CN102257342A - Carbon dioxide recovery method using cryo-condensation - Google Patents

Carbon dioxide recovery method using cryo-condensation Download PDF

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Publication number
CN102257342A
CN102257342A CN2009801511783A CN200980151178A CN102257342A CN 102257342 A CN102257342 A CN 102257342A CN 2009801511783 A CN2009801511783 A CN 2009801511783A CN 200980151178 A CN200980151178 A CN 200980151178A CN 102257342 A CN102257342 A CN 102257342A
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fluid
rich
small part
elementary
heat exchange
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CN102257342B (en
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F·洛克伍德
J-P·特拉尼耶
C·韦伯
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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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
    • B01D53/002—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 condensation
    • 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

Abstract

Disclosed is a method for producing at least one gas having a low CO2 concentration and one or more primary fluids having a high CO2 concentration from a fluid which is to be treated and contains CO2 and at least one compound that is more volatile than CO2.Said method comprises the following steps: a) the fluid to be treated is subjected to a first cooling process using heat exchange without the fluid undergoing a change of state; b) at least some of the fluid to be treated and cooled in step a) is cooled a second time such that a solid is obtained which contains mainly CO2 and at least the gas having a low CO2 concentration; and c) a step in which at least some of said solid is liquefied such that the one or more primary fluids having a high CO2 concentration are obtained. The disclosed method is characterized in that at least part of the first cooling process in step a) is carried out by heating at least some of the one or more primary fluids having a high CO2 concentration.

