CN109395570A - A method of resistance to carbonating calcium-base absorbing agent is prepared using infusion process - Google Patents
A method of resistance to carbonating calcium-base absorbing agent is prepared using infusion process Download PDFInfo
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- CN109395570A CN109395570A CN201811484040.2A CN201811484040A CN109395570A CN 109395570 A CN109395570 A CN 109395570A CN 201811484040 A CN201811484040 A CN 201811484040A CN 109395570 A CN109395570 A CN 109395570A
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/40—Alkaline earth metal or magnesium compounds
- B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/602—Oxides
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- 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
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- General Chemical & Material Sciences (AREA)
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- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of methods for preparing resistance to carbonating calcium-base absorbing agent using infusion process, and CaO solid is milled into powder；In the isopropanol and distilled water that CaO powder is dissolved in together with nine water aluminum nitrates, stirring heating, obtained solid is milled into powder, powder is dissolved in isopropanol and distilled water together with nine water ferric nitrates again, stirring heating, obtained solid is milled into powder, then plus in right amount distilled water facilitates powder to be twisted into bead；Bead is calcined 4 hours, product is obtained.Its molecular formula is FexOy/CaO‑Ca12Al14O33, Cyclic Carbonation stability obviously optimized, cyclic absorption-release CO2Ability get a promotion.
Description
Technical field
The present invention relates to a kind of methods for preparing resistance to carbonating calcium-base absorbing agent using infusion process, belong to CO2Cyclic absorption-
Release tech field.
Background technique
Mankind's activity is considered as greenhouse gases CO2The main reason of discharge.Due to the aggravation of world industry process,
The burning of a large amount of fossil fuels, the destruction of forest cover and the fast development of modern agriculture make global CO2Concentration abruptly increase causes complete
Ball sea-level rise, freshwater resources are reduced, and extreme climate occurs, and human health is on the hazard, and the world's ecosystems are by tight
It destroys again.IPCC points out that, if global mean temperature was made to increase 2.0-2.4 DEG C relative to 2000 by 205 years, the whole world needs to reduce
About 50%~80% CO2 emissions, scientific and reasonable solution CO2Emission problem is extremely urgent.
CO2Trap (CO2Capture) refer to and the industries such as metallurgy, cement, electric power are utilized into generation during fossil fuel
CO2The process that gas is separated and is enriched with.According to CO2The difference of trapping technique feature, generally can be by CO2Trapping is divided into burning
(Post-combustion), pre-combustion capture (Pre-combustion), oxygen-enriched combusting trapping (Oxy-fuel are trapped afterwards
Combustion) three categories.Collecting carbonic anhydride and seal up for safekeeping (CCS) be energy demand extreme growth period to greenhouse gases into
One of the important measures of row science emission reduction.CO at present2Plugging Technology Applied mainly includes geological storage, ocean is sealed up for safekeeping and industrial carbon sequestration.
So-called industry carbon sequestration, i.e., to CO2Gas carries out carbonation cycle reaction.According to International Energy Agency (International
Energy Agency) prediction, to the year two thousand fifty, the whole world, which carries out energy-saving and emission-reduction by CCS, can reduce by about 19% greenhouse gases.
Calcium-base absorbing agent method is currently for CO2One of widely used technology of gas trapping.Its principle is to utilize
Absorbent containing calcium base carries out carbonation reaction under certain condition to reach and absorb CO2Purpose.Calcium-base absorbing agent absorbs
Capacity height, good absorption effect, high temperature resistant and calcium source are extensive in distributed in nature.
But common CaO absorbent has the following problems when utilizing: CaO need to undergo long-time Cyclic Carbonation-calcining
After reaction, carbonation reaction activity is significantly reduced, this further results in CaO absorbent trapping CO2The decline of performance.
Summary of the invention
It is an object of the invention to: after being directed to common CaO absorbent long-time Cyclic Carbonation-calcination reaction, carbonic acid
Changing reaction reactivity significantly reduces, and proposes a kind of preparation method, to effectively improve calcium base Cyclic Carbonation activity.
