CN104785195A - Calcium oxide based high-temperature carbon dioxide adsorbent material doped with inert component and preparation method - Google Patents
Calcium oxide based high-temperature carbon dioxide adsorbent material doped with inert component and preparation method Download PDFInfo
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Abstract
The invention discloses a calcium oxide based high-temperature carbon dioxide adsorbent material doped with an inert component and a preparation method. The inert component is cerium oxide, and an active component for adsorbing carbon dioxide is calcium oxide. A calcium oxide based adsorbent is prepared with a sol-gel method, and cerium nitrate and calcium nitrate are precursors; citric acid is introduced, the mixture is sufficiently complexed in a water bath process, and calcium and cerium are uniformly dispersed; a large amount of gas is generated in a roasting process, and loose and porous morphology is formed. The material has the characteristics of excellent stability, high adsorption capacity, high molar conversion of calcium oxide and high adsorption rate when adsorbing carbon dioxide at the high temperature; the preparation process is simple, the cost is low, and the requirement for the preparation is lower; the adsorbent has a wider industrial application prospect when used for adsorbing carbon dioxide at the high temperature.
Description
Technical field
The invention belongs to a kind of calcium oxide-based high temperature carbon dioxide sorbing material and preparation method of inert component of adulterating.
Background technology
The excessive emissions of GHG carbon dioxide may be cause the main cause of global warming, and the burning of the fossil fuel that it is mainly used by power plant and carrier causes.In addition, because fossil fuel cost is lower, estimate that the discharge capacity of global carbon dioxide will increase further, therefore become the focus of research about the trapping of carbon dioxide.Employing solid absorbent absorbing carbon dioxide is a kind of mode of effective process carbon dioxide, adsorbent can be divided into low temperature adsorbent (<200 DEG C), middle temperature adsorbent (200-400 DEG C) and high-temperature adsorbing agent (>400 DEG C) according to the difference of adsorption temp, calcium oxide, as typical high-temp solid adsorbent, has great potential using value in process high temperature carbon dioxide.Calcium oxide wide material sources, can obtain from raw material roastings cheap and easy to get such as lime stones, cost is lower, for its commercial Application provides possibility.Calcium oxide is as carbon dioxide absorber, and adsorption capacity is higher, can reach 0.786gCO in theory
2/ gCaO.Meanwhile, calcium oxide has carbon dioxide adsorption speed faster, is adsorbable relatively large carbon dioxide in the short period of time.Therefore, absorption calcium oxide being applied to high temperature carbon dioxide is the inexorable trend of current era development.
But calcium oxide also exists obvious defect as high temperature carbon dioxide adsorbent, namely recycling less stable in process, along with the increase adsorption capacity of cycle-index obviously reduces, this is mainly because the sintering of adsorbent causes.Therefore need to change fresh adsorbent in time in application process, running cost is comparatively large, and investment increases, and the cheap limiting calcium oxide adsorbent uses.The domestic and international research to calcium oxide adsorbent at present mainly concentrates on the cyclical stability improving adsorbent, make the adsorbent prepared while adsorption capacity is high, have more excellent stability, adsorption capacity and cyclical stability are the topmost performance indications of calcium oxide adsorbent.
Report a variety of method to improve the cyclical stability of adsorbent at present, high-temperature heat treatment (Energy Fuels, 2009, 23 (3): 1437-1444), hydration-treated (Energy Fuels, 2011, 25 (3): 1294-1301), ethanolic solution modification (AIChEJournal, 2013, 59 (10): 3586-3593), preparation (the Environmental Science Technology of nano calcium oxide, 2010, 44 (8): 3093-3097), doping inert component (Journal of Physical Chemistry C, 2011, 115:24804-24812) etc., various method respectively has pluses and minuses above, needed for high-temperature heat treatment, energy consumption is higher, increase cost, modification or preparation nano material conventional method complexity, running cost is higher, is unfavorable for the suitability for industrialized production of adsorbent, preparation method is fairly simple for doping inert component, and easily operates, respond well to the raising of stability.When but inert component doping is too much, adsorption capacity can reduce, be unfavorable for the carrying out of adsorption process equally, be therefore applicable to the calcium oxide-based adsorbent of suitability for industrialized production by the method exploitation of doping, make it simultaneously have important content that higher adsorption capacity and good stability are research at present.
