WO2006049610A1 - Système et méthode de séparation sélective de mélanges gazeux employant des fibres creuses - Google Patents

Système et méthode de séparation sélective de mélanges gazeux employant des fibres creuses Download PDF

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Publication number
WO2006049610A1
WO2006049610A1 PCT/US2004/036036 US2004036036W WO2006049610A1 WO 2006049610 A1 WO2006049610 A1 WO 2006049610A1 US 2004036036 W US2004036036 W US 2004036036W WO 2006049610 A1 WO2006049610 A1 WO 2006049610A1
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Prior art keywords
gas
absorbent solution
gaseous mixture
absorption
solution
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PCT/US2004/036036
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English (en)
Inventor
Kamalesh K. Sirkar
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New Jersey Institute Of Technology
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Priority to PCT/US2004/036036 priority Critical patent/WO2006049610A1/fr
Publication of WO2006049610A1 publication Critical patent/WO2006049610A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/38—Liquid-membrane separation
    • 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
    • B01D53/22—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 diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • 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
    • 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 disclosure is directed to systems and methods for separating one or more components from a gaseous mixture and, more particularly, to systems and methods for separating carbon dioxide from a gaseous system, e.g., atmospheric air, using hydrophobic porous/nonporous hollow fibers that are in contact with an absorbent solution.
  • the present disclosure further relates to systems and methods for regenerating the absorbent solution on a periodic basis.
  • FTMs Gas separation using facilitated transport membranes
  • ILM immobilized liquid membrane
  • solvent- swollen polymer membrane a type of FTMs investigated generally fall into the following three categories: (1) immobilized liquid membrane (ILM), (2) solvent- swollen polymer membrane, and (3) fixed-carrier membranes.
  • ILM immobilized liquid membrane
  • FTMs over conventional polymeric membranes include enhanced selectivity and permeability for the target species because of reversible reactions between the carriers in FTM and the target species. This characteristic makes FTM especially attractive when the target species in the feed gas mixture exists in low concentrations because, to accomplish the separation and/or purification task, the limited transmembrane driving force is generally too small for conventional polymeric membranes.
  • ILM has been widely investigated for facilitated transport of carbon dioxide using various carriers.
  • Ward and Robb made a pioneering study on CO 2 permeation through a thin layer of carbonate/bicarbonate aqueous solution.
  • Otto and Quinn and later Suchdeo and Schultz made theoretical analyses Of CO 2 transport through carbonate/bicarbonate ILMs.
  • Other investigators used amines as the carriers and/or ion-exchange membranes as the substrates.
  • LeBlanc et al. and later Way et al. studied facilitated transport Of CO 2 in ion-exchange membranes using various organic amine counterions.
  • Teramoto et al. used monoethanolamine (MEA) solutions, while Guha et al. and Davis and Sandall used diethanolamine (DEA) solutions immobilized in porous substrates as ILMs to study CO 2 transport.
  • MEA monoethanolamine
  • DEA diethanolamine
  • EDA ethylenediamine
  • ILMs liquid solution
  • the low stability can be a result of liquid washout and/or the evaporation of the liquids into the gas phases during operation.
  • Various strategies have been employed to alleviate the problems of carrier loss and ILM drying out. Hughes et al. tried to circumvent the stability problem of an Ag+-containing ILM for olefin-paraffin separation by periodically regenerating it.
  • a more common practice when aqueous solutions are used as the ILM fluid is to humidify both the feed and sweep gas streams simultaneously.
  • Another alternative is to use low volatility and hygroscopic liquids, such as poly(ethylene glycol) (PEG) or glycerol as the major component in the ILM fluid.
  • VDF hydrophilic poly(vinylidene fluoride)
  • Na 2 C ⁇ 3-glycerol ILM showed high CO 2 /N 2 selectivities, but relatively low CO 2 permeances.
  • the glycerol-based ILM could be useful for CO 2 removal from gas streams containing low concentrations of CO 2 if its CO 2 permeance were to be significantly increased.
  • ILM liquid and carrier species Because the feed gas is normally not completely humidified (i.e., RH ⁇ 100%), the ILM must be stable when the feed stream RH is relatively low. Also, to conserve oxygen, the membrane should have very high CO 2 /O 2 selectivity (e.g., >2000) at low RHs. Moreover, the ILM components should be completely environmentally benign. Therefore, the most studied amines in the literature (e.g., MEA, DEA, and EDA) are not suitable for such application because of their relatively high volatilities and irritative nature.
