CN106693880B - A kind of calcium base CO2Adsorbent and preparation method thereof - Google Patents
A kind of calcium base CO2Adsorbent and preparation method thereof Download PDFInfo
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- CN106693880B CN106693880B CN201510788245.XA CN201510788245A CN106693880B CN 106693880 B CN106693880 B CN 106693880B CN 201510788245 A CN201510788245 A CN 201510788245A CN 106693880 B CN106693880 B CN 106693880B
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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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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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Abstract
The invention discloses a kind of calcium base CO2Adsorbent, including mass ratio are 1:9~1:1 Ca2MnO4And CaO, and Ca2MnO4Total mass fraction with CaO is 90%~99.9%, and the CaO is used for CO absorption2, the Ca2MnO4Uniform Doped is in the CaO, for enhancing CO2The anti-caking power of adsorbent, makes the CO2The cycle performance of adsorbent enhances, the calcium base CO2The grain size of adsorbent is less than 300 μm.The invention also discloses calcium base CO2The preparation method of adsorbent.Through the invention, it is prepared for a kind of Ca2MnO4Adulterate the calcium base CO of CaO2Adsorbent, the adsorbent adsorption capacity is strong, and anti-agglutinatting property is good, and preparation method is simple, has wide prospects for commercial application.
Description
Technical field
The invention belongs to CO2Sorbent material field, more particularly, to a kind of calcium base CO2Adsorbent and its preparation side
Method.
Background technology
In recent years, a large amount of uses of fossil fuel resulted in greenhouse gases CO2Excessive emissions, and then result in global change
A series of climatic issues such as warm.Therefore, emission reduction CO2The concern in worldwide is gradually caused.As one of which
CO after burning2Trapping technique, the calcium cyclic process raw material cheap and abundant by feat of its, higher theoretical adsorbance and very fast
The rate of adsorption the advantages that shown can the phase foreground.Calcium cyclic process passes through reversible reactionIt is real
Existing CO2Absorption and desorption.Adsorption process generally occurs at 650 DEG C or so, and desorption process is generally in the temperature higher than 900 DEG C
Lower realization.Since absorption is above CaCO with desorption temperature3Sintering temperature (Tamman's temperature：~533 DEG C), CaCO3With CaO crystalline substances
Body will be sintered, and then lead to the reunion of particle.Therefore, the specific surface area and porosity of adsorbent can all reduce.In this way, calcium
The absorption property of base adsorbent can be continuously decreased with the increase of cycle-index.For example, natural limestone cycle more than ten times after,
Conversion ratio can be reduced to 8%~9% or so.Therefore in the practical application of Ca-base adsorbent, it is necessary to fresh suction be continuously replenished
The attached dose of inactivation to avoid adsorbent increases the cost of investment and operating cost of adsorbent.
In order to solve or alleviate the deactivation prob of Ca-base adsorbent, it is exactly to adopt that current one kind, which having kind of an effective ameliorative way,
With new type natural calcium based mineral traditional natural limestone and white clouds are replaced to prepare the Ca-base adsorbent of doping inertia load
Stone.But at present the new type natural calcium mineral reported have the shortcomings that it is larger, for example, huntite (5th
International Symposium on Gas Cleaning at High Temperature.US DOE National
Energy Technology Laboratory, Morgantown,USA.“In situ gas conditioning in
Fuel reforming for hydrogen generation ") in the too low (CaCO of calcium content3·3MgCO3, active CaO content
About 30%), cause the adsorption capacity for calcining Ca-base adsorbent obtained to reduce, be unfavorable for the progress of adsorption process.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of calcium base CO2Its preparation of adsorbent
Method, its object is to prepare CO by raw material of calcimangite2Thus adsorbent solves the low technology of current material adsorption capacity
Problem.
To achieve the above object, according to one aspect of the present invention, a kind of calcium base CO is provided2Adsorbent, including quality
Than being 1:9~1:1 Ca2MnO4And CaO, and Ca2MnO4Total mass fraction with CaO is 90%~99.9%, and the CaO is used
In CO absorption2, the Ca2MnO4Uniform Doped is in the CaO, for enhancing the calcium base CO2The anti-sintering energy of adsorbent
Power makes the calcium base CO2The cycle performance of adsorbent enhances, the calcium base CO2The grain size of adsorbent is less than 300 μm.
Preferably, the Ca2MnO4Mass ratio with the CaO is 1:4~1:1.
Preferably, which further includes the oxide impurity that mass fraction is 0.1%~10%, the oxide impurity
Uniform Doped is in the CaO.
As it is further preferred that the oxide impurity is SiO2、MgO、Al2O3、SrO、K2One kind or more in O
Kind.