Summary of the invention
In the preparation of calcium oxide-based adsorbent, high-adsorption-capacity and excellent stability evaluate the leading indicator of adsorbent performance.Cerium oxide has higher Tamman's temperature, reaches about 1064 DEG C, it can be used as during doping component and not easily sinters, and effectively can play interval, support the effect of calcium oxide.Mainly concentrate at present the catalyst preparing of some catalyst system and catalyzing about the research of cerium oxide, it can be used as doping component to be applied to the research of calcium oxide-based adsorbent less.Therefore utilizing the high Tamman's temperature of cerium oxide and the feature of not easy-sintering, cerium oxide is incorporated into the cyclical stability improving adsorbent in calcium oxide-based adsorbent, making adsorbent show higher adsorption capacity by regulating calcium cerium mol ratio.The calcium oxide-based adsorbent of the doped cerium oxide that exploitation preparation is novel thus.
The present invention is devoted to adsorbent and the preparation method of the calcium oxide-based adsorbent high temperature adsorption carbon dioxide providing a kind of doped cerium oxide, for the deficiency of existing sorbent preparation method, the present invention prepares the calcium oxide-based adsorbent that a kind of cheap and easy to get, method is simple, be applicable to the doping inert component cerium oxide of suitability for industrialized production.By the control of preparation method, the adsorbent of acquisition has specific pattern, and absorption property is good, has higher carbon dioxide adsorption capacity and preferably cyclical stability.
Technical scheme of the present invention is as follows:
A calcium oxide-based adsorbent for inert component of adulterating, inert component is cerium oxide, and the active component of absorbing carbon dioxide is calcium oxide.
The preparation method of calcium oxide-based adsorbent of the present invention, adopt sol-gel process, step is as follows:
(1) using water as solvent, cerous nitrate and calcium nitrate are dissolved respectively, the mol ratio of calcium nitrate and cerous nitrate is 3 ~ 15:1;
(2) added by citric acid in the mixed solution of calcium nitrate and cerous nitrate, the molal quantity of citric acid and the ratio of metal ion total mole number are 2 ~ 3:1;
(3) be placed on Rotary Evaporators by mixed liquor, setting bath temperature is 60 ~ 80 DEG C, water bath time 3 ~ 5h;
(4) revolve after steaming is drained and mixture is put into baking oven drying, baking temperature is 100 DEG C;
(5) dried material is carried out roasting, obtain the calcium oxide-based adsorbent of doped cerium oxide.
In preferred steps (1), the mol ratio of calcium nitrate and cerous nitrate is 9 ~ 15:1.
In preferred steps (3), bath temperature is 70 DEG C.
The calcium oxide-based adsorbent of the present invention is used for absorbing carbon dioxide under hot conditions, the calcium oxide-based adsorbent of doped cerium oxide prepared by sol-gel process with calcium nitrate and cerous nitrate for presoma.Two metal ion species are abundant and citrate complexing in water-bath process, and uniform dispersion in the solution, is finally dispersed in adsorbent uniformly.The doping of cerium oxide greatly changes the pattern of adsorbent, makes pattern that adsorbent is compacted from bulk become loose porous, that shelly is crosslinked pattern, is conducive to carbon dioxide and adsorbent contact reacts; The doping of simultaneous oxidation cerium also effectively reduces the grain size of adsorbent, contributes to reaction and carries out in the fast reaction stage.
The present invention is applied to absorbing carbon dioxide under hot conditions: in thermogravimetric (STA-449F3), be seated in by adsorbent on alumina crucible, adsorbent is Powdered being laid on crucible.First under normal pressure, nitrogen atmosphere, rise to adsorption temp, stablize certain hour, logical carbon dioxide starts to carry out high temperature adsorption, and adsorption time is 20-60min; Total gas speed is 50-100mL/min, and the percentage by volume shared by carbon dioxide is 30-60%, and adsorption temp is 500-700 DEG C; After adsorption reaction completes, continue to be warming up to desorption temperature in a nitrogen atmosphere, desorption 20-40min under nitrogen atmosphere, desorption temperature is 650-800 DEG C.Again be cooled to adsorption temp after desorption reaction completes, carry out the mensuration of multiple adsorb/de-adsorption cycle and so forth.Mass change the real time measure is also preserved by computer record.
