CN105617978A - Preparation method of loaded type MgO/gamma-Al2O3 adsorbent capable of adsorbing CO2 at room temperature - Google Patents
Preparation method of loaded type MgO/gamma-Al2O3 adsorbent capable of adsorbing CO2 at room temperature Download PDFInfo
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Abstract
The invention provides a preparation method of a loaded type MgO/gamma-Al2O3 adsorbent capable of adsorbing CO2 at room temperature. The method comprises the following steps: (1) uniformly stirring P123 with inorganic aluminum salt and magnesium salt distilled water for 8-24 hours at the temperature of 20-60 DEG C to obtain sol; (2) adding a 3mol/L sodium metaaluminate solution into the sol, continuing to increase the temperature and stir, and carrying out double-hydrolysis reaction to prepare a mixed hydroxide suspension solution with Mg<-> and Al<->; (3) transferring the suspension solution to a reactor with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 12-36 hours at the temperature of 80-120 DEG C to obtain a hydrothermal reaction product; (4) cooling the hydrothermal reaction product, then centrifugally separating, vacuum-drying and grinding and roasting the hydrothermal reaction product successively to prepare the adsorbent. Through the preparation method of the loaded type MgO/gamma-Al2O3 adsorbent, a precursor of the adsorbent is directly prepared in the double-hydrolysis reaction process; the method replaces a conventional impregnation method of gamma-Al2O3 loaded magnesium salt; the inorganic aluminum salt and the magnesium salt used by the method are cheap and non-toxic; the preparation condition is mild; the prepared absorbent has excellent adsorption performance and stable cyclic regeneration adsorption performance on CO2 at the room temperature.
Description
Technical field
The present invention relates to CO2Catch, especially relate to a kind of double; two hydrolysis and prepare room temperature CO absorption2Support type MgO/ ��-Al2O3The method of adsorbent.
Background technology
It is known that the most great environmental problem that global warming is the mankind to be faced so far, it also it is one of the most complicated challenge of 21 century facing mankind. CO2It is one of large industrial predominant emissions, is again the predominant gas causing greenhouse effect. In recent years, CO2Discharge capacity raise year by year, exacerbate greenhouse effect and give the current and following global ecological environment constitute a serious threat. Therefore, CO is implemented2Catch and be enriched with there is important theoretical and practical significance.
At present, trapping CO2Main method have liquid phase scrubbing method, solid adsorbant method, membrane separation process etc. Wherein equipment is had severe corrosive, absorbent regeneration energy consumption big and easy to be oxidized degradable by liquid phase scrubbing method; Membrane separation process exists that separation efficiency is relatively low, high in cost of production problem, limits its application. By contrast, the operation of solid absorption method is relatively easy, and the corrosivity of equipment is little, is the CO of a great promotion prospect2Trapping recovery technology, due to CO2It it is sour gas, being readily adsorbed in the oxide surface with alkalescence, especially meso-porous alumina has a characteristic of high-ratio surface, soda acid both sexes, and magnesium oxide is best selection as middle highly basic, cheap, its adsorption temp has good CO at 25 DEG C��300 DEG C2Absorption property, can be used for high-temperature flue gas CO2Catch, and common magnesium oxide has relatively low specific surface area and pore volume. Based on this, utilizing the high-specific surface area of meso-porous alumina and magnesian middle highly basic characteristic is the CO of a kind of great competitiveness2Adsorbent.
The preparation method that CN103920463A discloses the modified silica-based solid amine carbon dioxide absorbing material of a kind of grafting, the mode that silane coupler diethylenetriamine base propyl trimethoxy silicane high for amine groups content utilizes later stage grafting modified distinguishes grafting to the silica substrate of four kinds of types with synthesis of solid adsorbing material, by silicon dioxide dry 2-3h at 110 DEG C, , then the 200ml toluene dried is added, reactor put in oil bath pan and fix, mix reflux condenser and then in reactor, pass into nitrogen purge, again reactor is sealed, it is at the uniform velocity stirred and is heated to 90 DEG C, subsequently 4ml divinyl triammonium base propyl trimethoxy silicane is joined in reactor and at the uniform velocity stir, 6h is carried out at 90 DEG C, after question response completes, synthesized material is filtered and uses 100ml dehydrated alcohol to rinse twice, then in vacuum drying oven 80 DEG C after dry 12 hours, last CO2Optimal adsorption amount is only 1.02mmol/g. The critical defect that the method also exists that operation is more, complex process, condition harsh and the organic solvent such as toluene is poisonous. CN103611491A discloses a kind of functional mesoporous alumina base low temperature CO of alkali metal2The preparation method of adsorbent. Adopt incipient impregnation and excessive impregnation technology, by different alkali metal salt soln loads at the ��-Al prepared2O3On carrier, to improve its room temperature CO2Absorption property. Its optimal adsorption amount is only 1.13mmol/g, is 1.07mmol/g during circulation absorption three times, and the method technics comparing is complicated, and cyclical stability is not good enough. CN102658080A discloses a kind of high dispersing microporous/mesoporous ��-Al2O3The preparation method of base alkali (soil) metal composite adsorbent, first use acidolysis Jiao Lvyuan, again the colloidal sol obtained is mixed with Pluronic triblock copolymer solution, add alkali (soil) metal precursor salts, after stirring, prepare alkali (soil) metal composite adsorbent through steps such as dry, roastings. CO under room temperature2Optimal adsorption amount is 1.34mmol/g, but its cyclical stability is not done further research, greatly reduces the prospect of its practical application.