It is another aspect of this invention to provide that providing a kind of calcium base CO2The preparation method of adsorbent, including following step
Suddenly：
(1) it is ground to grain size after being crushed calcimangite and is less than 300 μm, obtains calcimangite particle；
(2) 700 DEG C~1200 DEG C calcinings in oxygen-containing atmosphere by the calcimangite particle obtained in the step (1), directly
To in the calcimangite calcium containing compound and be fully converted to CaO and Ca containing manganese compound2MnO4, i.e., described in acquisition
Calcium base CO2Adsorbent.
Preferably, which is characterized in that be ground to grain size after being crushed calcimangite in the step (1) and be less than 200 μm.
Preferably, calcination temperature is 800 DEG C~1000 DEG C in the step (2).
In general, through the invention it is contemplated above technical scheme is compared with the prior art, due to calcimangite
For raw material, following advantageous effect can be obtained：
1, make CO by raw material of calcimangite2The mass fraction of CaO has been increased to 50% or more in adsorbent, to make
Obtaining the adsorption capacity of adsorbent is enhanced；
2, since there are MnCO in calcimangite3And MnO etc. contains manganese compound so that the CO being prepared2In adsorbent
Contain a certain proportion of Ca2MnO4, to enhance CO2The anti-caking power of adsorbent, at 650 DEG C, circulation absorption 20 times with
On, still maintain the adsorption capacity of nearly original half；
3, preparation method of the present invention is simple, and material source is wide, of low cost, has extensive industrial prospect.
Description of the drawings
Fig. 1 is the EDS Surface scan figures of calcimangite, wherein 1a is calcimangite, and 1b is Ca elements, and 1c is Mn elements；
Fig. 2 is calcimangite and CO prepared by embodiment 12The XRD spectrum of adsorbent；
Fig. 3 is adsorbent in N2With circulation absorption performance map under oxygen-enriched calcination condition；
Fig. 4 is SEM figures before and after sorbent circulation, and wherein Fig. 4 a, 4b, 4c are respectively to show adsorbent in different calcining gas
Under atmosphere recycle before, N2SEM schemes after cycle and after oxygen-enriched atmosphere cycle；
Fig. 5 is circulation absorption performance of the adsorbent under different calcination temperatures.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The present invention provides a kind of calcium base CO2Adsorbent, including mass ratio are 1:9~1:1 Ca2MnO4And CaO, and
Ca2MnO4Total mass fraction with CaO is 90%~99.9%, and the CaO is used for CO absorption2, the Ca2MnO4Uniform Doped in
In the CaO, for enhancing the calcium base CO2The anti-caking power of adsorbent makes the calcium base CO2The cycle performance of adsorbent
Enhancing, wherein the chemical valence of Ca is divalent, and the chemical valence of Mn is 4 valences, the calcium base CO2The grain size of adsorbent is less than 300 μm；
The adsorbent further includes the oxide impurity that mass fraction is 0.1%~10%, and the oxide impurity Uniform Doped is in described
In CaO, the oxide impurity is SiO2、MgO、Al2O3、SrO、 K2It is one or more in O.
Wherein, Ca2MnO4With the mass ratio and Ca of CaO2MnO4With the total mass fraction of CaO mainly with as raw material
The ingredient of calcimangite is related, wherein Ca2MnO4Mass fraction it is higher, the cycle performance of adsorbent is stronger, and the quality of CaO
Score is higher, and the absorption property of adsorbent is stronger, the Ca2MnO4Mass ratio with the CaO is 1:4~1:When 1, adsorbent
Cycle performance and absorption property can reach best balance.
Calcimangite has output in China, Mexico, Britain, Brazil, France, the U.S. and Germany, wherein China
The ground such as the Inner Mongol, Hunan and Taiwan are the calcimangite place of production, and the ingredient of calcimangite and its place of production are closely related.When in selection
When the calcimangite of Mongolia is as raw material, the ingredient of adsorbent is mainly：56.3% CaO, 41.7% Ca2MnO4, 1%
MgO, 0.6%Al2O3, 0.4% SiO2。
Calcium base CO2The preparation method of adsorbent, includes the following steps：
(1) it is ground to grain size after being crushed calcimangite and is less than 300 μm, obtains calcimangite particle, for so that preparing
Obtained calcium base CO2The specific surface area of adsorbent increases, to improve its absorption property, if grain size is less than 200 μm, and adsorptivity
More preferably, however when too small (such as less than 50 μm) sintering of product can be aggravated, and then influence its cycle performance；
(2) 700 DEG C~1200 DEG C calcinings in oxygen-containing atmosphere by the calcimangite particle obtained in the step (1), directly
To calcium containing compound (such as CaCO in the calcimangite3) and (such as MnCO containing manganese compound3、MnO、Mn3O4Deng) in
Carbonate decomposition, and divalent manganese is oxidized to 4 valence manganese, to be fully converted to CaO and Ca2MnO4, that is, obtain the calcium base CO2
Adsorbent.And the time calcined is then related to the temperature of calcining, when calcination temperature is 900 DEG C, the time needs can react for 30 minutes
Completely, calcination temperature is too low, influences conventional efficient, excessively high, influences the anti-sintering property of product, and 800 DEG C of generally use~
