CN102351147B - Moderate temperature pressure swing adsorption method for CO2, H2S and H2 mixed gas separation - Google Patents
Moderate temperature pressure swing adsorption method for CO2, H2S and H2 mixed gas separation Download PDFInfo
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- CN102351147B CN102351147B CN2011101996459A CN201110199645A CN102351147B CN 102351147 B CN102351147 B CN 102351147B CN 2011101996459 A CN2011101996459 A CN 2011101996459A CN 201110199645 A CN201110199645 A CN 201110199645A CN 102351147 B CN102351147 B CN 102351147B
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- 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
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- 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
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Abstract
The invention discloses a moderate temperature pressure swing adsorption method for CO2, H2S and H2 mixed gas separation, and belongs to the technical field of clean energy. The method of the invention conducts raw material gas separation under a moderate temperature without cooling and can recover raw material gas sensible heat, raise integral system heat efficiency, reduce system heat exchange equipment and lower system costs. Moderate temperature operation of the invention can effectively enhance adsorbent kinetics characteristics of adsorption and desorption and increase gas processing capability of the PSA system; meanwhile, simultaneous removal of CO2 and H2S components in the raw material gas is realized to reduce system equipment and system complexity; when the raw material gas only contains CO2 or H2S, individual removal of the CO2 or H2S from the raw material gas can be realized.
Description
Technical field
The invention belongs to the clean energy technology field, be specifically related to a kind of for CO
2, H
2s and H
2the middle temperature pressure swing absorption process that mixed gas separates.
Background technology
At present existing multiplely can pass through H
2s, CO
2segmentation removes and realizes CO
2/ H
2the traditional technology route separated, be mainly normal temperature or low temperature wet method (as Selexol/NHD technology, active MDEA technology, low-temperature rectisol technology) and pressure swing adsorption (PSA), above technology is able to widespread use in the energy, chemical industry.Selexol/NHD technology, low-temperature rectisol technology and active MDEA technology general designation solvent absorption are the decarbonization methods of maturation application.Active MDEA technology is chemical absorption method, and its principle is: MDEA liquid is in absorption tower and CO
2after chemical reaction occurs, CO
2be absorbed in solvent and form rich solution, rich solution enters the desorption tower thermal degradation and goes out carbonic acid gas, and absorption hockets with desorb, thereby realizes the Separation and Recovery of carbonic acid gas; Selexol/NHD technology and low-temperature rectisol technology are the physical absorption method, principle is to utilize the solubleness of each component in solvent along with the principle of pressure, temperature variation is separated, thereby reach the purpose of separating treatment carbonic acid gas, chemical reaction does not occur in whole absorption process, thereby the energy consumed is fewer than chemical absorption method.The common issue with that NHD, active MDEA and low-temp methanol washing process exist is that absorption temperature is low, solvent is expensive, desulfurization and decarburization need arrange and independently absorb and regeneration system rapidly, these wet method decarbonization process flow process complexity, facility investment and power consumption increase, and the maintenance and operation expense increases.