The technical solution adopted by the invention is as follows:
A method of resistance to carbonating calcium-base absorbing agent is prepared using infusion process, it is characterised in that: the following steps are included:
1) a certain amount of calcium acetate ((CH is taken3COO)2Ca·H2O) powder high temperature at 900 DEG C is forged 2 hours, and it is solid to obtain CaO
It is spare to be milled into powder for body；
2) by 1gCaO powder and nine water aluminum nitrate (Al (NO of 1.084g3)3·9H2O it) is dissolved in the isopropanol of 10ml together
In 50ml distilled water, mixed solution is placed in temperature and is set as on 75 DEG C of magnetic stirrer, and with the revolving speed of 300r/min
25min is stirred, until being completely dissolved, is then moved to solution in porcelain boat, it is 3 hours dry at 120 DEG C, by the solid after drying
It puts into Muffle furnace, 550 DEG C, and constant temperature 1 hour at 550 DEG C is warming up to the heating rate of 5 DEG C/mm, then continued with 5
DEG C/min is warming up to 1000 DEG C, and constant temperature 1 hour at 1000 DEG C from 550 DEG C, after temperature is reduced to room temperature, then from Muffle furnace
Middle taking-up；
3) obtained solid is milled into powder, then again by powder and nine water ferric nitrate (Fe (NO of 0.7215g3)3·
9H2O it) is dissolved in 20ml isopropanol and 225ml distilled water, mixed solution is placed on magnetic stirrer again together then,
Solution is then transferred to porcelain boat, is done at 120 DEG C up to being completely dissolved with 280r/min speed stirring 200min at 80 DEG C
Dry 2 hours；
4) solid obtained after drying is milled into powder, then plus in right amount distilled water facilitates powder to be twisted into partial size 3-4mm
Bead；
5) bead prepared is put into Muffle furnace and is calcined, Muffle furnace is warming up to the heating rate of 2 DEG C/mm by room temperature
900 DEG C, and calcined 4 hours at a high temperature of 900 DEG C, obtain product.
The product obtained afterwards by adopting the above technical scheme, molecular formula FexOy/CaO-Ca12Al14O33, recycle carbonic acid
Change stability obviously to be optimized, cyclic absorption-release CO2Ability get a promotion.
Detailed description of the invention
It is described in further detail below in conjunction with attached drawing and embodiments of the present invention
Fig. 1 is the circularly trapping CO of CaO, Ca-Fe, Ca-Al, Ca-Al-Fe2TGA result figure；Curve S1 is CaO, S2
For Ca-Fe, S3 Ca-Al, S4 Ca-Al-Fe；
Fig. 2 is the trapping performance map of the multicycle CO2 of Ca-Al-Fe；
Fig. 3 is the single-cycle thermogravimetric curve variation diagram of Ca-Al-Fe；
Fig. 4 is the thermogravimetric analysis variation diagram that Ca-Al-Fe absorbent controls the stage in multi-cycle carbonation kinetics；
Curve P1 is the 1st circulation, and P2, P3, P4 are the 5th, 10,15 circulation (recycling result overlapping several times), and P5 is the 20th circulation；
Fig. 5 is flow chart of the invention.
Specific embodiment
A kind of method preparing resistance to carbonating calcium-base absorbing agent using infusion process described in the present embodiment, including following step
It is rapid:
1) it takes a certain amount of calcium acetate ((CH3COO) 2CaH2O) powder high temperature at 900 DEG C to forge 2 hours, it is solid to obtain CaO
It is spare to be milled into powder for body；
2) 1gCaO powder and nine water aluminum nitrate of 1.084g (Al (NO3) 39H2O) are dissolved in the isopropanol of 10ml together
In 50ml distilled water, mixed solution is placed in temperature and is set as on 75 DEG C of magnetic stirrer, and with the revolving speed of 300r/min
25min is stirred, until being completely dissolved, is then moved to solution in porcelain boat, it is 3 hours dry at 120 DEG C, by the solid after drying
It puts into Muffle furnace, 550 DEG C, and constant temperature 1 hour at 550 DEG C is warming up to the heating rate of 5 DEG C/min, then continued with 5
DEG C/min is warming up to 1000 DEG C, and constant temperature 1 hour at 1000 DEG C from 550 DEG C, after temperature is reduced to room temperature, then from Muffle furnace
Middle taking-up；
3) obtained solid is milled into powder, then again by powder and nine water ferric nitrate of 0.7215g (Fe (NO3) 3
It 9H2O) is dissolved in 20ml isopropanol and 225ml distilled water, mixed solution is placed on magnetic stirrer again together then,
Solution is then transferred to porcelain boat, is done at 120 DEG C up to being completely dissolved with 280r/min speed stirring 200min at 80 DEG C
Dry 2 hours；
4) solid obtained after drying is milled into powder, then plus in right amount distilled water facilitates powder to be twisted into partial size 3-4mm
Bead；
5) bead prepared is put into Muffle furnace and is calcined, Muffle furnace is heated up with the heating rate of 2 DEG C/min by room temperature
It is calcined 4 hours to 900 DEG C, and at a high temperature of 900 DEG C, obtains product, molecular formula FexOy/CaO-Ca12Al14O33, it is denoted as
Ca-Al-Fe。
For the Fe obtained with above-mentioned technical proposalxOy/CaO-Ca12Al14O33(being denoted as Ca-Al-Fe) its to CO2Circulation is inhaled