1000 DEG C of calcination temperature is to take into account the two.
Embodiment 1：
(1) the natural blocky calcimangite that the place of production is the Inner Mongol is crushed, ground and is sized to 300 μm or less；
(2) the powdered calcimangite after screening is placed in Muffle furnace, in air atmosphere with the heating of 15 DEG C/min
Rate rises to 900 DEG C from room temperature, and 0.5h is then reacted at 900 DEG C, and doping Ca is obtained after cooling2MnO4Calcium base CO2Absorption
Agent.
Embodiment 2
Embodiment 1 is repeated with the same steps, difference lies in reaction temperature is 1000 DEG C in the step (2), instead
It is 25min between seasonable.
Embodiment 3
Embodiment 1 is repeated with the same steps, difference lies in reaction temperature is 1200 DEG C in the step (2), instead
It is 20min between seasonable.
Embodiment 4
(1) the natural blocky calcimangite that the place of production is Hunan is crushed, ground and is sized to 200 μm or less；
(2) the powdered calcimangite after screening is placed in Muffle furnace, in air atmosphere with the heating of 15 DEG C/min
Rate rises to 700 DEG C from room temperature, and 1h is then reacted at 700 DEG C, and doping Ca is obtained after cooling2MnO4Calcium base CO2Adsorbent.
Embodiment 5
(1) the natural blocky calcimangite that the place of production is Brazil is crushed, ground and is sized to 200 μm or less；
(2) the powdered calcimangite after screening is placed in Muffle furnace, with the heating of 15 DEG C/min under pure oxygen atmosphere
Rate rises to 800 DEG C from room temperature, and 40min is then reacted at 800 DEG C, and doping Ca is obtained after cooling2MnO4Calcium base CO2Absorption
Agent.
Analysis of experimental results：
EDS Surface scans have been carried out as former state to the calcimangite before being calcined in embodiment 1, as a result as shown in Fig. 2, can have been seen
Go out calcium constituent and manganese element in calcimangite original sample to be evenly distributed.
Fig. 2 is calcimangite and CO2The XRD spectrum of adsorbent, it can be seen that in calcimangite original sample mainly by Ca,
The carbonate of Mn forms, and the adsorbent prepared through calcining is mainly by CaO and Ca2MnO4It constitutes.To the calcimangite of embodiment 1
Raw material does XRD characterization, and the mass fraction of obtained each ingredient is as shown in table 1, wherein CaO, MnO, MgO, Al2O3And SiO2Point
Do not indicate that the oxide mass score to convert according to XRD characterization Ca, Mn, Mg, Al and element, mass loss solve for manganese side
Stone reduces the mass fraction of quality after firing.
Table 1
By table 1 it can be calculated that the calcium base CO being prepared2In adsorbent, the mass fraction of CaO is about 56.3%,
Ca2MnO4Mass fraction be about 41.7%, other impurity MgO, Al2O3And SiO2Total mass fraction be 2%.And combine figure
1 EDS characterization results it is found that preparation CO2In adsorbent, active constituent CaO and inertia load C a2MnO4It is evenly distributed,
Therefore evenly dispersed inertia load C a2MnO4It can be very good to play the role of metallic framework, enhance the anti-sintering energy of CaO
Power.
The CO that embodiment 2- embodiments 5 are prepared2Adsorbent is analyzed with same method, can be calculated
Go out, the CO being prepared2In adsorbent, Ca2MnO4Mass ratio with CaO is 1:9~1:1, and Ca2MnO4With the gross mass of CaO
Score is 90%~99.9%.
Circulation absorption/desorption process carries out in dual control temperature fixed bed.Weigh the adsorbent of the preparation of a certain amount of embodiment 1
It is positioned in quartz boat.Quartz boat is placed in adsorption zone 20min, temperature is 650 DEG C, and atmosphere is respectively 15vol.%CO2+
85vol.%N2(hereinafter simply referred to as N2Atmosphere) and 27vol.%O2+ 73vol.%CO2(hereinafter simply referred to as oxygen-enriched atmosphere),
Absorption is completed postcooling and is then weighed.Then, quartz boat is placed in desorption area 10min, temperature is 900 DEG C, and atmosphere is pure
N2.It waits after the completion of being desorbed, quartz boat is placed in adsorption zone again, carry out the survey of repeatedly absorption/de-adsorption cycle so on circulate
Examination.According to the quality weighed after the completion is adsorbed every time, each circulation absorption agent can be calculated in conjunction with initial adsorption agent quality
Conversion ratio.