Description

Reclaim the method for carbon dioxide by cryogenic condensation
The present invention relates to a kind of seizure comprises at least a than carbon dioxide CO 2Have more volatile compound, for example methane CH 4, oxygen O 2, argon Ar, nitrogen N 2, carbon monoxide CO, helium He and/or hydrogen H 2Fluid in the method for carbon dioxide.
The present invention can be specially adapted to the unit by carbon fuel such as coal, hydro carbons (natural gas, fuel oil, petrochemistry residue etc.), home scrap, living beings generation electricity and/or steam, but also, handle the natural gas when leaving producing well applicable to gas from refinery, chemical plant, steel mill or cement factory.It also applicable to the flue gas in the boiler of using from heating building or even be applicable to waste gas from the vehicles, more generally be applicable to produce to contain CO 2Any commercial run of flue gas.
Carbon dioxide is greenhouse gases.Because environment and/or economic cause become day by day and wish by catching CO 2, then, for example pass through CO 2Be stored in the suitable geological stratification or reduce or even eliminate CO by self assets value that realizes it 2Discharging in atmosphere.
The technology of the catching carbon dioxide of known some is for example based on using by chemical reaction separation of C O 2The method of compound solution wash fluid, for example use the method for MEA washing.These methods have following shortcoming usually:
-high energy consumption (be used for and CO 2The regeneration of the compound of reaction is relevant),
-with the degraded of the compound of carbon dioxide reaction,
-since with the corrosion of the compound of carbon dioxide reaction.
At cryogenic condensation, promptly cool off until solid CO occurring 2The field in, can mention document FR-A-2820052, it discloses a kind of CO of making 2The method of the extraction by anti-sublimation (anti-sublimation) (promptly by solidifying not via liquid state) by gas.Institute's chilling requirement provides by the fractionation of cryogenic fluid.The big energy of this method consumption.
Document FR-A-2894838 discloses the method for same type, wherein with the partially liq CO that produces 2Recirculation.With the poor CO of part that produces 2Gas is used for the water of this process mixture of condensation.Cold can be supplied by gasification LNG (liquefied natural gas).This synergy has reduced the specific energy consumption (specific energy consumption) of this method, however even now it also need big energy and need the LNG terminal.
An object of the present invention is to provide a kind of from containing CO 2Improvement method with catching carbon dioxide at least a fluid that has more volatile compound than carbon dioxide.
The present invention at first relates to a kind of by containing CO 2With at least a CO that compares 2The process fluid that has more volatile compound is produced at least a poor CO 2Gas and one or more rich CO 2Elementary fluid and the method for implementing according to the following step:
A) the passing through heat exchange of described process fluid and do not change state first the cooling;
B) in step a), cool off to the described process fluid of small part second the cooling to obtain at least a CO that mainly contains 2Solid and described at least poor CO 2Gas; With
C) comprise and liquefy to the described solid of small part and make it can obtain described one or more rich CO 2The step of elementary fluid;
Described method be characterised in that in step a), carry out described first be cooled to small part by being heated to described one or more the rich CO of small part 2Elementary fluid and obtaining.
This process fluid is usually from boiler or produce any device of flue gas.These flue gases can be carried out various preliminary treatment, particularly in order to remove NOx (nitrogen oxide), dust, SOx (oxysulfide) and/or water.
Before the separation, process fluid is single-phase, is gaseous state or liquid form, perhaps is heterogeneous." gaseous state " form is meant " basic gaseous state " form.Particularly, if process fluid is made of pretreated flue gas, then it can contain dust, solid particle such as cigarette ash and/or drop especially.
This process fluid contains CO 2, it is separated by cryogenic condensation with other components of described fluid.These other components comprise one or more and have more volatile compound than carbon dioxide with regard to condensations, for example methane CH 4, oxygen O 2, argon Ar, nitrogen N 2, carbon monoxide CO, helium He and/or hydrogen H 2This process fluid mainly comprises nitrogen usually or mainly comprises CO or mainly comprise hydrogen.
In step a), this process fluid is at first cooled off and should not become state.The inventor confirmed this cooling can be advantageously to small part by with rich CO from separating technology 2The heat exchange of fluid and carrying out.In addition, it can be advantageously to small part by with poor CO from separating technology 2Fluid thermal exchanges and carries out.Make these cold fluid heating, and make this process fluid cooling from separating technology.This makes can reduce cooling down operation institute energy requirement.