It receives characteristic to be compared, also be prepared for following several with reference to absorbent:
A, the CaO for obtaining step 1) according to step 4), 5) the method balling-up, obtained sample is denoted as CaO；
B, step 1) and the sample 2) obtained according to step 4), 5) the method balling-up obtain CaO-Ca12Al14O33, it is denoted as
Ca-Al；
C, the nine water ferric nitrate (Fe (NO of the CaO and 0.7215g obtained step 1)3)39H2O it is different that it) is dissolved in 20ml together
In propyl alcohol and 225ml distilled water, then mixed liquor is placed on magnetic stirrer, with the stirring of 280r/min speed at 80 DEG C
To being completely dissolved, the solution after stirring is transferred to from beaker porcelain boat, porcelain boat is then put into baking by mixing time 200min
In case, sample dry 120min at 120 DEG C；, obtained sample obtains Fe according to step 4,5 balling-upxOy- CaO is denoted as Ca-
Fe。
Using the Cyclic Carbonation performance of thermogravimetric analyzer (TGA) detection absorbent, evaluation absorbent Cyclic Carbonation is anti-
A stable important indicator of answering property is whether the collecting carbonic anhydride performance during seeing its multi-cycle is stable.It " carbonates-forges
The atmosphere tested during burning " cyclic test is 25%CO2+ 75%N2, gas flow 250mL/min.Laboratory operating procedures are such as
Under:
A certain amount of absorbent is first weighed using electronic balance, is made a record；
A) empty crucible is put into thermogravimetric analyzer, manually resets weight, then pour into load weighted laboratory sample
In empty crucible, and it is put into instrument；
B) start to set temperature program.Temperature is first from room temperature (about 25 DEG C) with 25 DEG C of min-1Heating rate temperature programming arrive
720℃；
C) the constant temperature 30min at 720 DEG C；
D) with the heating rate of 20 DEG C/min from 720 DEG C of temperature programmings to 850 DEG C；
E) the constant temperature 10min at 850 DEG C；
F) from 850 DEG C with rate of temperature fall be 20 DEG C of min-1 program is cooled to 720 DEG C.
Step (b)-(f) is first time " carbonating-calcining " cyclic process of TGA, repeats step (c)-(f), carries out altogether
20 cyclic tests.
Fig. 1 illustrates the circularly trapping CO of CaO, Ca-Fe, Ca-Al, Ca-Al-Fe2TGA as a result, curve S1 be CaO,
S2 is Ca-Fe, S3 Ca-Al, S4 Ca-Al-Fe.It can be seen from the figure that in " carbonating/calcining " reaction, Ca-Al-
Trapping CO of the Fe absorbent in preceding several periods2Performance is most weak, first circulation CO2Uptake only has 0.26mg-CO2/
Mg- absorbent, but with the progress of reaction, Ca-Al-Fe absorbent begins to exceed other absorbents from the 9th circulation,
Strongest CO is presented in four kinds of absorbents2Absorbability.So Ca-Al-Fe absorbent all shows in 10 circular responses
Good Cyclic Carbonation stability out absorbs CO2Amount first gradually increase, and it is last stable in 0.3mg or so always.
Starting the stage of reaction, the CO of CaO2Assimilation effect is best, the CO in first circulation2Uptake is up to 0.65mg-
CO2/ mg- absorbent, but its Cyclic Carbonation activity rapidly reduces, after ten circulations, the CO of CaO absorbent2Absorb energy
Power is only 0.11mg-CO2/ mg- absorbent reduces 83% compared with first circulation.And it is just small since the 5th circulation
In Ca-Al-Fe absorbent, it can be seen that, the stability of CaO absorbent is particularly poor, and CaO is easy to appear when reason is that reaction
Sintering phenomenon.
Compare two curves of CaO and Ca-Al, although in starting several periods, the trapping CO of CaO2Ability is stronger, still
After the 4th period, discovery Ca-Al absorbent ratio CaO shows higher CO2Capture ability and stability, this is due to forging
During burning, Ca-Al absorbent is supported with inert material, can effectively prevent or the sintering of delayed absorber.
In order to study addition iron presoma to CO2The influence for trapping performance compares Ca-Al and two kinds of Ca-Al-Fe absorptions
The capture situation of agent.According to available in figure, the CO of Ca-Al and Ca-Al-Fe2Acquisition performance and stability suffer from difference
Not.In preceding several periods, Ca-Al obviously illustrates its stronger CO2Capture ability, and significantly it is higher than Ca-Al-
Fe.This shows that addition iron presoma, ferriferous oxide can then be evenly distributed in the surface of CaO, can effectively prevent in absorbent
CO2It is diffused into the gap structure of CaO, will be greatly reduced CaO and absorb CO2Ability, therefore, this is it can be understood that Ca-Al ratio
Ca-Al-Fe has stronger CO2Capture ability.But addition iron presoma also has benefit, ferriferous oxide is evenly distributed on
The surface of CaO, can substantially reduce the surface sintering of CaO, this stability for also explaining Ca-Al-Fe in figure well is better than
Ca-Al.The absorption CO of Ca-Al2Ability is recycled to the tenth from first and recycles the absorption CO for having dropped 35%, Ca-Al-Fe2Energy
The trend gradually increased is then presented in power.
