CN102784630A - Preparation method for calcium-based CO2 sorbent - Google Patents

Preparation method for calcium-based CO2 sorbent Download PDF

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CN102784630A
CN102784630A CN2012102607359A CN201210260735A CN102784630A CN 102784630 A CN102784630 A CN 102784630A CN 2012102607359 A CN2012102607359 A CN 2012102607359A CN 201210260735 A CN201210260735 A CN 201210260735A CN 102784630 A CN102784630 A CN 102784630A
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calcium
presoma
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acid
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刘文强
徐明厚
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Huazhong University of Science and Technology
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Abstract

The invention provides a preparation method for a calcium-based CO2 sorbent. The preparation method comprises the following steps: mixing calcium precursor and an inert carrier precursor with a solvent so as to obtain a mixed solution containing the calcium precursor and the inert carrier precursor; stirring the mixed solution so as to allow the calcium precursor and the inert carrier precursor to be evenly mixed; then drying the mixed solution with a spray dryer so as to obtain a solid; and finally calcining the solid to obtain the calcium-based sorbent used for capturing CO2. The calcium-based CO2 sorbent prepared by using the method has good cyclic CO2 adsorption/desorption capacity and stability in cyclic adsorption/desorption of CO2 at a high temperature, is suitable for cyclic capture of CO2 at a high temperature, and has the characteristics of low energy consumption and small consumption of time.

Description

A kind of calcium base CO 2The preparation of adsorbent method
Technical field
The invention belongs to chemical field, relate to calcium base CO 2The preparation of adsorbent method, specifically relating to can be used for circulating under the high temperature catches CO 2Ca-base adsorbent.
Background technology
Calcium circulation CO absorption 2Process mainly utilize This reversible reaction.The positive reaction of this reaction is a carbonation reaction, and it is divided into two stages: be the surface chemical reaction stage early stage, and the later stage is the product layer DIFFUSION CONTROLLED stage.The back reaction of this reaction is calcining CaCO 3Process also is a CaO circular regeneration process.Calcium circulation CO absorption 2Be of wide application, its application comprises that carbon captures before the burning, burning back carbon captures and chemical heat pump etc.Such as, calcium circulation CO absorption 2Back capture CO is used to burn 2The time, the CO in the flue gas 2React in carbonation reactor with CaO (600～700 ℃), generate CaCO 3The CaCO that generates 3Carry circular regeneration CaO in calcination reactor (900 ℃), obtain the high concentration CO that can be used for sealing up for safekeeping simultaneously 2Calcium circulation CO absorption 2One of them major technology difficult point, promptly in carbonating/calcination cycle course of reaction because the high temperature of reaction atmosphere causes CaO/CaCO 3Sintering reduces specific area and pore volume, and the adsorption capacity that causes Ca-base adsorbent is along with cycle-index descends rapidly.
The method that present stage is alleviated this problem mainly contains: (i) calcining different calcium precursor to be to obtain to have the strong CaO of anti-caking power, (ii) aquation modification CaO, and inert carrier modification CaO (iii) mixes.Up to the present, be proved to be more than 10 kinds of effective doping method, the inert carrier of doping comprises Ca 12Al 14O 33, Ca 9A 16O 18, CaTiO 3, MgO, MgAl 2O 4, SiO 2, SBA-15 and cement etc.These doping methods generally comprise following step: (i) mix at least a calcium presoma, at least a inert carrier presoma and solvent (such as water, alcohol etc.); Obtain mixed solution (or suspension); (ii) adopt methods such as stirring, supersonic oscillations that calcium presoma and inert carrier presoma are mixed in solvent; (iii) the moisture in the evaporating liquid (or suspension) obtains solid mixture, and (iv) the calcining solid mixture obtains Ca-base adsorbent.
The circulation CO absorption of the modified calcium-based adsorbent of these method preparations 2Ability can obtain improvement in various degree basically.The general drying oven that uses of the 3rd step of these doping methods.Yet transpiring moisture is highly energy-consuming, time-consuming procedure in drying oven, so these methods are not suitable for industrial applications.