Pressure-variable adsorption (Pressure Swing Adsorption, PSA) the ultimate principle of technology utilizes the difference of gaseous fraction characterization of adsorption on solid porous sorbent material and adsorptive capacity with the characteristic of change in pressure, realizes separation or the purification of gas by periodic pressure conversion process.The product separated as required in absorption or non-adsorbed state, can be divided into Adsorption Phase product and fluid phase product in adsorption bed.For example, the synthetic gas of the industries such as gasification, gasifying biomass, petrochemical industry, Sweet natural gas, the composition of conversion gas there are differences because raw material is different, and its essentially consist mainly comprises: CO
2, CH
4, CO, O
2, N
2, H
2, H
2s, H
2o etc.In said components, common H
2o, CO
2, H
2s is strong absorbed component, CH
4, the CO adsorptive power is placed in the middle, O
2, N
2weak absorbed component, and H
2absorption hardly.Usually, in PSA, use a plurality of adsorption towers that are filled with sorbent material.Import unstripped gas in each adsorption tower, by repeatedly carrying out absorption process, decompression operation, desorption operation and the operation of boosting, obtain the product gas as object.The principle that obtains purpose gas is described below: if import the pressure of the unstripped gas in adsorption tower, uprise, the dividing potential drop that is included in the eliminating gas in unstripped gas also uprises, its result, get rid of gaseous constituent and be filled in the sorbent material absorption (from unstripped gas, removing some gaseous constituent) in adsorption tower, discharge gas in tower under this state, obtain getting rid of the goods gas that gaseous constituent is few, after this, with the adsorption tower internal pressure, reduce, or purge with non-adsorbed gas, get rid of gaseous constituent from sorbent material desorption (adsorbent reactivation), the composition of desorption becomes to be divided into non-adsorptivity purpose gas with other, the sorbent material of regeneration can be further used for removing from the unstripped gas of new importing gets rid of gaseous constituent, the sorbent material used in each adsorption tower need maybe should be removed gaseous species according to the purpose gaseous species and select, for example, if in order to remove CO from unstripped gas
2, obtain H
2goods gas, select gac, adsorbent of molecular sieve usually.
At present, the PSA gas separating method has been widely used in the CO in baking tail gases, lime-kiln gas in Sweet natural gas, coal firing boiler stack gas, synthetic-ammonia transformation gas, alumina producing
2remove and the field such as recovery, the shortcoming such as the method has overcome complicated operation in wet method decarburization, desulfurization, energy consumption is high, expense is high, equipment corrosion is large.But traditional PSA adsorption separation process sorbent suspension and equipment work condition restriction, often can only select normal temperature operation (as 20-45 ℃), need to first reduce gas temperature, cause the waste of unstripped gas sensible heat, the regeneration energy consumption is large, and the ratio that steam, power consumption account for respectively total operating cost is higher.Simultaneously, common PSA sorbent material (as molecular sieve) is for H
2the existence of O is also very responsive, at H
2in the situation of O and other gas coexistences, can preferentially optionally absorb H
2o therefore often need to increase the gas drying link in adsorption separation system, has increased facility investment, has also caused the loss of water vapour.In addition, traditional C O
2/ H
2separating technology adopts H
2s, CO
2segmentation removes, and has increased system complexity and cost of investment.
Summary of the invention
The object of the present invention is to provide a kind of for CO
2, H
2s and H
2the middle temperature pressure swing absorption process that mixed gas separates.
A kind of for CO
2, H
2s and H
2the middle temperature pressure swing absorption process that mixed gas separates successively by two or more adsorption towers, completes desulfurization, decarburization, recovery H by unstripped gas in adsorption tower
2process, each adsorption tower comprises following steps in one-period:
(1) pressurising
The unstripped gas or the gas product that by temperature, are 200-450 ℃ are boosted to adsorption tower, to adsorptive pressure 0.01-30MPa;
(2) absorption
Unstripped gas is sent into to adsorption tower from the adsorption tower bottom, the component CO easily adsorbed in adsorption tower
2and H
2in the S quilt, warm sorbent material is selected absorption, is difficult for the gas H of absorption
2, H
2o and N
2by whole adsorption tower bed, from outlet, discharge; When absorb leading-edge moves to the certain position of bed, stop adsorption operations;
(3) gas product reclaims
Discharge gas product from another pipeline of gas product end, along with gas product is constantly discharged, the bed internal pressure constantly descends, and when the adsorbed gas forward position is advanced to certain position, stops reclaiming product;
(4) all press
Adsorption tower product end Exhaust Gas, this part gas is used to another to complete the desorption process adsorption tower and boosts;
(5) forward bleed off pressure
Continue to emit gas along the absorption direction, return to the unstripped gas system; If, when gas product recycling step yield is larger, when pressure equalizing finishes, the tower internal pressure has been down to the low pressure of pressure-variable adsorption, system is without this step;
(6) reverse bleeding off pressure
Discharge in the other direction gas in adsorption tower along absorption, reduce pressure, this part gas can return to the unstripped gas system, or directly enters in addition and completed in the absorption tower of adsorbent reactivation;
(7) vacuum pump-down
When approaching normal atmosphere, adsorption tower is vacuumized to step-down when adsorption bed pressure;
(8) steam desorb
Pass into steam in adsorption tower, reduce the adsorbed gas dividing potential drop, realize adsorbent reactivation;
(9) rinse
By reverse bleeding off pressure, adsorption column pressure is down to normal pressure, for further reducing the impurity composition dividing potential drop, adopts the mode of rinsing sorbent material along venting, impurities partial pressure in adsorption tower is reduced, adsorbent reactivation is to the requirement of regulation.