In short, Ca-Al-Fe absorbent/catalyst has optimal cyclic carbon compared with Ca, Ca-Al, Ca-Fe absorbent
It is acidified stability, after 10 carbonating-calcination cycles, traps CO2Ability in four kinds of absorbents highest.
Fig. 3 illustrates the thermogravimetric curve variation of a circulation.For each " carbonating/calcining " cyclic process, all can
Three different stages are undergone, known to the circulation based on CaO absorbent: initial is the carbonation stages of fast chemical reaction,
Followed by the carbonation stages spread slowly, it is finally calcination stage.Fig. 2 illustrates the multicycle CO of Ca-Al-Fe2Catching
Can, according to left figure it can be found that Ca-Al-Fe absorbent traps CO with the increase of cycle-index2Ability slowly increasing,
Then maintain in a range.In the CO of the absorbent after 20 circulations2Trapping ability increases to 0.565 from 0.499, says
It is very stable that Ca-Al-Fe absorbent activity is illustrated, and with the increase of cycle-index, activity is more preferable instead.Illustrate Ca-
Easy in inactivation is not conducive to recycle Al-Fe absorbent.
The case where in order to more intuitively indicate Ca-Al-Fe absorbent multicycle kinetics, Fig. 4 is Ca-Al-Fe
Absorbent compares absorbent in carbonating rank in the thermogravimetric analysis variation diagram in multi-cycle carbonation kinetics control stage
Assimilation effect figure when section has chosen the 1st, 5,10,15,20 circulation respectively, and curve P1 is the 1st circulation, and P2, P3, P4 are
5th, 10,15 circulation (recycling result overlapping several times), P5 is the 20th circulation.From figure it can be found that with " carbonating-
The increase of calcining " cycle-index, fast reaction stage do not change, are held on a slope substantially, this phenomenon is advantageous
In the absorbent application in fluidized bed in the future.In the slow reaction stage, the trapping performance of carbon dioxide is with " carbonating-forge
Burn " increase of cycle-index and increase.
Claims (1)
1. a kind of method for preparing resistance to carbonating calcium-base absorbing agent using infusion process, it is characterised in that: the following steps are included:
1) a certain amount of calcium acetate ((CH is taken3COO)2Ca·H2O) powder high temperature at 900 DEG C is forged 2 hours, obtains CaO solid, will
It is spare that it is milled into powder；
2) by 1gCaO powder and nine water aluminum nitrate (Al (NO of 1.084g3)3·9H2O) be dissolved in together 10ml isopropanol and
In 50ml distilled water, mixed solution is placed in temperature and is set as on 75 DEG C of magnetic stirrer, and is stirred with the revolving speed of 300r/min
25min is mixed, until being completely dissolved, is then moved to solution in porcelain boat, it is 3 hours dry at 120 DEG C, the solid after drying is put
Into in Muffle furnace, 550 DEG C, and constant temperature 1 hour at 550 DEG C are warming up to the heating rate of 5 DEG C/min, then continue with 5 DEG C/
Min is warming up to 1000 DEG C, and constant temperature 1 hour at 1000 DEG C from 550 DEG C, after temperature is reduced to room temperature, then from Muffle furnace
It takes out；
3) obtained solid is milled into powder, then again by powder and nine water ferric nitrate (Fe (NO of 0.7215g3)3·9H2O) one
It rises and is dissolved in 20ml isopropanol and 225ml distilled water, then mixed solution is placed on magnetic stirrer again, at 80 DEG C
With 280r/min speed stirring 200min until being completely dissolved, solution is then transferred to porcelain boat, it is 2 hours dry at 120 DEG C；
4) solid obtained after drying is milled into powder, then plus in right amount distilled water facilitates powder to be twisted into the small of partial size 3-4mm
Ball；
5) bead prepared is put into Muffle furnace and is calcined, Muffle furnace is warming up to 900 by room temperature with the heating rate of 2 DEG C/min
DEG C, and calcined 4 hours at a high temperature of 900 DEG C, obtain product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116495762A (en) * | 2023-03-17 | 2023-07-28 | 浙江大学 | Calcium-based composite heat storage material and preparation method thereof |
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| WO2013024141A2 (en) * | 2011-08-16 | 2013-02-21 | Imperial Innovations Limited | Calcium sorbent doping process |
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| CN116495762A (en) * | 2023-03-17 | 2023-07-28 | 浙江大学 | Calcium-based composite heat storage material and preparation method thereof |
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Application publication date: 20190301 |