Compared with existing calcium oxide-based adsorbent, calcium oxide-based adsorbent provided by the invention has the more outstanding cyclical stability of higher adsorption capacity in for high temperature adsorption carbon dioxide, and wherein adsorption capacity can reach 0.59gCO
2/ g sorbent, experience 18 absorption/de-adsorption cycle adsorption capacities and keep completely constant, excellent in stability, is better than the calcium oxide-based sorbent systems of current diplomatic major part.
The invention has the advantages that: compared with existing calcium oxide-based sorbent systems, absorbent preparation process is simple, and lower to the requirement of preparation process parameter, cost is less, is suitable for large-scale production and application; The calcium oxide-based adsorbent of doped cerium oxide shows excellent absorption property simultaneously, and adsorption capacity is higher, makes the adsorbent amount of carbon dioxide of unit more; Cyclical stability is better, and adsorbent can be recycled in multiple adsorb/de-adsorption cycle.Calcium oxide-based adsorbent of the present invention is used for high temperature adsorption carbon dioxide more wide prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the material prepared by embodiment 1 and 2;
The calcium oxide-based adsorbent of different calcium cerium ratio, wherein: a-3; B-5; C-9; D-15; E-20; F-CaO;
Fig. 2 is the absorption property figure of the adsorbent of the different calcium cerium ratio of material prepared by embodiment 1 and 2;
Fig. 3 is the absorption property figure of the adsorbent of the different citric acid amounts of material prepared by embodiment 1 and 3;
Fig. 4 is the absorption property figure of the adsorbent of the different bath temperatures of material prepared by embodiment 1 and 4;
Fig. 5 is the absorption property figure of the adsorbent of the different water bath time of material prepared by embodiment 1 and 5;
Fig. 6 is the absorption property figure of the adsorbent of the different water bath time of material prepared by embodiment 1 and 6.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, and following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1:
Sol-gel process prepares the calcium oxide-based adsorbent of doped cerium oxide:
First using water as solvent, calcium nitrate and cerous nitrate are dissolved respectively, wherein the mol ratio of calcium nitrate and cerous nitrate is 15:1, is mixed by the nitrate solution after dissolving.Joined by citric acid in the mixed solution of nitrate, the ratio of citric acid and metal ion total mole number is 2:1.Be placed on Rotary Evaporators by mixed liquor after citric acid dissolves completely, setting bath temperature is 70 DEG C, and water bath time is 3h, makes calcium and cerium be able to even complexing.After water-bath 3h, vacuumize removing excessive moisture and obtain colloidal sol, colloidal sol is put into baking oven 100 DEG C of dry 12h.The expansion loose powdered obtained after drying is put into Muffle furnace roasting, obtains the calcium oxide-based adsorbent of doped cerium oxide.
Embodiment 2:
Adopt the preparation method in embodiment 1, regulate the mol ratio of calcium nitrate and cerous nitrate to be respectively 3:1,5:1,9:1,20:1, pure CaO, the calcium oxide-based adsorbent of obtained a series of different calcium cerium ratio.
Embodiment 3:
Adopt the preparation method in embodiment 1, the ratio regulating citric acid and metal ion total mole number is 1:1,3:1, obtains the calcium oxide-based adsorbent that some arrange different citric acid amount.
Embodiment 4:
Adopt the preparation method in embodiment 1, regulate bath temperature to be 60 DEG C, 80 DEG C, the calcium oxide-based adsorbent of obtained a series of different bath temperature.
Embodiment 5:
Adopt the preparation method in embodiment 1, regulate water bath time to be 1h, 5h, the calcium oxide-based adsorbent of obtained a series of different water bath time.