  • Glycine has been used as an additive in carbonate/bicarbonate solutions for the selective removal of CO 2 from industrial gas streams.
  • LeBlanc et al. demonstrated that glycine salt can be a better carrier species for CO 2 than carbonate in ion-exchange substrate-based ILMs.
  • glycine salts have been incorporated into polymeric membranes for enhanced CO 2 separation from gas streams containing CO 2 and H 2 .
  • Ho disclosed a CO 2 separating polymeric membrane fabricated from poly( vinyl alcohol) and glycine salts (e.g., glycine-K and glycine-Li).
  • carbon dioxide may be effectively separated from a gaseous system, e.g., atmospheric air, using hydrophobic porous/nonporous hollow fibers that are in contact with an absorbent solution.
  • Systems and methods for regenerating the absorbent solution on a periodic basis so as to permit further separation cycles are also provided according to the present disclosure.
  • a hygroscopic nonvolatile CO ⁇ -absorbent solution is placed in contact with hollow fibers.
  • the hygroscopic solution typically consists of one or more chemically-reactive, reversible, non- volatile carbon dioxide absorbents in a non-volatile hygroscopic solution.
  • the separation system generally includes hydrophobic porous/non-porous hollow fibers.
  • the gaseous mixture is generally heated and moist/humidified, and is advantageously fed through the hollow fibers. As the moist gaseous mixture passes through the hollow fibers, carbon dioxide is absorbed by the hygroscopic solution, i.e., the carbon dioxide passes through the hollow fibers and is selectively absorbed by the hygroscopic solution.
  • the hygroscopic solution is advantageously regenerated by passing a sweep gas through the hollow fibers.
  • the sweep gas is typically heated and dry, thereby facilitating effective carbon dioxide desorption from the hygroscopic solution.
  • the gas, e.g., carbon dioxide, previously absorbed by the hygroscopic solution is absorbed by the sweep gas, thereby regenerating the absorbent solution so that such solution may be used for subsequent absorption cycles.
  • the disclosed systems and methods provide an effective means for removal of a gas, e.g., carbon dioxide, from atmospheric air on a cyclic basis.
  • Figure 1 is a schematic diagram of a system for gas separation according to an exemplary embodiment of the present disclosure
  • Figure 2 is a plot that shows the absorption behavior of CO 2 in pure glycerol carbonate and 0.5 M sodium glycinate in a water and glycerol carbonate mixture with a completely humidified feed according to an exemplary embodiment of the present disclosure
  • Figure 3 is a plot that shows the absorption behavior of CO 2 absorbed in an exemplary hollow fiber module with a completely humidified feed according to the present disclosure for 1 M sodium glycinate and 0.5 M sodium glycinate absorbent solutions;
  • Figure 4 is a plot that shows absorption behavior of CO 2 for feed gas humidities of 75% and 95% according to an exemplary embodiment of the present disclosure
  • Figure 5 is a plot of CO 2 concentration in the gas stream at an absorber outlet according to an exemplary embodiment of the present disclosure
  • Figure 6 is a plot of CO 2 concentration at an absorber outlet for successive absorption steps for a glycerol-containing absorbent solution according to an exemplary embodiment of the present disclosure
  • Figure 7 is a plot of CO 2 concentration at an absorber outlet for 0.833 M and 1.5 M sodium glycinate absorbent solutions (feed gas flow rate of 4 cc/min) according to an exemplary embodiment of the present disclosure.
  • Figure 8 is a plot of CO 2 concentration at an absorber outlet for successive absorption steps for 3 M sodium glycinate with a glycerol-based absorbent solution according to an exemplary embodiment of the present disclosure.
  • the present disclosure provides advantageous systems and methods for separating one or more gaseous components/molecules from a gaseous mixture.
  • the disclosed systems and methods are particularly advantageous for separating carbon dioxide from a gaseous system, e.g., atmospheric air.
  • hydrophobic porous/nonporous hollow fibers are placed in contact with an absorbent solution and a gaseous mixture is passed through the hollow fibers.
  • the absorbent solution advantageously absorbs the desired component or components from the gaseous mixture, e.g., CO 2 , for an extended period of time. Thereafter, the absorbent solution is regenerated on a periodic basis, e.g., using a sweep gas that is passed through the hollow fibers.
  • the systems and methods of the present disclosure are susceptible to many commercial and/or industrial applications.
  • the systems and methods described herein for separating a gas or gases from a gas mixture have significant utility in the battery and fuel cell fields.
