CN104826610A - Metallic organic skeletal material PEI@UiO-66, preparation method thereof, and application thereof in adsorptive separation of CO2 - Google Patents
Metallic organic skeletal material PEI@UiO-66, preparation method thereof, and application thereof in adsorptive separation of CO2 Download PDFInfo
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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Abstract
The invention discloses a metallic organic skeletal material PEI@UiO-66, a preparation method thereof, and an application thereof in adsorptive separation of CO2. The method comprises the following steps: 1, adding anhydrous ethanol into polyethyleneimine (PEI) in a dropwise manner, and carrying out ultrasonic mixing until the PEI is completely dissolved; 2, adding the above obtained mixed solution into a preprocessed UiO-66 metallic organic skeletal material in a dropwise manner; 3, drying a pasty mixture obtained in step 2 in N2 atmosphere; and 4, carrying out vacuum drying on the dried material to prepare the PEI@UiO-66 adsorbent. When the PEI@UiO-66 prepared in step 4 is used to adsorb CO2, the temperature and the relative humidity of a charged gas can be adjusted in order to further improve the CO2 adsorption capacity of the PEI@UiO-66. The PEI@UiO-66 adsorbent prepared in the invention has very good hydrothermal stability, and greatly improves the CO2 adsorption capacity and the CO2/CH4 mixed gas separation selectivity of the UiO-66 material under mild temperature and wet conditions.
Description
Technical field
The invention belongs to chemical adsorbing separation science and technology field, be specifically related to a kind of metal-organic framework materials PEI@UiO-66 and preparation method thereof with at adsorbing separation CO
2in application.
Background technology
CH
4be fuel important in productive life and raw material, the source of methane mainly comprises gas field exploitation and biomass ferment.Normal containing more CO in methane mixed gas
2, N
2, sulfide, the impurity such as steam, the existence of these gases not only makes methane gas can not directly apply but also considerably increase the cost of gas transmission.In these impurity gas, CO
2on natural gas and biological methane gas use and to transport impact the most serious, first, even if a small amount of CO
2existence in methane gas also can affect the burning quality of fuel; The second, CO
2be sour gas, to transport pipeline and transfer cask, there is larger corrosivity, add cost of equipment maintenance; Finally, CO
2molecular weight is large, and post liquefaction mass per volume is comparatively large, adds cost of transportation.
Adsorption method of separation is by the CO in natural gas and biological methane gaseous mixture
2the effective means separated, adsorbent is the key of adsorption method of separation, and its performance directly determines energy consumption and the efficiency of whole separation process.In addition, under actual condition, steam is immanent, when ubiquity mist contains steam, due to the competitive Adsorption of water, can cause adsorbent CO
2hydraulic performance decline.
MOFs(Metal Organic frameworks) material mainly a class be connected with transition metal ions containing the organic ligand of oxygen or nitrogen element and the multidimensional periodicity mesh skeleton that formed, specific area, the pore structure with superelevation are adjustable, gas absorption be separated in there is good application prospect.But existing MOFs material major part is steam instability, and MOFs material is once adsorbed water, and its structure will be caved in, although some stablize, price or performance not ideal enough.Therefore, a kind of Stability Analysis of Structures how is prepared, again to CO
2there is high-adsorption-capacity, to CO
2/ CH
4high score is had to be problem demanding prompt solution from optionally MOFs adsorbent.A kind of porous material that UiO-66 is Stability Analysis of Structures in current MOFs material, preparation cost is lower, have potential application prospect, weak point is: it is to CO
2adsorption capacity and CO
2/ CH
4adsorbing separation selective not high enough, for this problem, this project has invented a kind of raising metal-organic framework materials UiO-66 adsorbing separation CO
2the method of performance.
Summary of the invention
In order to solve, UiO-66 material structure is stable, preparation cost is lower, but it is to CO
2adsorption capacity and CO
2/ CH
4the selective not high enough problem of adsorbing separation, the first object of the present invention is the preparation method providing a kind of metal-organic framework materials PEI@UiO-66.