Step b) comprises by making process fluid be increased to CO 2The temperature that three phase point (triple point) is following and CO in the process fluid simultaneously 2Divide and be pressed in CO 2Three phase point pressure is following and solidify originally gaseous state CO 2For example the stagnation pressure of process fluid is near atmospheric pressure.This solidifies operation and is known as CO sometimes 2" cryogenic condensation " or " anti-sublimation " of (by expansion) process fluid.
Compare CO 2Having more volatile specific compound does not solidify and still is gaseous state.With not solidified CO 2Together, these constitute described poor CO 2Gas promptly is constructed as follows described gas, and it comprises less than 50 volume %CO 2, preferably less than 10 volume %CO 2According to a particular, described poor CO 2Gas contains less than 1 volume %CO 2According to other particular, it contains greater than 2%CO 2According to other particular, it contains greater than 5%CO 2The solid that forms mainly comprises CO 2, that is,, contain at least 90 volume % if consider gaseous state, preferably contain at least 95 volume %, more preferably also contain at least 99 volume %CO 2
Except CO 2In addition, this solid can comprise other compounds.For example can mention other compounds that also may solidify, or be included in bubble and/or fluid drop in the described solid block.This has explained that how this solid is can be potentially not only by solid CO 2Constitute.Should " solid " can contain non-solid part such as fluid inclusions (drip, bubble etc.).
Then with also not solidified compound separation behind this solid and the cryogenic condensation and recovery.Next, in step c), solid is got back to such temperature and pressure condition so that it becomes fluid, liquid and/or gaseous state.Then to the described solid liquefiable of small part.This produces one or more rich CO then 2Elementary fluid.With these fluids be described as " elementary " be described as " secondary " and handle fluid and distinguish." rich CO 2" be meant and in implication defined above, " mainly comprise CO 2" something or other.
The inventor confirmed by with rich CO 2The primary flow body heat exchanges and carries out cooling off to small part first of process fluid is favourable.This advantage is the cold that they contain is recovered and has reduced the demand of extra cold energy, and wherein this extra cold energy provides by one or more kind of refrigeration cycle usually.The described rich CO of this hypothesis part 2Elementary fluid gasifies and causes just in order to transport described rich CO 2Fluid and/or be injected into subsoil and the extra cost of the compression carried out.
According to circumstances, the inventive method can comprise one or more following features:
-described step b) is at the feasible CO that is contained in the described process fluid 2Dividing potential drop is less than or equal to CO 2Carry out under the stagnation pressure of three phase point pressure, described stagnation pressure is preferably near atmospheric pressure.
-described step c) is at CO 2More than the three phase point pressure, preferably near carrying out under its stagnation pressure.
The liquefaction that-step c) comprises is introduced by the described solid of near small part and is mainly contained CO 2Liquid bath in and from described liquid bath, extract at least a rich CO 2Primary liquid obtains.
-described liquid bath heats by one or more following methods:
● by described fluid is mixed with described liquid bath with the fluid thermal exchange;
● by with rich CO 2Secondary fluid heat exchange and described secondary fluid is mixed with described liquid bath is wherein with described rich CO 2Secondary fluid is used for heating the described liquid bath that circulates in the closed-loop path and by heating with described process fluid heat exchange; And/or
● by with rich CO 2Described liquid bath is introduced and sneaked into to secondary fluid.
-to the described rich CO of small part 2Elementary fluid is by described rich CO 2Primary liquid obtains by one or more following methods:
● be higher than CO 2The pressure of three phase point pressure expands down to produce fluid; And/or
● be compressed to one or more CO of being higher than 2The stress level of three phase point pressure.These stress levels of part can make CO 2Dividing potential drop is higher than CO 2Critical-point pressure.Therefore, this fluid is false liquid (pseudo-liquid state).
-to the described rich CO of small part 2Elementary fluid comprises liquid phase and to the described rich CO of small part 2Elementary fluid pass through described heating and gasifying with the heat exchange of described process fluid to this liquid phase of small part.
-by with the heat exchange of described process fluid to the described rich CO of small part 2In the described heating process of elementary fluid, described rich CO 2Elementary fluid is one of at least still for liquid phase or be false liquid.False liquid state is defined as CO 2Dividing potential drop is higher than critical pressure and temperature is included between setting temperature and the critical point temperature.
-in step a), carry out described first be cooled to small part by obtaining with the central fluid heat exchange, this central fluid with to described one or more the rich CO of small part 2The cold exchange of elementary fluid.