Described unstripped gas comprises CO
2, CH
4, CO, O
2, N
2, H
2, H
2s and H
2o; Described gas product is mainly H
2.
Described sorbent material is seated in adsorption tower; The mixture that sorbent material is middle temperature sorbent material or middle temperature sorbent material and low temperature adsorbent, during mixture that sorbent material is middle temperature sorbent material and low temperature adsorbent in warm sorbent material account for the 2-100% of sorbent material total mass.
Hydrotalcite, the houghite of modification, Na that described middle temperature sorbent material is hydrotalcite, houghite, modification
2the Al that O modifies
2o
3or other can realize CO under 200-450 ℃ of condition
2, H
2the material of the adsorption and desorption of S; Described low temperature adsorbent is molecular sieve or gac.
Modification or unmodified hydrotalcite or houghite sorbing material can be expressed as following general type:
[M1
1-xM2
x(OH)
2][A
n-]
x-2·yH
2O·zM1
2(1-w)M3
wB
Wherein, M1 is Li
+, Na
+, K
+, Cr
+, Rb
+in monovalent cation or its mixture; M2 is Mg
2+, Ca
2+, Mn
2+, Fe
2+, Co
2+, Ni
2+, Zn
2+in divalent cation or its mixture; M3 is Al
3+, Cr
3+, Mn
3+, Co
3+, Ni
3+, La
3+in Tricationic or its mixture.[A
n-] be NO
3 -, SO
4 2-, CO
3 2-, Cl
-, Br
-, F
-, I
-; B is O
2-or CO
3 2-; N=1,2; X=0-1; Y=0-4; Z=0-7, this system typical material of r=0-1. is K
2cO
3the Mg-Al hydrotalcite of modifying.
Middle temperature sorbent material can also be modification or unmodified double salt sorbent material, and this double salt sorbent material is the salt that two or more positively charged ion and a kind of negatively charged ion form.Wherein, positively charged ion is from above-mentioned M1, and M2, select in M3, and negatively charged ion is from above-mentioned [A
n-], O
2-, CO
3-middle selection.This system typical material is MgO-K
2o double salt.
Beneficial effect of the present invention: carry out the unstripped gas separation under the medium temperature condition of 200～450 ℃, without cooling, can reclaim the unstripped gas sensible heat, improve entire system thermo-efficiency; Minimizing system heat-exchange equipment, reduce system cost; Middle temperature operation can effectively improve the attached dynamics of sorbent material Adsorption and desorption, can improve PSA system gas processing power; The present invention can realize CO in unstripped gas
2with H
2jointly removing of S component, can reduce system device, reduces system complexity.CO is only arranged in unstripped gas
2or H
2during S, also can realize removing separately CO from unstripped gas
2or H
2s.In the present invention, all press step to change according to the adsorption tower number change, can be 0-6 time.