The second object of the present invention is to provide above-mentioned metal-organic framework materials PEI@UiO-66 at adsorbing separation CO
2in application.
In order to realize the first object, the present invention adopts following technical scheme:
(1) be added to by absolute ethyl alcohol in polymine (PEI), under normal temperature, the ultrasonic PEI that is mixed to dissolves, and obtains PEI/ absolute ethyl alcohol mixed liquor;
(2) step (1) gained PEI/ absolute ethyl alcohol mixed liquor is joined in UiO-66 material lentamente, then stir, obtain pasty mixture;
(3) by the pasty mixture of step (2) gained in N
2dry in atmosphere;
(4) step (3) resulting materials is carried out vacuum drying, obtain sorbing material and metal-organic framework materials PEI@UiO-66.
In said method, described in step (1), the mass ratio of absolute ethyl alcohol and polymine is 9 ~ 39, and the described ultrasonic time is 5 ~ 20 min.
In said method, described in step (2), the mass ratio of PEI/ absolute ethyl alcohol mixed liquor and UiO-66 is 1 ~ 16.
In said method, the temperature of drying described in step (3) is 30 ~ 90 DEG C.
In said method, described in step (4), vacuum drying temperature is 90 ~ 130 DEG C, and the time is 4 ~ 10 h.
In order to realize the second object, the present invention adopts following technical scheme: CO absorption
2time, the temperature of regulation and control feed gas is 25 ~ 75 DEG C, and relative humidity is 0 ~ 80 %, plays the synergy of steam and PEI with this, improves sorbing material and metal-organic framework materials PEI@UiO-66 CO absorption further
2capacity.
Above-mentioned PEI and absolute ethyl alcohol all directly can be bought from market, and synthesize the raw material needed for UiO-66, if terephthalic acid (TPA) and zirconium chloride are also easy chemicals commercially.
The present invention has following advantage and effect relative to prior art:
(1) the metal-organic framework materials PEI@UiO-66 for preparing of the present invention is due to the introducing of PEI, adds the alkalescence of material surface and greatly reduces the pore volume of UiO-66 material, thus at raising UiO-66 material to CO
2adsorbance while reduce it to CH
4adsorbance, namely significantly improve material to CO
2/ CH
4adsorbing separation selective.
(2) the metal-organic framework materials PEI@UiO-66 for preparing of the present invention is at adsorbing separation CO
2time, when feed gas temperature raises, CO
2diffusion in PEI@UiO-66 duct is promoted, and thus material is to CO
2adsorption capacity improve further; And when steam exists, under the confinement effect of PEI@UiO-66 duct, hydrone meeting and CO
2form carbonic acid, be then combined by the amino of hydrogen bond on PEI@UiO-66, thus have and greatly facilitate PEI@UiO-66 to CO
2adsorption capacity and CO
2/ CH
4adsorptive selectivity.
(3) because UiO-66 has excellent hydrothermal stability and alkaline stability, and PEI@UiO-66 is to CO
2absorption/desorption reversible, the PEI@UiO-66 adsorbent therefore prepared by the present invention can repeatedly circular regeneration use.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of PEI@UiO-66 material prepared by different embodiment.
Fig. 2 is the FTIR spectrogram of PEI@UiO-66 material prepared by different embodiment.
Fig. 3 a and Fig. 3 b is respectively material prepared by different embodiment under 298 K to CO
2and CH
4adsorption isotherm.
The PEI@UiO-66 material of Fig. 4 a prepared by UiO-66 and embodiment 3 is to CO
2/ CH
4two components absorption H103 resin; The material CO at different temperatures of Fig. 4 b prepared by embodiment 3
2/ CH
4h103 resin; The PEI@UiO-66 material of Fig. 4 c prepared by embodiment 3 is to CO
2work adsorption capacity and CO
2/ CH
4the column diagram of separation selectivity.