  • applications for effectively and efficiently scrubbing or removing gas/gases from a gas mixture are innumerable, particularly where regeneration and/or replacement of an absorbent solution is avoided/unnecessary for extended periods.
  • the disclosed systems and methods are to be understood to find applicability in all gas separation applications wherein it is desired to remove a gas (or gases) from a gas mixture over an extended period (e.g., multiple hours), and to subsequently regenerate the absorbent solution employed in such separation process for effective reuse.
  • Atmospheric air generally includes carbon dioxide at levels of about 350 ppm. In a variety of applications, substantial reductions in carbon dioxide levels are desired and/or required. In certain applications, it may be desired to reduce the presence of carbon dioxide to levels of 5 ppm, 50 ppm, 100 ppm or the like.
  • Zn-air batteries generally exhibit enhanced operation when the carbon dioxide level in the air is at or approaches zero.
  • alkaline fuel cells generally exhibit enhanced performance when operated in gaseous environments that are substantially devoid of carbon dioxide.
  • System 100 includes a hollow fiber membrane module 102 that houses a plurality of hollow fiber membranes 104.
  • the hollow fiber membranes 104 are generally aligned with the longitudinal axis of module 102, although alternative geometric configurations may be employed.
  • Module 102 is typically defined by an outer housing 106 that serves to confine the hollow fiber membranes 104 within module 102 and to maintain an absorbent solution on the shell side of the fibers.
  • Input and output ports 108a, 108b are generally provided for facilitating introduction and withdrawal of an absorbent solution from module 102.
  • Gas flow is generally introduced to hollow fiber membrane module 102 at a first end 110 thereof. Gas flow exits module 102 at a second end 112 which is generally opposite first end 110.
  • a gas supply 114 is generally provided upstream of hollow fiber membrane module 102.
  • gas supply 114 takes the form of a canister containing a CO 2 /N 2 gas mixture.
  • hollow fiber membrane modules of the present disclosure may be employed with gas feed streams that originate from a variety of sources and that constitute/comprise various gaseous components, as will be apparent to persons skilled in the art.
  • Pressure gauge(s) 116 are typically positioned with respect to gas flow line 118, thereby permitting real time monitoring of gas pressure at the feed side of system 100.
  • Humidifier(s) 120 are advantageously associated with feed line 118, thereby permitting the humidification of the gas flow from gas supply 114.
  • a plurality of humidifiers 120 are provided in series in system 100.
  • Valving 122 is typically provided to permit routing of the gas flow relative to humidifiers 120, e.g., to permit bypassing of humidifiers (in whole or in part), as may be desired in connection with operation of system 100.
  • a controller 124 and/or a mass flow transducer 126 may also be included in feed line 118 to control and/or measure the gas flow rate through gas line 118 and into module 102.
  • the gas feed is introduced to module 102 at first end 110.
  • the gas flow is distributed to individual hollow fibers 104 that are positioned within outer housing 106.
  • the hollow fibers 104 may be fabricated from various materials, although in exemplary embodiments of the present disclosure hollow fibers 104 are fabricated from polypropylene, e.g., microporous, hydrophobic polypropylene.
  • the geometric properties and characteristics of hollow fibers 104 are generally selected to provide desired absorption levels into the absorption solution that surrounds the hollow fibers 104 within housing 106.
  • hollow fibers 104 constituted microporous, hydrophobic polypropylene fibers of 17 cm length, an inner diameter (ID) of 240 ⁇ m and an outer diameter (OD) of 300 ⁇ m.
  • the present disclosure is not limited to such exemplary hollow fibers, but is merely illustrated thereby.
  • the system 100 that is schematically depicted in Fig. 1 includes a gas chromatograph 128 associated with egress line 130 that exits from the second end 112 of module 102. Although gas chromatograph 128 is shown "in line" with egress line 130, such arrangement is not required according to the present disclosure. Rather, gas component levels in the gas egress from module 102 may be measured through periodic sampling, as desired, or may be presumed to meet desired levels based on the design and operation of system 100, as will be readily apparent to persons skilled in the art.
  • the absorbent solution for use in membrane module 102 is selected to provide absorption properties relative to the gas/gases that is/are to be separated from the gas mixture fed to module 102.
  • Exemplary absorption solutions for use according to the present disclosure include glycerol and/or glycerol carbonate.
  • a reactive carrier may be added to the foregoing solution(s), e.g., sodium glycinate, lithium glycinate, potassium glycinate, and the like, to increase the solution's absorption properties.
  • the reactive carrier/absorption solution may further include water, e.g., if the combination of the reactive carrier and the absorption solution exhibit, in whole or in part, the characteristics of a suspension.