-by with described process fluid heat exchange heating after, the described rich CO of near small part 2Elementary fluid is compressed to one or more CO of being higher than 2The stress level of supercritical pressure.
Above-mentioned " liquid bath " can be contained in the container.Usually be included in-50 ℃ to CO 2Between the three phase point temperature (56.6 ℃), preferred-55 ℃ to-56.6 ℃ temperature.The liquid CO that it is mainly obtained by the increase (mounting) of the described solid that obtains by cryogenic condensation 2Constitute.The stagnation pressure of the above operation of liquid bath is greater than or equal to CO 2Three phase point pressure is preferably near the latter.With rich CO 2Primary liquid extracts by suitable method from this bath.
The temperature of the solid in this liquid bath of impouring is lower than this bath temperature, therefore must heat this bath to keep this temperature and to guarantee that this solid melts.This heating can be carried out in every way, and by exchanging with one or more other fluid thermal, it is undertaken by mediate contact rather than mixing usually.
According to a particular, heat exchange can be by being higher than one or more temperature the rich CO of this bath temperature 2Fluid is introduced in this liquid bath and is undertaken by direct contact.Described heat exchange by directly contact is more effective than indirect exchange usually.This moment is a little than the rich CO of this liquid bath heat 2Fluid gets final product.This has limited irreversibility and has improved process efficiency.
The liquid itself of bathing by the indirect exchange heating liquid cools off.Therefore it can be used for the process for cooling fluid.By this way, the cold energy that is added liquid bath by the solid from low temp compensating can have value at least partially in other places of this method, especially for first cooling of this process fluid.Therefore improved gross efficiency.
According to a particular, several rich CO 2Fluid produces under different pressures.After the exchange, this allows the amount of conducting heat and recompresses rich CO 2The meticulous adjustment of the required energy of elementary fluid.Rich CO 2The low pressure of fluid and evaporation help reclaiming cold energy, but make the cost squeeze of these products higher.
According to another particular, rich CO 2Heat exchange between fluid and the process fluid can be carried out via one or more central fluid, promptly should richness CO 2Fluid is given described central fluid with its part cold, and this central fluid is given process fluid with this cold then.
The invention still further relates to and be applicable to that industrial flue gas is to catch CO 2Method.
According to a particular, these flue gases also can be carried out preliminary treatment from the device of produce power (steam).
To understand the present invention better when reading following nonrestrictive explanation and embodiment.They are with reference to the following drawings:
-Fig. 1 schematic representation adopt the CO of the inventive method 2Capture unit and
-Fig. 2 schematic representation the inventive method based on the use in the TRT of coal.
Device shown in Figure 1 is implemented step as described below.
-will in compressor 101, compress by the fluid 24 that flue gas constitutes, particularly compensate the pressure loss in each Device element of this unit.Notice this compression also can with the compression combination that is called as traction compression (draft compression) of the boiler that produces flue gas.It also can carry out between other steps of this method, or at CO 2Carry out in the downstream of separation method;
-compressed fluid 30 is injected filter 103 so that particle is reduced to 1mg/m 3Below, preferred 100 μ g/m 3Following concentration level;
-next, make dustless fluid 32 be cooled to temperature near 0 ℃, be generally 0-10 ℃, thus its steam of containing of condensation.This cooling is carried out in tower 105, moisture two-stage wherein, and cooling water 36 and temperature are injected near the water 34 of environment temperature.Also can be configured to mediate contact.This tower 105 can have or not have filler;
-fluid 38 delivered to for example use a kind of and/or other following method to eliminate the unit 107 of residual water vapor:
Zero adsorbs on fixed bed, fluid bed and/or rotary dryer, and wherein this adsorbent can be activated alumina, silica gel or molecular sieve (3A, 4A, 5A, 13X...);
Zero condensation in the interchanger of directly contact or mediate contact.
-then drying fluid 40 is introduced interchanger 109, it is approaching that fluid is cooled to, but be higher than CO in all cases 2The temperature of setting temperature.This temperature can be determined by the pressure of being familiar with process fluid 40 and the those skilled in the art that form.If the CO of process fluid 2Content be about 15 volume % and pressure near atmospheric pressure, then this temperature is about-100 ℃ approximately,