The accompanying drawing explanation
Fig. 1 is four tower configuration CO
2, H
2s and H
2warm pressure swing adsorption system schematic diagram during mixed gas separates;
In figure, A, B, C and D respectively represent an adsorption tower.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
This example adopts four adsorption tower configurations, sees Fig. 1.Unstripped gas by utilidor, through high temperature resistant sequencing valve, is delivered to adsorption tower by the unstripped gas surge tank; Pressure-variable adsorption consists of 4 adsorption towers; Each adsorption tower needs experience absorption, 2 equal pressure drops, forward bleeds off pressure, reversely bleeds off pressure, rinses in a loop cycle, 2 equal voltage rises, rush totally 9 steps eventually.
Unstripped gas is the exit gas of typical gasification gas after shift-converter, and its component is:
Raw gas pressure: 2.7MPa
Unstripped gas temperature: 200-350 ℃,
Four adsorption column pressures are adjustable, and sorbent material is housed in adsorption tower, and sorbent material is by K
2cO
3mg-Al hydrotalcite and molecular sieve, the gac modified are composited, K
2cO
3the Mg-Al hydrotalcite of modifying accounts for the 2-100% of sorbent material total mass.
After unstripped gas enters adsorption tower, CO
2, H
2s etc. easily adsorbed gas are adsorbed the sorbent material absorption of loading in device, and hydrogen flows out adsorption tower; When the loading capacity of mixed fillers reaches set(ting)value, between adsorption tower, to automatically switch, the adsorption tower step-down of previous work enters the step-down reproduced state, and the adsorption tower of having regenerated enters adsorbed state through pre-loading to operating pressure again; The regeneration of adsorption tower is mainly according to the pressure difference, and the principle that the adsorptive capacity of adsorbate on mixed fillers is different, when reducing the pressure of adsorption tower, is attracted to the automatic desorption of impurity on mixed fillers, is excluded adsorption tower, and mixed fillers is realized regeneration.
The regeneration of adsorption tower comprises drop pressure, reverse step-down, rinses three states.Drop pressure refer to adsorption tower in the step-down reproduced state by the gas in adsorption tower all in pre-loading state and its low adsorption tower of pressure ratio, can effectively utilize like this residual air in adsorption tower, avoid, by its discharge system, causing waste, improve the rate of recovery; Reverse step-down refers to the adsorption tower in the step-down reproduced state, when its pressure is in all adsorption towers during minimal pressure, the part of this part residual gas is collected through backflow gas.
Be below the above pressure-swing adsorption process operation steps:
A. absorption
Unstripped gas enters from the adsorption tower bottom, and the impurity composition in unstripped gas is optionally adsorbed by multiple sorbent material.The hydrogen be not adsorbed goes the user as gas product.Obtained qualified gas product by this step.
B. desorb
1. all press
The sorbent material that completes adsorption process contains a large amount of impurity compositions, utilize sorbent material loading capacity under high pressure, low temperature large, low pressure, the characteristics that the high temperature adsorption capacity is little, by all pressures between adsorption tower, the working pressure that reduces sorbent material makes the impurity be adsorbed obtain the part desorb.
2. forward bleed off pressure
After completing pressure equalizing, direction along absorption is emitted the gas that a part of density of hydrogen is very high, source of the gas as another one in the rinse step adsorption tower, reduce the impurities partial pressure in purge column, purge column is regenerated, by suitable, put, the spontaneous pressure of adsorption tower decreases, and impurity obtains the part desorb.
3. reverse bleeding off pressure
After completing equal pressure drop process, certain pressure that adsorption tower generally all exists.At this moment, the impurity composition that adsorption tower is desorbed out is full of, and this partial impurities is emitted adsorption tower against the direction of absorption, by the inverse put process, makes adsorption column pressure approach normal pressure.
4. rinse
Be down to normal pressure by the inverse put adsorption column pressure, for further reducing the impurity composition dividing potential drop, adopt the mode of rinsing sorbent material along venting, impurities partial pressure in adsorption tower is reduced, adsorbent reactivation is to the requirement of regulation.