Summary of the invention
Task of the present invention provides a kind of calcium base CO 2The preparation of adsorbent method, the power consumption that exists in the prior art is high to overcome, the problem of length consuming time, can obtain solid mixture rapidly, reduces the energy consumption of preparation process, has promptly that energy consumption is low, the characteristics of weak point consuming time, and makes the calcium base CO with this method preparation 2Adsorbent has good circulation absorption/desorption CO 2Ability, and have at high temperature circulation absorption/desorption CO 2Stability, being applicable under the high temperature that circulation catches CO 2Characteristics.
Realize that technical scheme of the present invention is:
This calcium base CO provided by the invention 2The preparation of adsorbent method may further comprise the steps:
Step 1: be taken to less a kind of calcium presoma and at least a inert carrier presoma and solvent, obtain containing the mixed liquor of calcium presoma and inert carrier presoma;
Step 2: the mixed liquor that the method for employing agitator or supersonic oscillations obtains step 1 stirs or vibrates, and calcium presoma and inert carrier presoma are mixed;
Step 3: adopt spray dryer that the mixed liquor after handling through step 2 is carried out drying and obtain solids;
Step 4: the solids to step 3 obtains is calcined, and calcining heat is 700-1200 ℃, obtains being used for circulating under the high temperature catching CO 2Ca-base adsorbent.
Calcium presoma described in the above preparation method can but be not limited to be calcium oxide, calcium hydroxide, calcium carbonate, organic calcium salt or be the mineral matter of main component with the calcium containing compound; Described organic calcium salt can but to be not limited to be the L-calcium lactate; Calcium acetate; Maltonic acid calcium, calcium butyrate, calcium acetate, calcium stearate or calcium benzoate; Described with the calcium containing compound be main component mineral matter can but to be not limited to be lime, lime stone, calcite or dolomite.
Inert carrier presoma described in the above preparation method can but to be not limited to be cement, flyash, clay, metal oxide, metal hydroxides, metal carbonic acid thing or organic metal salt; Described organic metal salt can but to be not limited to be acetate, benzoate, acetate, butyrate, gluconate or stearate.
Solvent described in the above preparation method is water, ethanol, alcohol, gasoline, chloroform, acetone or organic acid, described organic acid can but to be not limited to be acetate, benzoic acid, acetic acid, butyric acid, gluconic acid or stearic acid.
In above-described preparation method; The mixed proportion scope of calcium presoma and inert carrier presoma is: make that the weight ratio of calcium oxide is 5%-95% in the final adsorbent; The weight ratio of inert carrier is 95%-5% in the final adsorbent, and the weight ratio that solvent accounts for solution is 5%-95%.
In above-described preparation method, described calcium presoma is a calcium acetate, and described inert carrier presoma is a magnesium acetate; Or described calcium presoma is the L-calcium lactate, and described inert carrier presoma is a magnesium acetate; Or described calcium presoma is maltonic acid calcium, and described inert carrier presoma is a maltonic acid magnesium; Or described calcium presoma is the nanoscale calcium oxide, and described inert carrier presoma is a cement; Or described calcium presoma is calcium hydroxide, and described inert carrier presoma is a cement.
In above-mentioned preparation method, the concrete service condition of spray dryer is that inlet temperature is 100-220 ° of C in the step 3, and suction pump is set to 10-50m 3/ h, peristaltic pump is set to 1.5-10ml/min, and the nozzle air current flow is 100-700l/h, in cyclone separator, collects and obtains solids.Calcining heat is 1100 ° of C of 6500 – in the step 4, and calcination time is more than or equal to 1 second, or is less than or equal to 12 hours.