Embodiment 6:
Adopt the preparation method in embodiment 1, regulate baking temperature to be 80 DEG C, 120 DEG C, the calcium oxide-based adsorbent of obtained a series of different baking temperature.
Embodiment 7:
Adsorption process is carried out in STA449-F3, and the absorbent powder taken after a certain amount of roasting is positioned on the flat crucible of aluminium oxide.Be warming up to 600 DEG C in a nitrogen atmosphere, stablize certain hour, pass into carbon dioxide and carry out adsorption reaction, the total gas speed of adsorption process is 100mL/min, and carbon dioxide volume content is 50%.After adsorption reaction completes, be warming up to 700 DEG C in a nitrogen atmosphere, in a nitrogen atmosphere desorption 20min.After desorption reaction completes, again cool to 600 DEG C, re-start adsorption reaction after a period of stabilisation.So move in circles, the absorption property completing multiple adsorb/de-adsorption cycle measures.In experimentation, the mass change of adsorbent can be monitored and record in real time, can calculate the carbon dioxide adsorption capacity of adsorbent according to the mass change of adsorbent before and after adsorption reaction, and can find out the stable circulation implementations of calcium oxide-based adsorbent.
Embodiment 8:
Carried out SEM sign to the calcium oxide-based adsorbent of different calcium cerium ratio in embodiment 1 and 2, result as shown in Figure 1.
Can find out that pure CaO presents a kind of block structure by SEM figure, compact and do not have obvious hole in the surface of adsorbent.As Ca/Ce=20, not there is too large change in the basic configuration of adsorbent for pure CaO, remain block structure, but the surface of block adsorbent becomes fluffy.The adsorbent pattern of Ca/Ce=15 with Ca/Ce=5 is similar, is all made up of some half thinner shells, and is interconnected to form a loose entirety between these half shells.The adsorbent of Ca/Ce=9 presents a kind of structure of similar blister of porous, and the inside of balloon-shaped structure exists a large amount of gaps.Further raising Ca/Ce than to 3 time, adsorbent presents a kind of bulk laminated structure.
Embodiment 9:
Adopt the absorption/desorption conditions in embodiment 7 to carry out absorption property evaluation to the calcium oxide-based adsorbent of different calcium cerium ratio in embodiment 1 and 4, result as shown in Figure 2.
The adsorbent of all doped Ce all shows excellent stability as can be seen from Figure 2, and except the adsorbent stability of Ca/Ce=20 is slightly weaker, after experiencing 18 absorption/de-adsorption cycle, adsorption capacity is by original 0.58gCO
2/ g sorbent has been reduced to 0.49gCO
2/ g sorbent, the adsorbent of other calcium cerium ratios (Ca/Ce=3,5,9,15) after experience 18 absorption/de-adsorption cycle, CO
2adsorption capacity, compared with initial adsorption capacity, all keeps completely constant, is respectively 0.35gCO
2/ g sorbent, 0.45gCO
2/ gsorbent, 0.54gCO
2/ g sorbent and 0.59gCO
2/ g sorbent.The adsorbent of Ca/Ce=15 is selected to be best, because this adsorbent has the highest adsorption capacity (0.59gCO while having excellent cycling stability
2/ g sorbent), therefore this adsorbent possesses the potentiality of industrialization production requirements.
Embodiment 10:
Adopt the absorption/desorption conditions in embodiment 7 to carry out absorption property evaluation to the calcium oxide-based adsorbent of citric acid amount in embodiment 1 and 3, result as shown in Figure 3.
As can be seen from Figure 3 citric acid amount number impact is to a certain degree existed on the absorption property of adsorbent but impact is little.When citric acid and metal ion mol ratio are 1:1, the stability of adsorbent declines to some extent, experiences 18 adsorption/desorption/de-adsorption cycle adsorption capacities from 0.56gCO
2/ g sorbent drops to about 0.53gCO
2/ g sorbent; Mol ratio is when 2:1-3:1, and the absorption property of adsorbent is identical, excellent in stability, experiences 18 absorption/de-adsorption cycle adsorption capacities constant, therefore selects the citric acid of this scope for best.
