absorber unit ( Figure 1) is charged with part of said solution (0.300 dm 3 ) and the temperature of the device is kept constant to 20°C by means of a thermostatic bath.
  • the remaining part of the solution 0.300 dm 3 , is pre-carbonated with pure C0 2 up to 50% of its maximum solubility and afterwards it is transferred into the desorber unit.
  • the absorption-desorption process is carried out as described above in Example 1 but using three different temperature values: 65 , 70 a n d 75°C.
  • a precipitated is formed, that contains a mixture of carbamate [(AMPH 2 + )(AMPC0 2 " )] and carbonate [(AMPH 2 + ) 2 (C0 3 2" )] of protonated AMP that are decomposed in the desorption step.
  • Table 1 The results are reported in Table 1.
  • a solution of AMP and DEA in the 1 : 1 molar ratio and overall amine concentration 2.0 mol dm "3 (19.3% by weight) is prepared by dissolving 53.5 g of AMP and 63.1 g of DEA in a 1 : 1 (v/v) mixture of ethylene glycol and methanol to the overall volume of 0.600 dm 3 .
  • the absorber unit ( Figure 1) is charged with part of said solution (0.300 dm 3 ) and the temperature of the device is kept constant to 20°C by means of a thermostatic bath.
  • the remaining part of the solution 0.300 dm 3 , is pre-carbonated with pure C0 2 up to 50% of its maximum solubility and afterwards it is transferred into the desorber unit.
  • the absorption-desorption process is carried out as described above in Example 1 at three different temperature values: 65, 70 and 75°C.
  • the results are reported in Table 1.
  • the 13 C-NMR analysis of the reaction mixtures shows that C0 2 is stored in solution as DEA carbamate (DEAC0 2 " ), mono carbonate of ethylene glycol (HOCH2CH2OCO2 " ), and methyl carbonate (CH 3 OC0 2 " ).
  • a solution of AMP and MDEA in 1 : 1 molar ratio and overall amine concentration 2,0 mol dm "3 (20.7% by weight) is prepared by dissolving 53.5 g of AMP and 71.5 g of MDEA in a 1 : 1 mixture (v/v) of ethylene glycol and methanol to the overall volume of
  • the absorber unit ( Figure 1 ) is charged with part of said solution (0.300 dm 3 ) and the temperature of the device is kept constant to 20° C by means of a thermostatic bath.
  • 2,0 mol dm "3 (16.9 % by weight) is prepared by dissolving 53.5 g of AMP and 45.1 g of MMEA in a 1 : 1 (v/v) mixture of ethylene glycol and methanol to the overall volume of
  • the absorber unit ( Figure 1 ) is charged with part of said solution (0.300 dm 3 ) and the temperature of the device is kept constant to 20° C by means of a thermostatic bath. The remaining part of the solution, 0.300 dm 3 , is pre-carbonated with pure C0 2 up to 50% of its maximum solubility, then transferred into the desorber unit.
  • the absorption-desorption process is carried out as described above in Example
  • EXAMPLE 7 A solution of DGA 2,0 mol dm "3 (22.0 % by weight) is prepared by dissolving 126 g of DGA in the monoethyl ether of ethylene glycol to the overall volume of 0.600 dm 3 .
  • the absorber unit ( Figure 1) is charged with part of said solution (0.300 dm 3 ) and the temperature of the device is kept constant to 20°C by means of a thermostatic bath.
  • the remaining part of the solution, 0.300dm 3 is pre-carbonated with pure C0 2 up to 50% of its maximum solubility and afterwards it is transferred into the desorber unit.
  • the absorption-desorption process is carried out as described above in Example 1. The results are reported in Table 1 .
  • the 13 C-NMR analysis of the reaction mixtures allows to verify that most of C0 2 is stored in solution as carbamate of DGA (DGAC0 2 " ).
  • a solution of AMP 2.0 mol dm "3 is prepared by dissolving 53.3 g of AMP in 1- propanol to the overall volume of 0.300 dm 3 .
  • the so obtained solution is transferred into the absorber unit where the temperature is kept constant to 20°C and the absorption is carried out with pure C0 2 to its maximum solubility.
  • a precipitate is obtained, that contains a mixture of carbamate [(AMPH 2 + )(AMPOC0 2 " )] and carbonate [(AMPH 2 + ) 2 (C0 3 2" )] of protonated amine.
  • the reactors containing the heterogeneous mixture are placed into a heating bath and the temperature is gradually increased from 50 to 65°C.
  • the reactor is connected to a gastight apparatus for the measure of the gas volume equipped with a pressure equalizing system at room temperature.
  • the maximum loading capacity measured on four absorption-desorption cycles (average loading), was 0.72 mol of C0 2 for 1 mol of the amine, corresponding to 35.6% by weight.
  • the C0 2 desorption efficiency and the regeneration efficiency of the amine was 94%.