By the acting in conjunction of top three kinds of modes, the regeneration of sorbent material complete.
C. absorption is prepared
The absorption set-up procedure is mainly that adsorption column pressure is returned back to system pressure, and its Recovery Process generally is divided into
1. all press
By and complete between the adsorption tower of adsorption process the mode that adopts pressure in twos average, the pressure of the adsorption tower of regeneration is improved.Pressure equalizing is the process of boosting, and is also a process that reclaims dead space active principle in other adsorption towers simultaneously.
2. pressurising
By equal voltage rise, can only be that adsorption column pressure is necessarily raise, also there be certain difference in the pressure of itself and whole system, and this part difference is finally used gas product to carry out pressurising, and adsorption column pressure is risen to system pressure.
So far, single adsorption tower has completed a complete absorption-desorption circulation after experiencing above process, can start the adsorption process of new one-period, and other three adsorption towers are like this equally, and just each time step staggers mutually.One time loop cycle is 30 minutes, CO in unstripped gas
2decreasing ratio>90%, H
2s decreasing ratio>95%, product hydrogen purity>90%, products C O
2purity>90%.Whole process temperature be controlled between 250-350 degree centigrade in warm pressure-variable adsorption, complete assembly is selected corrosion-resistant withstand voltage material, all devices has Insulation.
Claims (3)
1. one kind for CO
2, H
2s and H
2the middle temperature pressure swing absorption process that mixed gas separates, is characterized in that, the unstripped gas that is 200-450 ℃ by temperature by two or more adsorption towers, completes desulfurization, decarburization, recovery H successively in adsorption tower
2process, each adsorption tower comprises following steps in one-period:
(1) pressurising
With unstripped gas or gas product, adsorption tower is boosted, to adsorptive pressure 0.01-30MPa;
(2) absorption
Unstripped gas is sent into to adsorption tower from the adsorption tower bottom, the component CO easily adsorbed in adsorption tower
2and H
2s is adsorbed agent and selects absorption, is difficult for the gas H of absorption
2, H
2o and N
2by whole adsorption tower bed, from outlet, discharge; When absorb leading-edge moves to the certain position of bed, stop adsorption operations; The mixture that described sorbent material is middle temperature sorbent material or middle temperature sorbent material and low temperature adsorbent, during mixture that sorbent material is middle temperature sorbent material and low temperature adsorbent in warm sorbent material account for the 2-100% of sorbent material total mass;
(3) gas product reclaims
Discharge gas product from another pipeline of gas product end, along with gas product is constantly discharged, the bed internal pressure constantly descends, and when the adsorbed gas forward position is advanced to certain position, stops reclaiming product;
(4) all press
Adsorption tower product end Exhaust Gas, this part gas is used to another to complete the desorption process adsorption tower and boosts;
(5) forward bleed off pressure
Continue to emit gas along the absorption direction, return to the unstripped gas system; If, when gas product recycling step yield is larger, when pressure equalizing finishes, the tower internal pressure has been down to the low pressure of pressure-variable adsorption, system is without this step;
(6) reverse bleeding off pressure
Discharge in the other direction gas in adsorption tower along absorption, reduce pressure, this part gas can return to the unstripped gas system, or directly enters in addition and completed in the adsorption tower of adsorbent reactivation;
(7) vacuum pump-down
When approaching normal atmosphere, adsorption tower is vacuumized to step-down when the adsorption tower internal pressure;
(8) steam desorb
Pass into steam in adsorption tower, reduce the adsorbed gas dividing potential drop, realize adsorbent reactivation;
(9) rinse
By reverse bleeding off pressure, adsorption column pressure is down to normal pressure, for further reducing the impurity composition dividing potential drop, adopts the mode of rinsing sorbent material along venting, impurities partial pressure in adsorption tower is reduced, adsorbent reactivation is to the requirement of regulation.