Embodiment 11:
Adopt the absorption/desorption conditions in embodiment 7 to carry out absorption property evaluation to the calcium oxide-based adsorbent of different bath temperature in embodiment 1 and 4, result as shown in Figure 4.
As can be seen from Figure 4 when bath temperature is in the scope of 60 DEG C-80 DEG C, bath temperature does not affect the adsorption capacity of adsorbent and stability, and adsorbent all shows high adsorption capacity and excellent stability.
Embodiment 12:
Adopt the absorption/desorption conditions in embodiment 7 to carry out absorption property evaluation to the calcium oxide-based adsorbent of different water bath time in embodiment 1 and 5, result as shown in Figure 5.
The stability of water bath time to adsorbent has considerable influence as can be seen from Figure 5.When water bath time is 1h, the less stable of adsorbent, 18 times absorption/de-adsorption cycle adsorption capacity obviously declines, by initial 0.59gCO
2/ g sorbent reduces to about 0.5gCO
2/ g sorbent; When water bath time is 3-5h, absorption property is better, and excellent in stability, 18 times absorption/de-adsorption cycle adsorption capacity remains unchanged, and therefore 3-5h is decided to be the optimum water bath time preparing adsorbent.
Embodiment 13:
Adopt the absorption/desorption conditions in embodiment 7 to carry out absorption property evaluation to the calcium oxide-based adsorbent of different baking temperature in embodiment 1 and 6, result as shown in Figure 6.
The absorption property impact of baking temperature on adsorbent is larger as can be seen from Figure 6.When baking temperature be 80 DEG C and 120 DEG C time, adsorbent shows poor stability, and after 18 absorption/de-adsorption cycle, obvious decline has appearred in adsorption capacity; And baking temperature to be the adsorbent of 100 DEG C functional, excellent in stability, therefore selecting 100 DEG C is optimum drying temperature.
The calcium oxide-based adsorbent being further illustrated doped cerium oxide by above each embodiment has excellent absorption property, and calcium cerium reaches 0.59gCO than the adsorbent carbon dioxide adsorption capacity being 15
2/ g sorbent, and keep 18 absorption/de-adsorption cycle completely constant, be better than the absorption property of a lot of calcium oxide-based adsorbent of current bibliographical information.The calcium oxide-based adsorbent of adulterated al, when 600 DEG C of absorption, experiences 13 absorption/de-adsorption cycle adsorption capacities and is reduced to 0.4gCO by initial 0.6
2/ g sorbent (Fuel, 2013,111:636-642); The calcium oxide-based adsorbent of doping zirconium experiences 20 absorption/de-adsorption cycle adsorption capacities and is reduced to 0.45gCO by initial 0.5
2/ g sorbent (Fuel, 2014,127:94-100).The calcium oxide-based sorbent circulation stability of visible doped cerium oxide is obviously better than adulterating the adsorbent of other inert components, has good high temperature carbon dioxide absorption property.
The calcium oxide-based adsorbent of the doped cerium oxide adopting sol-gel process to prepare, under the condition of adsorption temp 600 DEG C, carbon dioxide content 50vol%, total gas speed 100mL/min, adsorb 45min, adsorption capacity reaches 0.59gCO
2/ g sorbent; Desorption under 700 DEG C of nitrogen atmospheres, experience 18 absorption/de-adsorption cycle adsorption capacities and keep completely constant, cyclical stability is high.The preparation technology of adsorbent is simple, and cost is low, is convenient to large-scale one-tenth and produces standby.There is very large change in the calcium oxide-based adsorbent pattern of doped cerium oxide simultaneously, and the pattern that the bulk multi-hole of formation, shelly are cross-linked is conducive to the reaction of adsorbent and carbon dioxide, can reach higher adsorption capacity.Adsorbent prepared by sol-gel process can make cerium oxide be dispersed in uniformly in adsorbent, effectively plays the effect hindering adsorbent sintering, makes adsorbent show preferably stability.Finally it is emphasized that whole preparation and absorbing process environmental protection, meet the theory of Green Chemistry.Therefore the calcium oxide-based adsorbent of doped cerium oxide has good industrial prospect in high temperature adsorption carbon dioxide direction.