-the fluid 42 that will carry out first cooling 109 is then introduced containers 111, and continuing therein to be cooled to provides required CO 2The temperature of seizure level.Cryogenic condensation to small part is contained in the CO in the fluid 42 2Produce poor CO on the one hand 2Gas 44, generation mainly comprises CO on the other hand 2Solid 62.Gas 44 leaves container 111 with about-120 ℃ temperature.As CO 2The function of captured target level is selected this temperature.Under this temperature, the CO of gas 44 2Content is about 1.5 volume %, promptly by containing 15%CO 2The seizure level that begins of process fluid be 90%.The various technology that can be used in this container 111 are as follows:
Zero continuous solid body cryogenic condensation interchanger, wherein solid CO 2Form with dry ice produces, and for example use screw rod to extract, and pressurization is to be introduced into liquid CO 2Bathe in 121, obtain to be higher than CO therein 2The pressure of three phase point pressure.This pressurization also can be carried out in the warehouse system in batches.Continuous solid body cryogenic condensation itself can carry out with following variety of way:
■ surface scraping interchanger, its middle scraper for example is the extraction of screw form with the promotion solid,
■ fluid bed interchanger, thus carry dry ice and use as have each pipe of particle cleaning greater than the density of dry ice,
The ■ interchanger, solid extracts by vibrations, ultrasonic, pneumatic or heat effect (thereby intermittently heating makes the dry ice landing) therein,
■ assembles from the teeth outwards, and periodically " nature " falls into jar.
Zero solid cryogenic condensation in batches, at this moment, several interchangers in parallel can be used alternatingly.They separate then, are pressurized to be higher than CO 2The pressure of three phase point pressure, thereby fluidized solid CO 2And can make its partial gasification.
-then fluid 46 is heated in interchanger 109.Along with leaving of it, also fluid 48 can be used in particular for such unit of regenerating, be that it is used to eliminate residual vapor (107), and/or be used for producing cooling waters (115) at direct contact tower 115 by evaporation, directly introducing drying fluid 50 in the contact tower, use water saturation then, make its partial gasification;
-in container 111, carry out the required part cold of cryogenic condensation to provide by one or more cooling sources (75).Equally, first cooling, 109 required part colds provide by one or more cooling sources (76);
-will mainly comprise CO 2Solid 62 be transferred to liquid CO 2Bathe 121;
-thereby thereby this bath 121 needs heating remain the interpolation (latent heat of fusion and sensible heat) of liquid compensation from the cold of solid 62.This can carry out in every way:
Zero by with than hot fluid 72 heat exchanges.Cold energy from fluid 74 can be used in other places of this method,
Zero by directly exchange, for example by releasing from the fluid 80 of bathing 121, it is heated in interchanger 109, and it is annotated back bath 121 again;
-will mainly comprise CO 2Liquid 64 emit from bathing 121.
-this liquid is divided into three bursts of materials flows.In each example, first by expanding 65 to 5.5 crust (definitely) and produce two-phase, solution-air, fluid 66 acquisitions.The second, 68 by compression 67, for example to 10 crust acquisitions.With the three, 70, compression is for example to 55 crust.This 5.5 crust level provides and has been near CO 2The cold of the temperature of three phase point temperature.This 10 crust level makes in the evaporation latent heat transfer of-40 ℃ of following fluids 68 approximately.At last, under 55 crust, fluid 70 does not gasify in the process of exchange 109.Effectively use the cold energy that in the process of exchange 109, is contained in the fluid 64, and restriction produces CO simultaneously 2Purification and the required energy of compressed stream 5;
-after exchange 109, use compressor 131,132,133 to be compressed to elementary fluid 66,68,70 greater than CO 2The stress level of critical pressure.
Fig. 2 has described the device by coal power generation, adopts each unit 4,5,6 and 7 with purification flue gas 19.
Main air-flow 15 makes coal 15 pulverize the burner that also carries together to boiler 1 by unit 3 therein.Secondary airflow 16 is directly used in burner thereby the coal required other oxygen that almost completely burns is provided.Feed water 17 is delivered to boiler 1 to produce steam 18, and it expands in turbine 8.
To and comprise nitrogen, CO by the burning gained 2, steam and other impurity flue gas 19 carry out various processing to remove some described impurity.NOx is for example removed by catalysis in unit 4 in the presence of ammoniacal liquor.Unit 5 for example uses electrostatic filter to remove dust, and unit 6 is for removing SO 2And/or SO 3Desulphurization system.Depend on required product composition, it is unnecessary that unit 4 and 6 can be.To deliver to the cryogenic condensation purifier units 7 of low temperature to produce purer CO from the purification materials flow 24 of unit 6 (or 5, if 6 non-existent words) then 2The residual materials flow 25 of materials flow 5 and rich nitrogen.This unit 7 also is called as CO 2Capture unit and for example implement the inventive method as shown in Figure 1.
Therefore major advantage of the present invention is:
-reduced and separated and compression CO 2Power consumption,
-can adjust it to be fit to various operation constraints, particularly just wherein to obtain CO 2Pressure, availability and cryogenic condensation separate the cost of required cold energy.