Wen Xia et al. (L.Li, X.Wen, X.Fu, F.Wang, N.Zhao, F.Xiao, W.WeiandY.Sun, Energy&Fuels, 2010,24,5773-5780.) is with ��-Al2O3For carrier, excessive infusion process is adopted to be prepared for magnesium-modified load type adsorbing agent MgO/Al2O3, but its dip loading process is comparatively laborious, and nitrogen roasting condition compares power consumption. JeongGilSeo et al. (S.J.Han, Y.Bang, H.Lee, K.Lee, I.K.SongandJ.G.Seo, ChemicalEngineeringJournal, 2015,270,411-417.) with Pluronic triblock copolymer P123 and ionic liquid C16mimCl for double template, evaporation induced self-assembly method is adopted to be prepared for MgO-Al2O3Compound adsorbent, but its preparation process uses poisonous and expensive organo-aluminium alcoholate as aluminum source, volatility nitric acid is as acid regulator, and this and current Green Chemistry are advocated employing theory nontoxic, harmless material and be not inconsistent.
To sum up, method of production simplicity, mild condition, cheaper starting materials, nontoxic and circulation absorption meso-porous alumina base compound CO of good performance2Adsorbing material has important scientific value and good application prospect.
Summary of the invention
The technical problem to be solved is: provide a kind of cheaper starting materials and nontoxic, preparation condition is gentle, without routine dipping support type MgO/ ��-Al2O3The preparation method of adsorbent, prepared adsorbent is at room temperature to main greenhouse gas CO2There is excellent absorption property and stable circular regeneration absorption property.
This invention address that its technical problem adopts following technical scheme:
Room temperature CO absorption provided by the invention2Support type MgO/ ��-Al2O3The preparation method of adsorbent, is that a kind of double; two hydrolysis prepares room temperature CO absorption2Support type MgO/ ��-Al2O3The method of adsorbent, comprises the following steps:
(1) water solublity Pluronic triblock copolymer P123 and inorganic aluminate, magnesium salt are added in distilled water, at 20��60 DEG C, stir 8��24h, obtain colloidal sol;
(2) then raise temperature to 70 DEG C, colloidal sol is stirred 4h, adds the sodium aluminate solution of 3mol/L, at 70��90 DEG C of temperature, then stir 2��6h, through double; two hydrolysis, obtain the suspension of Mg-, Al-mixed hydroxides;
(3) being transferred to by above-mentioned suspension in the reactor of inner liner polytetrafluoroethylene, at 80��120 DEG C of temperature, hydro-thermal 12��36h, obtains hydrothermal product;
(4) successively through including centrifugation, vacuum drying, grinding and calcination steps after hydrothermal product cooling, described room temperature CO absorption is prepared2Support type MgO/ ��-Al2O3Adsorbent.
Described inorganic aluminate is aluminum nitrate, aluminum chloride or aluminum sulfate.
Described magnesium salt is magnesium nitrate, magnesium chloride or magnesium sulfate.
Described suspension, wherein Mg-and Al-Mol ratio be 0.1��0.3.
In said method, gained support type MgO/ ��-Al2O3Adsorbent CO2After, then de-adsorption cycle regeneration at different temperature.
Described adsorbent CO2Temperature be 25, DEG C desorption temperature is 150��400. DEG C
The present invention compared with prior art has following main advantage:
(1) cheaper starting materials, preparation condition are gentle, it is to avoid adopting expensive and poisonous organo-aluminium alcoholate is aluminum source;
(2) raw material sodium metaaluminate is precipitant, is also inorganic aluminum source;
(3) gentle, easy double; two hydrolysis one step is adopted quickly to prepare support type MgO/ ��-Al2O3Adsorbent, eliminates the load step of conventional infusion process, and efficiency increases substantially, and magnesium oxide is evenly distributed in the skeleton of meso-porous alumina;
(4) the support type MgO/ ��-Al prepared by2O3CO absorption2After can regenerate at a lower temperature (by CO absorption2After sample on the TriStar of new generation II 3020 type Sorption Analyzer degasser that Merck & Co., Inc of the U.S. produces in 400, degassed 4h under DEG C vacuum condition, regeneration tests can be completed), and its circular regeneration absorption property is excellent.