The invention provides a kind of calcium base CO 2The preparation of adsorbent method; This preparation method comprises following step: (i) mix at least a calcium presoma, at least a inert carrier presoma and solvent; Obtain mixed solution (or suspension); (ii) adopt stirring, supersonic oscillations method that calcium presoma and inert carrier presoma are mixed, (iii) adopt spray-drying to obtain solid mixture rapidly, (iv) the calcining solid mixture obtains calcium base CO 2Adsorbent.Calcium base CO according to the inventive method preparation 2Adsorbent has circulation absorption/desorption CO at high temperature 2Stability.Therefore, this method is suitable for preparing being used for circulating under the high temperature and catches CO 2Calcium base CO 2Adsorbent.The present invention overcomes the power consumption height that exists in the prior art, the defective of length consuming time, the 3rd step of the inert carrier that also promptly mixes, and promptly the moisture in the evaporating liquid (or suspension) obtains solid mixture, the problem of power consumption height, length consuming time in this process.The present invention proposes to adopt spray drying process, thereby obtains solid mixture rapidly, reduces the energy consumption of dry run.The calcium base CO of the inventive method preparation 2Adsorbent has good circulation absorption/desorption CO 2Ability, wherein maltonic acid calcium and maltonic acid magnesium are that the result of adsorbent in the thermogravimetric appearance of presoma preparation shows that it can also remain on 0.46 gram CO after 44 circulations 2The adsorption capacity of every gram adsorbent.
Description of drawings
Fig. 1 is that preparation provided by the invention is used under the high temperature circulation and catches CO 2Calcium base CO 2The flow chart of adsorbent.
Fig. 2 is a Buchi Mini B-290 spray dryer sketch map.
Fig. 3 is powder solid thing mixture u-CG-MG-75, the adsorption desorption thermoisopleth of u-CG-MG-75-1 and u-CGMG-75-2 and BJH pore size distribution figure.
Fig. 4 is the wherein particle size distribution of three samples (CG-MG-75, CG-MG75-1 and CG-MG75-2) of sample.
Fig. 5 is the X-ray diffraction analysis of two samples (CH-CE75 and CaO160nm-CE-75) wherein.
Fig. 6 is the adsorbent absorption/desorption CO that in Cahn TG121 thermogravimetric appearance, circulates 2Test result.
Fig. 7 is the lengthening circulation absorption/desorption CO of sample CG-MG-75 in Cahn TG121 thermogravimetric appearance 2Test result.
Fig. 8 be sample CG-MG-75 before circulation with 44 circulations after the SEM image comparison.
The specific embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Embodiment 1
Press flow process shown in Fig. 1, at first select 5 kinds of calcium presomas:
Calcium hydroxide (calcium hydroxide, 96%, Ajax Finechem),
Maltonic acid calcium (calcium D-gluconate monohydrate, 98%, Sigma),
The L-calcium lactate (calcium L-lactate hydrate, 98%, Fluka),
Calcium acetate (calcium acetate hydrate, 99%, Sigma-Aldrich), and
Nanoscale calcium oxide (nanosized calcium oxide) (160nm, 98%, Aldrich).
Select 3 kinds of inert carrier presomas again:
Cement,
Magnesium acetate (magnesium acetate tetrahydrate,>99%, Amresco)
Maltonic acid magnesium (magnesium D-gluconate hydrate, 98%, Sigma).
As shown in table 1, select at least a calcium presoma and at least a inert carrier presoma, mix with water then.
Wherein, maltonic acid calcium, the L-calcium lactate, calcium acetate, magnesium acetate and maltonic acid magnesium are water-soluble acylate.
If what obtain after only adopting the water of these presomas and capacity to mix is solution.
If what obtained after having adopted calcium hydroxide or cement and water to mix is suspension.
Adopt the magnetic force heating stirrer to mix solution (or suspension), make calcium presoma and inert carrier presoma mix.