  • Additional absorbent materials for use according to the present disclosure include polyamidoamine (PAMAM) dendrimers of generation zero.
  • PAMAM polyamidoamine
  • Dendrimers are structurally controlled macromolecules that are highly branched polymers composed of treelike dendrons emanating from a central core. Dendrimer structure is generally characterized by the number of generations (g), functionality of the branching points (f), and the length of the chain units between them.
  • the absorbent solution is generally packed in the shell side of the module without air gaps to create a stable, immobilized absorbent-gas interface at each pore mouth of the hollow fiber membrane.
  • an absorbent solution is introduced to a module that contains hollow fiber membranes, e.g., exemplary hollow fiber membrane module 102 schematically depicted in Fig. 1.
  • the absorbent solution contacts the outer shell of the hollow fibers positioned within the module, e.g., hollow fibers 104 schematically depicted in Fig. 1.
  • a gaseous mixture is introduced to the module and flows through the hollow fibers. Typically, the gaseous mixture is humidified before introduction to the module.
  • the absorption solution is effective in absorbing desired gas/gases from the gaseous mixture, such gas molecules passing through the pores of the hollow fiber membranes for absorption by the absorption solution.
  • the separation system of the present disclosure has been found to operate effectively for extended periods, e.g., for periods extending up to eight hours without intervening regeneration of the absorption solution.
  • Such advantageous performance e.g., for separation of carbon dioxide from a CO 2 /N 2 gas mixture, is highly desirable and surprising in view of prior art teachings.
  • the reactive carrier sodium glycinate was added. Since the prepared IM sodium glycinate solution in glycerol carbonate turned out to be a suspension, water was added in a 1:1 volume ratio. In addition, a 0.5 M sodium glycinate solution in glycerol carbonate and water was tested as an absorbent solution and its absorption characteristics were studied using a completely humidified feed containing 5 vol % of CO 2 (95% N 2 ). The absorption behaviors of these systems were compared with that of pure glycerol carbonate as the absorbent (see Fig. 2).
  • Fig. 2 compares the amount of CO 2 absorbed in the hollow fiber module per min by 0.5 M and 1.0 M sodium glycinate solutions in glycerol carbonate plus water. Based on this experimental work, only a limited increase in the absorption capacity of the absorbent was observed when the carrier concentration was doubled.
  • the presence of moisture is known to influence the reaction of CO 2 with a carrier (e.g., sodium glycinate).
  • a carrier e.g., sodium glycinate
  • the effect of humidity level of the feed gas on CO 2 absorption was studied for one of the foregoing absorbent solutions (i.e., a solution of 1 M sodium glycinate in glycerol carbonate plus water (1 :1)).
  • Part of the experimental setup was modified so as to facilitate relativity humidity adjustments of the feed gas to 75%.
  • Unsteady state absorption characteristics of the absorbent solution were studied using a feed gas at 75% relative humidity containing 5% CO 2 in nitrogen (balance), and compared with that of a feed gas at 95% relative humidity.
  • the comparative results are shown in the plot of Fig. 4. After a period of about three and half hours, a significant decrease in CO 2 absorption was observed for the 75% relative humidity feed gas as compared to the 95% relative humidity feed gas.
  • glycerol in the absorbent solution can function to retain moisture more effectively and can therefore increase the absorption capacity of an.absorbent solution.
  • an absorbent solution having 10 vol% glycerol and 20 vol% water in glycerol carbonate, such solution also having a total sodium glycinate concentration of 0.83 M was prepared and tested in the separation system described above. Successive and repetitive absorption and desorption experiments were carried out with the foregoing absorbent solution using air that initially contained 350 ppm Of CO 2 as the feed gas and N 2 as the stripping gas.
  • the absorption step was carried out by passing feed gas at a constant flow rate of 8.3 cc/min for eight (8) hours, followed by an immediate desorption step, in which N 2 was passed through the hollow fibers for a period of twelve (12) hours at a constant rate of 20 cc/min.
  • the first three absorption steps were carried out using a feed gas having 75% relative humidity.
  • a small improvement in the absorption capacity of the absorbent solution was observed when glycerol was added to the absorbent solution.
  • the absorption behavior of successive absorption steps is plotted in Fig. 6. From these results, it is noted that there is a small difference in the amount of CO 2 separated from the feed stream between successive absorption steps.
  • the fourth absorption step was carried out with a feed stream having 95% relative humidity.