Accompanying drawing explanation
Fig. 1 is the support type MgO/ ��-Al prepared by embodiment 1��72O3, mesoporous ��-Al2O3(sample A0-1) and MgO (sample A0-2) are at room temperature to CO2Adsorption curve.
Fig. 2 is the support type MgO/ ��-Al prepared by embodiment 12O3Adsorbent is at room temperature to CO2Circulation absorption figure.
Fig. 3 is mesoporous ��-Al2O3TEM picture.
Fig. 4 is the support type MgO/ ��-Al prepared by embodiment 12O3The TEM picture of adsorbent.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, and these embodiments are only the description to better embodiment of the present invention, but are not limited to following described content.
Embodiment 1:
First, joining in 32.5ml distilled water by 1.875g nine water aluminum nitrate, 0.64g magnesium nitrate hexahydrate and 2.26gP123, stir 16h and obtain vitreosol at 40 DEG C, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 1.6394g sodium metaaluminate and 6.5ml distilled water solution is slowly added dropwise in reaction system, product stirs 4h further at 70 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 24h at 80 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, finally in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.12O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature be 400 DEG C. Its CO2Adsorbance is 1.51mmol/g (see curve A1 in Fig. 1).
Embodiment 2:
First, joining in 32.5ml distilled water by 1.875g nine water aluminum nitrate, 0.5083g magnesium chloride hexahydrate and 2.26gP123, stir 16h at 40 DEG C and obtain vitreosol, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 1.6394g sodium metaaluminate and 6.5ml distilled water solution is slowly added dropwise in reaction system, product stirs 4h further at 70 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 24h at 80 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, last in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.12O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature be 400 DEG C. Its CO2Adsorbance is 1.03mmol/g (see curve A2 in Fig. 1).
Embodiment 3:
First, joining in 32.5ml distilled water by 1.875g nine water aluminum nitrate, 0.3g magnesium sulfate and 2.26gP123, stir 16h at 40 DEG C and obtain vitreosol, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 1.6394g sodium metaaluminate and 6.5ml distilled water solution is slowly added dropwise in reaction system, product stirs 4h further at 70 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 24h at 80 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, last in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.12O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature be 275 DEG C. Its CO2Adsorbance is 0.974mmol/g (see curve A3 in Fig. 1).
Embodiment 4:
First, joining in 32.5ml distilled water by 1.2072g Aluminum Chloride Hexahydrate, 0.3g magnesium sulfate and 2.26gP123, stir 24h at 40 DEG C and obtain vitreosol, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 1.6394 sodium metaaluminates and 6.5ml distilled water solution is slowly added dropwise in reaction system, product stirs 4h further at 80 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 24h at 120 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, last in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.12O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature be 150 DEG C, its CO2Adsorbance is 0.614mmol/g (see curve A4 in Fig. 1).
Embodiment 5:
First, joining in 32.5ml distilled water by 1.2072g Aluminum Chloride Hexahydrate, 0.80245g magnesium sulfate and 2.26gP123, stir 24h at 60 DEG C and obtain vitreosol, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 2.3238g sodium metaaluminate and 9.5ml distilled water solution is slowly added dropwise in reaction system, product stirs 4h further at 80 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 24h at 100 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, last in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.22O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature be 275 DEG C, its CO2Adsorbance is 0.553mmol/g (see curve A5 in Fig. 1).
Embodiment 6:
First, joining in 32.5ml distilled water by 3.3321g aluminum sulfate octadecahydrate, 6.099g magnesium chloride hexahydrate and 2.26gP123, stir 8h at 20 DEG C and obtain vitreosol, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 7.3775g sodium metaaluminate and 30ml distilled water solution is slowly added dropwise in reaction system, product stirs 2h further at 70 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 12h at 80 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, last in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.32O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature be 150 DEG C, its CO2Adsorbance is 0.617mmol/g (see curve A6 in Fig. 1).