Although be described the preferred embodiments of the present invention by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, can also make the concrete conversion of a lot of form, these all belong within protection scope of the present invention.
Claims (4)
1. a calcium oxide-based high temperature carbon dioxide sorbing material for inert component of adulterating, is characterized in that, inert component is cerium oxide, and the active component of absorbing carbon dioxide is calcium oxide.
2. the preparation method of the calcium oxide-based high temperature carbon dioxide sorbing material of inert component of adulterating described in claim 1, it is characterized in that, step is as follows:
(1) using water as solvent, cerous nitrate and calcium nitrate are dissolved respectively, the mol ratio of calcium nitrate and cerous nitrate is 3 ~ 15:1;
(2) added by citric acid in the mixed solution of calcium nitrate and cerous nitrate, the molal quantity of citric acid and the ratio of metal ion total mole number are 2 ~ 3:1;
(3) be placed on Rotary Evaporators by mixed liquor, setting bath temperature is 60 ~ 80 DEG C, water bath time 3 ~ 5h;
(4) revolve after steaming is drained and mixture is put into baking oven drying, baking temperature is 100 DEG C;
(5) dried material is carried out roasting, obtain the calcium oxide-based adsorbent of doped cerium oxide.
3. preparation method as claimed in claim 2, is characterized in that, in step (1), the mol ratio of calcium nitrate and cerous nitrate is 9 ~ 15:1.
4. preparation method according to claim 2, is characterized in that, in step (3), bath temperature is 70 DEG C.
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Cited By (4)
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| CN106861601A (en) * | 2015-12-11 | 2017-06-20 | 华中科技大学 | A kind of CO of ytterbium doping2Adsorbent and preparation method thereof |
| CN109012008A (en) * | 2018-07-27 | 2018-12-18 | 昆明理工大学 | It is a kind of to prepare calcium base CO using the doping of rare earth waste2The method of adsorbent |
| CN109153002A (en) * | 2016-05-16 | 2019-01-04 | 日立化成株式会社 | Adsorbent, the removing method of carbon dioxide, carbon dioxide removing device and carbon dioxide remove system |
| CN113512409A (en) * | 2021-07-07 | 2021-10-19 | 中国科学院工程热物理研究所 | Method for preparing porous calcium-based material by using eggshells and application of porous calcium-based material in thermochemical energy storage |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106861601A (en) * | 2015-12-11 | 2017-06-20 | 华中科技大学 | A kind of CO of ytterbium doping2Adsorbent and preparation method thereof |
| CN106861601B (en) * | 2015-12-11 | 2019-08-13 | 华中科技大学 | A kind of CO of ytterbium doping2Adsorbent and preparation method thereof |
| CN109153002A (en) * | 2016-05-16 | 2019-01-04 | 日立化成株式会社 | Adsorbent, the removing method of carbon dioxide, carbon dioxide removing device and carbon dioxide remove system |
| CN109153000A (en) * | 2016-05-16 | 2019-01-04 | 日立化成株式会社 | Adsorbent, the removing method of carbon dioxide, carbon dioxide removing device and carbon dioxide remove system |
| CN109012008A (en) * | 2018-07-27 | 2018-12-18 | 昆明理工大学 | It is a kind of to prepare calcium base CO using the doping of rare earth waste2The method of adsorbent |
| CN109012008B (en) * | 2018-07-27 | 2021-06-18 | 昆明理工大学 | Preparation of calcium-based CO by doping rare earth waste2Method for producing adsorbent |
| CN113512409A (en) * | 2021-07-07 | 2021-10-19 | 中国科学院工程热物理研究所 | Method for preparing porous calcium-based material by using eggshells and application of porous calcium-based material in thermochemical energy storage |
| CN113512409B (en) * | 2021-07-07 | 2023-02-03 | 中国科学院工程热物理研究所 | Method for preparing porous calcium-based material by using eggshells and application of porous calcium-based material in thermochemical energy storage |
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Application publication date: 20150722 |