Claims (10)

1. one kind by containing CO 2With at least a CO that compares 2The process fluid (40) that has more volatile compound is produced at least a poor CO 2Gas (44) and one or more rich CO 2The method of elementary fluid (66,68,70), it implements the following step:
A) do not change by heat exchange state described process fluid (40) first the cooling (109);
B) in step a), cool off to the described process fluid of small part (42) second the cooling (111) to obtain at least a CO that mainly contains 2Solid (62) and described at least poor CO 2Gas (44); With
C) comprise and liquefy to the described solid of small part (62) and make it possible to obtain described one or more rich CO 2The step (121) of elementary fluid (66,68,70);
Described method be characterised in that in step a), carry out described first the cooling (109) to small part by the heating (109) to described one or more the rich CO of small part 2Elementary fluid (66,68,70) obtains.
2. the method for claim 1 is characterized in that described step b) (111) is at the feasible CO that is contained in the described process fluid (42) 2Dividing potential drop is less than or equal to CO 2Carry out under the stagnation pressure of three phase point pressure, described stagnation pressure is preferably near atmospheric pressure, and described step c) (121) is at CO 2More than the three phase point pressure, preferably near carrying out under its stagnation pressure.
3. method as claimed in claim 2, it is characterized in that step c) comprises to introduce by the described solid of near small part (62) mainly contains CO 2Liquid bath (121) in and from described liquid bath (121), extract at least a rich CO 2The liquefaction that primary liquid (64) obtains.
4. method as claimed in claim 3 is characterized in that described liquid bath (121) heats by one or more following methods:
-by described fluid (72,74) is mixed with described liquid bath (121) with fluid (72,74) heat exchange;
-by with rich CO 2Secondary fluid (72,74) heat exchange and described secondary fluid (72,74) is mixed with described liquid bath (121) is wherein with described rich CO 2Secondary fluid (72) is used for heating the described liquid bath (121) that circulates in the closed-loop path and is heated by the heat exchange (109) with described process fluid (40); And/or
-pass through rich CO 2Described liquid bath (121) is introduced and sneaked into to secondary fluid (81).
5. as claim 3 or 4 described methods, it is characterized in that to the described rich CO of small part 2Elementary fluid (66,68,70) is by described rich CO 2Primary liquid (64) obtains by one or more following methods:
-be higher than CO 2Expansion under the pressure of three phase point pressure (65) is to produce fluid (66); And/or
-compression (67,69) is to one or more CO that are higher than 2The stress level of three phase point pressure (68,70).
6. as each method among the claim 1-5, it is characterized in that to the described rich CO of small part 2Elementary fluid (66,68) comprise liquid phase and by with the heat exchange of described process fluid (40) carry out to the described rich CO of small part 2The described heating (109) of elementary fluid (66,68) is gasified to this liquid phase of small part.
7. as each method among the claim 1-5, it is characterized in that by with the heat exchange of described process fluid (40) carry out to the described rich CO of small part 2In described heating (109) process of elementary fluid (70), at least a described rich CO 2Elementary fluid (70) remains liquid phase or is false liquid.
8. as each method among the claim 1-7, it is characterized in that described first cooling (109) to the small part of carrying out obtains by the heat exchange with central fluid in step a), this central fluid with to described one or more the rich CO of small part 2The cold exchange of elementary fluid (66,68,70).
9. as each method among the claim 1-8, it is characterized in that by with the heat exchange heating (109) of described process fluid (40) afterwards, the described rich CO of near small part 2Elementary fluid (66,68,70) compression (131,132,133) is to one or more CO that are higher than 2The stress level of supercritical pressure.
10. as each method among the claim 1-9, it is characterized in that it is used for industrial flue gas to catch CO 2
CN200980151178.3A 2008-12-19 2009-12-14 Carbon dioxide recovery method using cryo-condensation Expired - Fee Related CN102257342B (en)

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FR0858872 2008-12-19
FR0858872A FR2940414B1 (en) 2008-12-19 2008-12-19 PROCESS FOR CAPTURING CARBON DIOXIDE BY CRYO-CONDENSATION
PCT/FR2009/052505 WO2010076463A1 (en) 2008-12-19 2009-12-14 Carbon dioxide recovery method using cryo-condensation

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CN108956232B (en) * 2018-08-03 2021-03-30 中国核动力研究设计院 Sample preparation method and sample preparation equipment for carbon-14 in biological sample

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WO2010076463A1 (en) 2010-07-08
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US20110252828A1 (en) 2011-10-20
FR2940414A1 (en) 2010-06-25

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