Fig. 3 is the sorbent circulation absorption property figure, and abscissa is absorption/de-adsorption cycle number, and ordinate is that absorption turns
Rate.Wherein, square indicates N2The circulation absorption performance of atmosphere, circle indicate the circulation absorption performance of oxygen-enriched atmosphere, can see
Go out, in N2It adsorbs under atmosphere, adsorbent has shown good conversion ratio in 20 cyclic processes；When calcination atmosphere is changed into
When oxygen-enriched atmosphere, declining occurs in sorbent circulation absorption property, but still has good performance.Fig. 4 a, 4b, 4c are respectively
CO prepared by embodiment 12Adsorbent is before cycle, 20 N2After the sorption cycle of atmosphere and the absorption of 20 oxygen-enriched atmospheres follows
SEM pictures after ring.As can be seen that no matter in N2Under oxygen-enriched atmosphere, adsorbent is after it experienced 20 cycles, still preferably
Ground maintains the pattern of its script.
Table 2 is CO prepared by embodiment 12Specific surface area changes feelings before and after adsorbent recycles 20 times under different calcination atmospheres
Condition.It is as shown in the table, in N2After being recycled with oxygen-enriched calcination atmosphere, the specific surface area of adsorbent does not change substantially, illustrates adsorbent
With good anti-caking power.
Table 2
The adsorbent for weighing the preparation of a certain amount of embodiment 1 is positioned in quartz boat.Quartz boat is placed in adsorption zone
20min, temperature are 650 DEG C, atmosphere 15%CO2And 85%N2, adsorb and complete postcooling and then weighed.It then, will be quartzy
Boat is placed in desorption area 10min, and temperature is respectively 900 DEG C, 950 DEG C and 1000 DEG C, and atmosphere is pure oxygen-enriched calcination atmosphere (27%O2+
73%CO2).It waits after the completion of being desorbed, quartz boat is placed in adsorption zone again, carry out repeatedly absorption/desorption so on circulate and follow
The test of ring.Fig. 5 is the circulation absorption performance of the adsorbent that is prepared in embodiment 1 under different calcination temperatures.As can be seen that
When calcination temperature changes, there is not significant change, i.e., the adsorbent pair that prepared by the present invention in the circulation absorption performance of adsorbent
The variation of calcination temperature is insensitive in a certain range.The CO that embodiment 2- embodiments 5 are prepared2Adsorbent is with similarly
Method, which is analyzed, also can be obtained similar results.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (3)
1. a kind of calcium base CO2The preparation method of adsorbent, which is characterized in that include the following steps：
(1) it is ground to grain size after being crushed calcimangite and is less than 300 μm, obtains calcimangite particle；
(2) 700 DEG C~1200 DEG C calcinings in oxygen-containing atmosphere by the calcimangite particle obtained in the step (1), until institute
It states the calcium containing compound in calcimangite and is fully converted to CaO and Ca containing manganese compound2MnO4, that is, obtain the calcium base
CO2Adsorbent；
The calcium base CO2Adsorbent includes that mass ratio is 1:9~1:1 Ca2MnO4And CaO, and Ca2MnO4With the gross mass of CaO
Score is 90%~99.9%, and the CaO is used for CO absorption2, the Ca2MnO4Uniform Doped is in the CaO, for enhancing
The calcium base CO2The anti-caking power of adsorbent makes the calcium base CO2The cycle performance of adsorbent enhances, the calcium base CO2It inhales
Attached dose of grain size is less than 300 μm.
2. preparation method as described in claim 1, which is characterized in that ground after being crushed calcimangite in the step (1)
It is milled to grain size and is less than 200 μm.
3. preparation method as described in claim 1, which is characterized in that calcination temperature is 800 DEG C~1000 in step (2)
℃。
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| CN107321296B (en) * | 2017-07-18 | 2020-02-07 | 华东理工大学 | Composite MgO-based CO2Medium temperature adsorbent and preparation method thereof |
| CN109621891B (en) * | 2018-12-24 | 2020-08-18 | 华中科技大学 | Lithium-based CO2Adsorbent and preparation method thereof |
| CN111603902A (en) * | 2020-05-18 | 2020-09-01 | 武汉理工大学 | Magnesium chloride-based adsorbent and preparation method thereof |
| CN112604696A (en) * | 2020-11-20 | 2021-04-06 | 沪东重机有限公司 | Denitration catalyst for purifying tail gas of marine diesel engine and preparation method thereof |
| CN113318699B (en) * | 2021-01-28 | 2023-04-25 | 华中科技大学 | Method for reducing composite molten salt in adsorbent by adding high-activity ions |
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