Embodiment 7:
First, joining in 32.5ml distilled water by 1.875g nine water aluminum nitrate, 0.64g magnesium nitrate hexahydrate and 2.26gP123, stir 16h at 40 DEG C and obtain vitreosol, vitreosol continues stirring 4h after being warming up to 70 DEG C. Then, prepared to 1.6394g sodium metaaluminate and 6.5ml distilled water solution is slowly added dropwise in reaction system, product stirs 6h further at 90 DEG C, it is subsequently transferred in the reactor of inner liner polytetrafluoroethylene, hydro-thermal 36h at 120 DEG C, gained hydrothermal product is performing centrifugal separation on, 80 DEG C of vacuum dryings, last in Muffle furnace in the still air of 500 DEG C roasting 2h, obtain the MgO/ ��-Al that Mg-and Al-mol ratio is 0.12O3Composite. Gained sample adsorption CO2Temperature be 25 DEG C, desorption temperature is 400 DEG C, its CO2Adsorbance is 0.979mmol/g (see curve A7 in Fig. 1).
By CO absorption2After the degasser of TriStar of new generation II 3020 type Sorption Analyzer that produces in Merck & Co., Inc of the U.S. of sample in 400 DEG C, degassed 4h under vacuum condition. Then the sample after degassed is circulated adsorption experiment, circulates 10 times, its room temperature CO2Adsorbance substantially remains in 1.51mmol/g, and the circular regeneration showing excellence uses ability (see Fig. 2)
As shown in Figure 3: meso-porous alumina and support type MgO/ ��-Al2O3Adsorbent has vermiform duct, is unordered mesoporous material, and MgO introduces front and rear gaps does not have significant change.
Claims (6)
1. a room temperature CO absorption2Support type MgO/ ��-Al2O3The preparation method of adsorbent, is characterized in that a kind of double; two hydrolysis prepares room temperature CO absorption2Support type MgO/ ��-Al2O3The method of adsorbent, comprises the following steps:
(1) water solublity Pluronic triblock copolymer P123 and inorganic aluminate, magnesium salt are added in distilled water, at 20��60 DEG C, stir 8��24h, obtain colloidal sol;
(2) then raise temperature to 70 DEG C, colloidal sol is stirred 4h, adds the sodium aluminate solution of 3mol/L, at 70��90 DEG C of temperature, then stir 2��6h, through double; two hydrolysis, obtain the suspension of Mg-, Al-mixed hydroxides;
(3) being transferred to by above-mentioned suspension in the reactor of inner liner polytetrafluoroethylene, at 80��120 DEG C of temperature, hydro-thermal 12��36h, obtains hydrothermal product;
(4) successively through including centrifugation, vacuum drying, grinding and calcination steps after hydrothermal product cooling, described room temperature CO absorption is prepared2Support type MgO/ ��-Al2O3Adsorbent.
2. preparation method according to claim 1, it is characterised in that described inorganic aluminate is aluminum nitrate, aluminum chloride or aluminum sulfate.
3. preparation method according to claim 1, it is characterised in that described magnesium salt is magnesium nitrate, magnesium chloride or magnesium sulfate.
4. preparation method according to claim 1, it is characterised in that described suspension, wherein Mg-and Al-Mol ratio be 0.1��0.3.
5. preparation method according to claim 1, it is characterised in that gained support type MgO/ ��-Al2O3Adsorbent CO2After, then de-adsorption cycle regeneration at different temperature.
6. preparation method according to claim 5, it is characterised in that described adsorbent CO2Temperature be 25 DEG C, desorption temperature is 150��400 DEG C.
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| CN108097200A (en) * | 2016-11-25 | 2018-06-01 | 中国石油化工股份有限公司 | A kind of method for preparing modified aluminas |
| CN110639465A (en) * | 2019-07-05 | 2020-01-03 | 南京理工大学 | High-strength sodium-based solid adsorbent suitable for carbon capture and preparation method thereof |
| CN111298760A (en) * | 2020-03-16 | 2020-06-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of flower-like aluminum oxide-magnesium oxide composite adsorbent, product and application thereof |
| CN114602418A (en) * | 2022-04-02 | 2022-06-10 | 安徽芈源环保科技有限公司 | Setaria viridis-shaped metal oxide nano material with bionic structure and preparation method thereof |
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| CN110639465A (en) * | 2019-07-05 | 2020-01-03 | 南京理工大学 | High-strength sodium-based solid adsorbent suitable for carbon capture and preparation method thereof |
| CN111298760A (en) * | 2020-03-16 | 2020-06-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of flower-like aluminum oxide-magnesium oxide composite adsorbent, product and application thereof |
| CN114602418A (en) * | 2022-04-02 | 2022-06-10 | 安徽芈源环保科技有限公司 | Setaria viridis-shaped metal oxide nano material with bionic structure and preparation method thereof |
| CN114797753A (en) * | 2022-04-29 | 2022-07-29 | 武汉理工大学 | Alumina-based trapping material for efficiently adsorbing carbon dioxide and preparation method and application thereof |
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