  • the results of this fourth step are compared with the previous three absorption steps in Fig. 6.
  • the absorption behavior of the fourth absorption step closely parallels the performance of the third absorption step over the course of the eight (8) hour experimental run.
  • the difference in CO 2 absorption performance between successive absorption steps may be addressed, at least in part.
  • an absorption solution having 25% glycerol, 20% water in glycerol carbonate having a sodium glycinate concentration of 1.5 M was prepared and tested.
  • the absorption characteristics of this absorption solution is set forth in the plot of Fig. 7, and is compared with a comparable absorption solution having 0.833 M sodium glycinate. Only a small improvement in CO 2 absorption was observed when more glycerol, and hence more sodium glycinate, was added to the absorbent solution.
  • the module it is generally more effective to design the module based on the fiber area required to achieve the desired level of gas separation, rather than on the amount of absorbent solution needed to perform the task. Since the experimental data for 3 M sodium glycinate solution in glycerol as absorbent solution and feed gas flow rate of 8.33 cc/min achieves a desirable level of performance (i.e., effluent CO 2 concentration during the initial period was about 47 ppm and slowly increased to 97 ppm in a period of eight hours), exemplary module design calculations are provided herein based on the foregoing experimental data.
  • the sodium glycinate concentration in glycerol can be increased, e.g., from 3 M to 4 M.
  • Higher concentrations of carrier(s), e.g., acid salts, may be employed to further enhance system performance, subject to solubility restraints.
  • An increased concentration of sodium glycinate would likely increase the gas flow rate that can be effectively treated by a module having 40 fibers/17 cm length from 8.33 cc/min to about 12.5 cc/min.
  • a module of 5" diameter and 18" length having 99,150 fibers should be sufficient to perform the required level of CO 2 separation at the increased sodium glycinate concentration.
  • modules design and/or sizing may be undertaken according to the present disclosure, e.g., by modifying the absorbent solution, as will be apparent to persons skilled in the art from the present disclosure.
  • solutions with higher absorption capacity can reduce the module dimension, e.g., to a 3-4" diameter range.
  • Regeneration of the absorbent solution or stripping of CO 2 from the absorbent solution may be accomplished by passing N 2 through the hollow fibers for a period of twelve (12) hours at a constant rate of 20 cc/min. Since the module design data was based on a feed gas of relative humidity 75%, the exemplary module disclosed herein should perform steadily when atmospheric air is treated. In the experimental runs described herein, N 2 gas was used for the regeneration/desorption process. However, alternative sweep gases, e.g., hot air, are contemplated for use in regeneration of the absorbent solution after succeeding absorption step.
  • exemplary absorbent solutions according to the present disclosure e.g., 3 M sodium glycinate in glycerol
  • the use of hot air should not pose an issue for desorption.
  • Experimental runs to study the effects of hot air on the performance of the system and to model the flow rate, temperature specifications of hot air and time needed for regeneration, would further establish the efficacy of hot air for regeneration of absorbent solutions according to the v present disclosure.

Abstract

La présente invention a pour objet un système et une méthode de séparation d’un gaz, par exemple le dioxyde de carbone, à partir d’un mélange gazeux, en employant un module membranaire à fibres creuses. Ledit module contient une solution absorbante qui absorbe efficacement les gaz pendant une période de temps prolongée, par exemple huit heures, sans régénération ni remplacement. La solution absorbante est ensuite régénérée en faisant passer un gaz de purge à travers les fibres creuses du module. Ledit système de séparation peut en particulier être employé dans des applications de type piles à combustibles ou accumulateurs.
PCT/US2004/036036 2004-10-29 2004-10-29 Système et méthode de séparation sélective de mélanges gazeux employant des fibres creuses WO2006049610A1 (fr)

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US20120111192A1 (en) * 2009-04-02 2012-05-10 Jewgeni Nazarko Apparatus and method for removing carbon dioxide (co2) from the flue gas of a furnace after the energy conversion
US8784532B2 (en) 2011-03-03 2014-07-22 Phillips 66 Company Sorbent regeneration in a heated hollow-fiber assembly
CN108579706A (zh) * 2011-05-17 2018-09-28 恩弗里德系统公司 用于从室内空气降低二氧化碳的吸着剂

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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US8784532B2 (en) 2011-03-03 2014-07-22 Phillips 66 Company Sorbent regeneration in a heated hollow-fiber assembly
CN108579706A (zh) * 2011-05-17 2018-09-28 恩弗里德系统公司 用于从室内空气降低二氧化碳的吸着剂

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