2. a kind of for CO according to claim 1
2, H
2s and H
2the middle temperature pressure swing absorption process that mixed gas separates is characterized in that described unstripped gas comprises CO
2, CH
4, CO, O
2, N
2, H
2, H
2s and H
2o; Described gas product is mainly H
2.
3. a kind of for CO according to claim 1
2, H
2s and H
2the middle temperature pressure swing absorption process that mixed gas separates, is characterized in that hydrotalcite, the houghite of modification, Na that described middle temperature sorbent material is hydrotalcite, houghite, modification
2the Al that O modifies
2o
3or other can realize CO under 200-450 ℃ of condition
2, H
2the material of the adsorption and desorption of S; Described low temperature adsorbent is molecular sieve or gac.
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| CN103101882A (en) * | 2013-01-09 | 2013-05-15 | 何巨堂 | Processing method of gas containing H2S, CO2, CH4 and H2 |
| CN103466546B (en) * | 2013-09-06 | 2015-04-15 | 清华大学 | Intermediate temperate pressure swing adsorption method for using bifunctional adsorbent in adsorption enhanced type vapor reforming and water-vapor transformation reactions |
| NL2013759B1 (en) * | 2014-11-10 | 2016-09-07 | Stichting Energieonderzoek Centrum Nederland | Improved process for removing and recovering H2S from a gas stream. |
| CN105413394B (en) * | 2015-12-25 | 2019-01-15 | 杨皓 | A method of combined using pressure swing adsorption technique from flue gas and produces sour gas and purity nitrogen |
| CN105858604B (en) * | 2016-03-31 | 2018-06-29 | 四川天采科技有限责任公司 | A kind of full temperature journey pressure swing adsorption method of enriched gas source removing hydrogen sulfide |
| CN107344058B (en) * | 2017-09-08 | 2023-05-26 | 成都盛利达科技有限公司 | Energy-saving hydrogen chloride gas deep purification process |
| CN108128754A (en) * | 2017-12-28 | 2018-06-08 | 上海华林工业气体有限公司 | A kind of System and method for for being easy to judge whether HyCO ice chests block |
| CN111375288B (en) * | 2018-12-27 | 2022-04-05 | 中国石油化工股份有限公司 | Memory, optimization method, device and equipment of pressure swing adsorption device |
| CN110124447B (en) * | 2019-06-11 | 2023-10-27 | 成都益志科技有限责任公司 | Pressure swing adsorption gas separation system and separation method for improving adsorption efficiency without energy consumption |
| CN111013536A (en) * | 2019-12-26 | 2020-04-17 | 清华大学 | Preparation of medium-temperature renewable hydrogen sulfide adsorbent and circulating desulfurization method thereof |
| CN112744788B (en) * | 2020-12-16 | 2022-09-23 | 四川天采科技有限责任公司 | Separation and purification method for deep dehydration and impurity removal of FTrPSA refined by anhydrous HF (hydrogen fluoride) produced by fluosilicic acid method |
| CN113830735B (en) * | 2021-11-23 | 2022-07-12 | 清华大学 | Medium-temperature purification hydrogen production method and equipment for reforming hydrocarbon fuel and fuel cell energy supply system |
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| CN1075741C (en) * | 1997-08-21 | 2001-12-05 | 成都新华化工研究所 | Pressure-variable adsorption method for extracting hydrogen from hydrogen-rich waste gas |
| CN1215624A (en) * | 1997-10-24 | 1999-05-05 | 化学工业部西南化工研究设计院 | Multi-bed vacuum pressure swing adsorption process for extracting hydrogen from hydrogen-contg. mixed gas |
| US6293998B1 (en) * | 1998-12-11 | 2001-09-25 | Uop Llc | Apparatus for use in pressure and temperature swing adsorption processes |
| CN1349841A (en) * | 2000-10-19 | 2002-05-22 | 四川华泰投资有限责任公司 | Pressure swing absorption process of separating relieved gas from methanol synthesis to prepare high-purity hydrogen and CO2 |
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