Fig. 5 is that the PEI@UiO-66 material of 4 embodiments is to CO
2work adsorption capacity and CO
2/ CH
4adsorptive selectivity comparison diagram.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described, the present invention is not limited thereto.
embodiment 1
First, by 9:1(absolute ethyl alcohol: PEI) mass ratio, absolute ethyl alcohol is slowly added in PEI, under normal temperature ultrasonic be mixed to PEI dissolve, obtain PEI/ absolute ethyl alcohol mixed liquor; Then, by the mass ratio (PEI/ absolute ethyl alcohol mixed liquor: UiO-66) of 1:1, PEI/ absolute ethyl alcohol mixed liquor is joined in UiO-66 material, then stirs under normal temperature; Gained pasty mixture is at N
2dry at 30 DEG C in atmosphere; By material transfer vacuum drying 4 h at 130 DEG C in vacuum drying chamber after drying, just obtained metal-organic framework materials 10% PEI@UiO-66.
Application: obtained metal-organic framework materials 10% PEI UiO-66 is seated in fixed bed, under the damp condition of 298K and 0%, passes into CO
2/ CH
4mist, Simultaneously test its absorption H103 resin, the H103 resin experimentally obtained, calculate this material to CO
2work adsorption capacity can reach 0.45 mmol/g, to CO
2/ CH
4the selectivity factor of Dynamic Adsorption is 3.5.
embodiment 2
First, by 19:1(absolute ethyl alcohol: PEI) mass ratio, absolute ethyl alcohol is slowly added in PEI, under normal temperature ultrasonic be mixed to PEI dissolve, obtain PEI/ absolute ethyl alcohol mixed liquor; Then, by the mass ratio (PEI/ absolute ethyl alcohol mixed liquor: UiO-66) of 4:1, PEI/ absolute ethyl alcohol mixed liquor is joined in UiO-66 material, then stirs under normal temperature; Gained pasty mixture is at N
2dry at 45 DEG C in atmosphere; By material transfer vacuum drying 6 h at 110 DEG C in vacuum drying chamber after drying, just obtained metal-organic framework materials 20% PEI@UiO-66.
Application: by 20% obtained PEI UiO-66 mixture in fixed bed, under the damp condition of 318K and 30%, pass into CO
2/ CH
4mist, Simultaneously test its absorption H103 resin, the H103 resin experimentally obtained, calculate this material to CO
2work adsorption capacity can reach 0.90 mmol/g, to CO
2/ CH
4the selectivity factor of Dynamic Adsorption is 24.
embodiment 3
First, by 29:1(absolute ethyl alcohol: PEI) mass ratio, absolute ethyl alcohol is slowly added in PEI, under normal temperature ultrasonic be mixed to PEI dissolve, obtain PEI/ absolute ethyl alcohol mixed liquor; Then, by the mass ratio (PEI/ absolute ethyl alcohol mixed liquor: UiO-66) of 9:1, PEI/ absolute ethyl alcohol mixed liquor is joined in UiO-66 material, then stirs under normal temperature; Gained pasty mixture is at N
2dry at 65 DEG C in atmosphere; By material transfer vacuum drying 8 h at 100 DEG C in vacuum drying chamber after drying, just obtained metal-organic framework materials 30% PEI@UiO-66.
Application: by 30% obtained PEI UiO-66 mixture in fixed bed, under the damp condition of 338K and 55%, pass into CO
2/ CH
4mist, Simultaneously test its absorption H103 resin, the H103 resin experimentally obtained, calculate this material to CO
2work adsorption capacity can reach 2.4 mmol/g, to CO
2/ CH
4dynamic Adsorption selectivity factor be 167.
embodiment 4
First, by 39:1(absolute ethyl alcohol: PEI) mass ratio, absolute ethyl alcohol is slowly added in PEI, under normal temperature ultrasonic be mixed to PEI dissolve, obtain PEI/ absolute ethyl alcohol mixed liquor; Then, by the mass ratio (PEI/ absolute ethyl alcohol mixed liquor: UiO-66) of 16:1, PEI/ absolute ethyl alcohol mixed liquor is joined in UiO-66 material, then stirs under normal temperature; Gained pasty mixture is at N
2dry at 65 DEG C in atmosphere; By material transfer vacuum drying 10 h at 90 DEG C in vacuum drying chamber after drying, just obtained metal-organic framework materials 40% PEI@UiO-66.