Next, adopt the Buchi Mini B-290 above-mentioned mixed solution of drying machine rapid draing (or suspension) as shown in Figure 2.The spray dryer service condition is as shown in table 1: inlet temperature is 200 ° of C, and suction pump is set to 100% work (38m 3/ h), peristaltic pump is set to 5-25 (1.5-7.5ml/min), and the nozzle air current flow is 421 or 541l/h (the nozzle spinner flowmeter elects 35 or 45 as).Solution (or suspension) is dispersed into vaporific drop through the compressed air ejection from second fluid nozzle.Drop contacts back moisture with high-temperature hot-air and evaporates rapidly in hothouse, obtain solid mixture.Solid mixture is collected in cyclone separator.The solid mixture of collecting is the homogeneous mixture of calcium precursor and inert carrier presoma.To this mixture calcining,, obtain a series of calcium base CO at last according to the difference of precursor 2Adsorbent (as shown in table 1).Illustrate: the implication of CA-MA-75 is: the calcium presoma of this adsorbent is a calcium acetate, and the inert carrier presoma is a magnesium acetate, adopts in the adsorbent that preparation flow shown in Figure 1 obtains, and the weight ratio of CaO is 75%.
In order to study the influence of the different service conditions of spray-drying,, when adopting different suction pump settings (25,15% and 5%), obtain corresponding solid mixture (u-CG-MG-75, u-CG-MG-75-1 and u-CG-MG-75-2) when other conditions are identical.As shown in table 2, the BET specific area of these solid mixtures records and is respectively 7.7227,8.1828and6.8367m 2/ g.In addition, as shown in Figure 3, their BJH pore size distribution is also similar.As shown in Figure 4, after calcining, the particles of powder size that obtains is also very similar: peak value is 10-12 μ m.
Table 1: according to the adsorbent of the inventive method preparation and in spray dryer the condition during operation:
Adsorbent is synthetic by different presomas, and the abbreviation implication is following: CA: calcium acetate, CL:L-calcium lactate; CG: calcium gluconae, CH: calcium hydroxide, CaO160nm: the nanoscale calcium oxide (160nm); CE: cement; MA: magnesium acetate, the MG:D-magnesium gluconate, 75: the weight ratio of CaO is 75% in the adsorbent.
Table 1:
Figure BDA00001932470400071
Table 2: the BET specific area of the solid mixture that in cyclone separator, obtains, abbreviation implication: u: calcined powder not, other are with table 1.
Table 2:
Figure BDA00001932470400072
As shown in Figure 5, when adopting cement to be the inert carrier presoma, contained element comprises CaO, Ca (OH) in the adsorbent 2And Ca 12Al 14O 33Because the final step of this preparation of adsorbent is calcining, this calcining heat (900 ℃) is far longer than Ca (OH) 2Decomposition temperature, so Ca (OH) 2Can think that in doing the XRD process moisture in the CaO absorbed air forms.It is the mixture of CaO and MgO that other three parts of adsorbents, (CA-MA-75, CL-MA-75 and CG-MG-75) are.
Next, circulation absorption/desorption CO in the test adsorbent Cahn TG121 thermogravimetric appearance 2Ability.Wherein, absorption (carbonating) reaction condition is: 650 ° of C, 30min, 15%CO 2The calcination reaction condition is: 900 ℃, and 10min, 100%N 2Test result is shown in Fig. 6 and 7.Wherein, (A) – (E) is a CaO conversion ratio time history plot to Fig. 6, and Fig. 6 (F) is that maximum CaO conversion ratio in each cyclic process is with the cycle-index variation diagram.As shown in, the circulation CO absorption of all adsorbents of the method preparation 2Ability all is better than CaO (the CaO conversion ratio after 22 circulations before the modification before the modification far away<20%).Wherein, adsorbent CG-MG-75 can also keep stable adsorption capacity after 22 circulation absorption/desorption CO2.Therefore, this sample is being carried out finding behind the further test experiments this adsorbent can also keep 45 circulations>80% CaO conversion ratio, see Fig. 7.In addition, shown in Fig. 7 (B), the circulation adsorption capacity of this adsorbent is far superior to not have the inertia load, promptly directly calcines the CaO adsorbent that maltonic acid calcium (calcium D-gluconate monohydrate) obtains.As shown in Figure 8, adsorbent CG-MG-75 before circulation with 44 circulations after the SEM image change very big, promptly from irregularly shaped (Fig. 8 A) to spherical form transformation (Fig. 8 B).