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Abstract

La présente invention concerne un procédé pour la capture de CO2 dans des mélanges de gaz et pour l'élimination de CO2 de déchets gazeux de processus industriels ou de gaz de combustion, qui est conduit en mettant en contact les mélanges de gaz avec une solution absorbante d'amines dans des alcools anhydres ; ce procédé comprend l'absorption de CO2 (1) à température ambiante et pression atmosphérique et l'absorption de CO2 (5) et la régénération d'amines à des températures inférieures à la température d'ébullition de la solution et à pression atmosphérique.
PCT/EP2011/065531 2010-09-13 2011-09-08 Procédé pour la séparation et la capture de co2 à partir de mélanges de gaz utilisant des solutions d'amines dans des alcools anhydres WO2012034921A1 (fr)

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WO2014099268A1 (fr) * 2012-12-21 2014-06-26 Exxonmobil Research And Engineering Company Capture de co2 par séparation des phases d'un produit amine-co2
WO2015123490A1 (fr) * 2014-02-13 2015-08-20 Research Triangle Institute Contrôle de l'eau dans des systèmes de récupération de gaz acide non aqueux
KR20170034587A (ko) 2015-09-21 2017-03-29 경희대학교 산학협력단 이산화탄소 흡수제
US9707512B2 (en) 2012-12-21 2017-07-18 Exxonmobil Research And Engineering Company Amine promotion for CO2 capture
CN107427759A (zh) * 2015-03-26 2017-12-01 新日铁住金株式会社 用于分离和捕集二氧化碳的吸收液以及使用所述吸收液分离和捕集二氧化碳的方法
WO2021119058A1 (fr) * 2019-12-11 2021-06-17 Research Triangle Institute Solvant non aqueux pour éliminer un gaz acide d'un flux de gaz de traitement pour des applications à haute pression
WO2023073389A1 (fr) 2021-10-26 2023-05-04 Totalenergies Onetech Procédé de purification d'un mélange gazeux comprenant du dioxyde de carbone et éventuellement du sulfure d'hydrogène

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WO2014099268A1 (fr) * 2012-12-21 2014-06-26 Exxonmobil Research And Engineering Company Capture de co2 par séparation des phases d'un produit amine-co2
US9707512B2 (en) 2012-12-21 2017-07-18 Exxonmobil Research And Engineering Company Amine promotion for CO2 capture
WO2015123490A1 (fr) * 2014-02-13 2015-08-20 Research Triangle Institute Contrôle de l'eau dans des systèmes de récupération de gaz acide non aqueux
JP2017506150A (ja) * 2014-02-13 2017-03-02 リサーチ トライアングル インスティテュート 非水酸性ガス除去システムにおける水分制御
US10166503B2 (en) 2014-02-13 2019-01-01 Research Triangle Institute Water control in non-aqueous acid gas recovery systems
CN107427759A (zh) * 2015-03-26 2017-12-01 新日铁住金株式会社 用于分离和捕集二氧化碳的吸收液以及使用所述吸收液分离和捕集二氧化碳的方法
EP3275526A4 (fr) * 2015-03-26 2018-12-12 Nippon Steel & Sumitomo Metal Corporation Solution absorbante pour séparer et récupérer du dioxyde de carbone, et pour séparer et récupérer du dioxyde de carbone dans lequel cette dernière est utilisée
US10717038B2 (en) 2015-03-26 2020-07-21 Research Institute Of Innovative Technology For The Earth Absorbing solution for separating and capturing carbon dioxide, and method for separating and capturing carbon dioxide in which same is used
KR20170034587A (ko) 2015-09-21 2017-03-29 경희대학교 산학협력단 이산화탄소 흡수제
US10543454B2 (en) 2015-09-21 2020-01-28 University-Industry Cooperation Group Of Kyung Hee University Carbon dioxide absorbent
WO2021119058A1 (fr) * 2019-12-11 2021-06-17 Research Triangle Institute Solvant non aqueux pour éliminer un gaz acide d'un flux de gaz de traitement pour des applications à haute pression
WO2023073389A1 (fr) 2021-10-26 2023-05-04 Totalenergies Onetech Procédé de purification d'un mélange gazeux comprenant du dioxyde de carbone et éventuellement du sulfure d'hydrogène

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