Application: by 40% obtained PEI UiO-66 mixture in fixed bed, under the damp condition of 348K and 80%, pass into CO
2/ CH
4mist, Simultaneously test its absorption H103 resin, the H103 resin experimentally obtained, calculate this material to CO
2work adsorption capacity can reach 1.5 mmol/g, to CO
2/ CH
4dynamic Adsorption selectivity factor be 86.
For the metal-organic framework materials PEI@UiO-66 further illustrating PEI modification prepared by various embodiments of the present invention has good stability, and to CO
2adsorbance and CO
2/ CH
4separation selectivity be all largely increased, PEI@UiO-66 the present invention prepared and UiO-66 material have carried out the contrast of several aspect.Characterize and absorption property evaluation result as follows:
material structure and surface characteristic
Fig. 1 is the XRD spectra of UiO-66 and four embodiment material.Different embodiment material each peak position and intensity compared with UiO-66 material is almost identical as we can see from the figure, and this illustrates that the crystal structure of the later UiO-66 of load strong basicity polymer PEI still remains unchanged.This mainly has benefited from the good alkaline stability of UiO-66.
Fig. 2 is the FTIR spectrogram of UiO-66 and four embodiment material.As we can see from the figure: at 2800-3300 cm
-1in wave-length coverage, all there is the bending vibrations peak of CH and NH in four embodiment materials, and this is owing to containing a large amount of CH and NH in PEI molecule.The appearance side at these peaks reflects PEI and has successfully loaded on UiO-66 material.
the evaluation of absorption property
Fig. 3 a is UiO-66 and 4 CO of embodiment material under 298K condition
2adsorption isotherm.As seen from the figure: the CO of PEI@UiO-66
2adsorbance significantly improves than UiO-66.Wherein, embodiment 3 couples of CO
2adsorbance up to 3.3 mmol/g(1bar); Fig. 3 b is corresponding CH
4adsorption isotherm, as seen from the figure: the load due to PEI occupies the pore volume of UiO-66, therefore PEI@UiO-66 is to CH
4adsorbance have obvious decline than UiO-66, and embodiment 4 material that wherein PEI load capacity is maximum is to CH
4adsorbance minimum.
Fig. 4 a be UiO-66 and 30% PEI@UiO-66 material prepared by embodiment 3 under 298 K to CO
2/ CH
4the absorption H103 resin of (1/9, v/v) two component gases.As seen from the figure: 30% PEI@UiO-66 material of embodiment 3 correspondence is to CO
2absorption had raising clearly through the time relative to UiO-66, and to CH
4do not have significant change through the time.Illustrate that 30% PEI@UiO-66 of embodiment 3 correspondence not only has larger CO
2work adsorbance (0.74 mmol/g), and to CO
2/ CH
4two component mist selective reaches 10 and compares UiO-66 and there has also been and significantly improve.Fig. 4 b be under condition of different temperatures embodiment 3 gained 30% PEI@UiO-66 material to CO
2/ CH
4the absorption H103 resin of two component gases.As we can see from the figure: 30% PEI@UiO-66 is to CO
2work adsorbance raise along with the rising of temperature, be 0 % when temperature reaches 338 K(humidity) time, 30% PEI@UiO-66 is to CO
2work adsorbance and CO
2/ CH
4separation selectivity is that 1.6 mmol/g and 111(reach maximum).Temperature rises and causes CO
2adsorbance and CO
2/ CH
4the main cause that separation selectivity significantly improves is: (1) raised temperature is conducive to PEI mounted molecule thus adds porosity, is conducive to CO
2molecule is in the diffusion of PEI@UiO-66 material internal; (2) CO
2the diffusion rate of molecule significantly increases along with the rising of temperature, thus further promotes CO
2diffusion rate in PEI@UiO-66 duct.And as temperatures as high 348 K, CO
2work adsorbance does not continue to raise but starts to decline, and is because after reaching uniform temperature, CO
2adsorption capacity and CO
2/ CH
4separation selectivity by Adsorption thermodynamics non-dynamics dominate, temperature raise thermodynamically be unfavorable for absorption, so when increasing the temperature to certain value, CO
2work adsorption capacity on PEI@UiO-66 and to CO
2/ CH
4separation selectivity all can decline.