Claims (13)

1. calcium base CO 2The preparation of adsorbent method may further comprise the steps:
Step 1: be taken to less a kind of calcium presoma and at least a inert carrier presoma and solvent, obtain containing the mixed liquor of calcium presoma and inert carrier presoma;
Step 2: the mixed liquor that the method for employing agitator or supersonic oscillations obtains step 1 stirs or vibrates, and calcium presoma and inert carrier presoma are mixed;
Step 3: adopt spray dryer that the mixed liquor after handling through step 2 is carried out drying and obtain solids;
Step 4: the solids to step 3 obtains is calcined, and calcining heat is 700-1200 ℃, obtains being used for circulating under the high temperature catching CO 2Ca-base adsorbent.
2. preparation method according to claim 1 is characterized in that: described calcium presoma can but be not limited to be calcium oxide, calcium hydroxide, calcium carbonate, organic calcium salt or be the mineral matter of main component with the calcium containing compound.
3. preparation method according to claim 2 is characterized in that: described organic calcium salt can but to be not limited to be the L-calcium lactate, calcium acetate, maltonic acid calcium, calcium butyrate, calcium acetate, calcium stearate or calcium benzoate.
4. preparation method according to claim 2 is characterized in that: described with the calcium containing compound be main component mineral matter can but to be not limited to be lime, lime stone, calcite or dolomite.
5. preparation method according to claim 1 is characterized in that: described inert carrier presoma can but to be not limited to be cement, flyash, clay, metal oxide, metal hydroxides, metal carbonic acid thing or organic metal salt.
6. preparation method according to claim 5 is characterized in that: described organic metal salt can but to be not limited to be acetate, benzoate, acetate, butyrate, gluconate or stearate.
7. preparation method according to claim 1 is characterized in that: described solvent is water, ethanol, alcohol, gasoline, chloroform, acetone or organic acid.
8. preparation method according to claim 7 is characterized in that: described organic acid can but to be not limited to be acetate, benzoic acid, acetic acid, butyric acid, gluconic acid or stearic acid.
9. preparation method according to claim 1; It is characterized in that: the mixed proportion scope of calcium presoma and inert carrier presoma is: make that the weight ratio of calcium oxide is 5%-95% in the final adsorbent; The weight ratio of inert carrier is 95%-5% in the final adsorbent, and the weight ratio that solvent accounts for solution is 5%-95%.
10. preparation method according to claim 1 is characterized in that:
Described calcium presoma is a calcium acetate, and described inert carrier presoma is a magnesium acetate; Or
Described calcium presoma is the L-calcium lactate, and described inert carrier presoma is a magnesium acetate; Or
Described calcium presoma is a maltonic acid calcium, and described inert carrier presoma is a maltonic acid magnesium; Or
Described calcium presoma is the nanoscale calcium oxide, and described inert carrier presoma is a cement; Or
Described calcium presoma is a calcium hydroxide, and described inert carrier presoma is a cement.
11. preparation method according to claim 1; It is characterized in that; The concrete service condition of spray dryer is that inlet temperature is 100-220 ° of C in the step 3, and suction pump is set to 10-50m3/h, and peristaltic pump is set to 1.5-10ml/min; The nozzle air current flow is 100-700l/h, in cyclone separator, collects and obtains solids.
12. preparation method according to claim 1 is characterized in that, calcining heat is 6500-1100 ° of C in the step 4, and calcination time is more than or equal to 1 second, or is less than or equal to 12 hours.
13. preparation method according to claim 1 is characterized in that, the calcination reaction condition is in the step 4: 900 ℃, and 10min, 100%N 2
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