Fig. 5 is that 4 embodiments are to CO
2work adsorption capacity and CO
2/ CH
4the block diagram of adsorptive selectivity.As seen from the figure: under moderate amount of moisture, PEI@UiO-66 material is to CO
2work adsorbance than there being obvious raising under drying condition, this is because under damp condition, amido: H
2o:CO
2the bicarbonate of temperature is generated with the reaction of the ratio of 1:1:1; And in dry conditions, amido: CO
2stable carbonate is generated with the reaction of the ratio of 1:2.But humidity continues to be increased to CO after 85% RH
2adsorbance declines on the contrary.This is mainly because the existence of large quantity of moisture is that competitive Adsorption effect becomes obvious, and hydrone occupies the CO on part PEI
2strong adsorption site causes CO
2adsorption potential reduces.
Claims (8)
1. a preparation method of metal-organic framework materials PEI UiO-66, is characterized in that comprising the steps:
(1) be added to by absolute ethyl alcohol in polymine (PEI), under normal temperature, the ultrasonic PEI that is mixed to dissolves, and obtains PEI/ absolute ethyl alcohol mixed liquor;
(2) step (1) gained PEI/ absolute ethyl alcohol mixed liquor is joined in UiO-66 material lentamente, then stir, obtain pasty mixture;
(3) by the pasty mixture of step (2) gained in N
2dry in atmosphere;
(4) step (3) resulting materials is carried out vacuum drying, obtain sorbing material and metal-organic framework materials PEI@UiO-66.
2. the preparation method of metal-organic framework materials PEI@UiO-66 according to claim 1, it is characterized in that: described in step (1), the mass ratio of absolute ethyl alcohol and polymine is 9 ~ 39, the described ultrasonic time is 5 ~ 20 min.
3. the preparation method of metal-organic framework materials PEI@UiO-66 according to claim 1, is characterized in that: described in step (2), the mass ratio of PEI/ absolute ethyl alcohol mixed liquor and UiO-66 is 1 ~ 16.
4. the preparation method of metal-organic framework materials PEI@UiO-66 according to claim 1, is characterized in that: the temperature of drying described in step (3) is 30 ~ 90 DEG C.
5. the preparation method of metal-organic framework materials PEI@UiO-66 according to claim 1, is characterized in that: described in step (4), vacuum drying temperature is 90 ~ 130 DEG C, and the time of described drying is 4 ~ 10 h.
6. the metal-organic framework materials PEI@UiO-66 obtained by preparation method described in any one of claim 1 ~ 5.
7. metal-organic framework materials PEI@UiO-66 described in claim 6 is at adsorbing separation CO
2in application, it is characterized in that: CO absorption
2time, the temperature of regulation and control feed gas and relative humidity, play the synergy of steam and PEI, improves sorbing material and metal-organic framework materials PEI@UiO-66 CO absorption
2capacity.
8. according to claim 7 application, it is characterized in that, be 25 ~ 75 DEG C by the temperature adjusting of feed gas; Relative humidity is regulated to 0 ~ 80 %.
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| CN113842885A (en) * | 2021-09-08 | 2021-12-28 | 中国科学院大连化学物理研究所 | Metal anchoring organic amine CO2Adsorbent, preparation and application thereof |
| CN113842885B (en) * | 2021-09-08 | 2024-03-08 | 中国科学院大连化学物理研究所 | Metal anchored organic amine CO 2 Adsorbent, preparation and application thereof |
| CN116603513A (en) * | 2023-06-12 | 2023-08-18 | 深碳科技(深圳)有限公司 | Solid amine adsorbent and preparation method thereof |
| CN116603513B (en) * | 2023-06-12 | 2024-02-20 | 深碳科技(深圳)有限公司 | Solid amine adsorbent and preparation method thereof |
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