CN110787584A - Application of cerium-based metal organic framework structure material in CO2Adsorption separation application of - Google Patents
Application of cerium-based metal organic framework structure material in CO2Adsorption separation application of Download PDFInfo
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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Abstract
The invention uses cerium-based metal organic framework structure material for CO2The adsorption separation application of (1). In the process of preparing the cerium-based metal organic framework structure powder material, the mixed solution containing the cerium source and the organic ligand is placed in the microwave reactor for reaction, so that the reaction time is greatly shortened, and the prepared Ce-MOF powder has good regular octahedral morphology, thereby effectively improving the synthesis efficiency of the Ce-MOF and reducing the energy consumption.
Description
Technical Field
The invention relates to the technical field of metal organic framework structure materials, in particular to a cerium-based metal organic framework structure material for CO2The adsorption separation application of (1).
Background
Excessive emission of carbon dioxide is a major concern worldwide, and china is one of the countries with the highest emission of carbon dioxide worldwide. Despite the use of renewable energy sources, many countries, including china, are still converting fossil fuels to meet the ever-increasing energy demand, with a further increase in global carbon dioxide emissions.
In recent years, carbon capture and sequestration have often been addressedAnd, that is, carbon dioxide is captured by various means and then stored or utilized. Common methods of carbon capture are: chemical absorption, adsorption, physical absorption, membrane separation, and the like. CO is common as the most commonly used-adsorption method2The adsorbent comprises zeolite, mesoporous silicon, active carbon, ionic liquid, solid material with amino, metal oxide, metal organic framework structure and the like. However, these materials have the disadvantages that: for example, solid materials with amino groups and metal oxides on CO2The adsorption capacity is low, and the energy consumption required during the cyclic utilization is large; zeolite, activated carbon and mesoporous silica material have good adsorption performance but have good CO adsorption performance2Specific adsorption performance is not available, and the adsorption performance is greatly influenced by temperature and water content; the metal-organic framework structure is ideal for CO due to the ultra-high specific surface area and the changeable metal ions and ligands2A material that specifically adsorbs.
In recent years, Metal Organic Framework Structures (MOFs) have attracted a wide interest as adsorbents. MOFs are crystalline porous materials with a specific topology and regular pore size formed by the coordination bonds of metal centers or clusters and organic linkers. Based on the diversity of metal ions, organic ligands, MOFs exhibit some unique advantages: for example, the longer the organic ligand, the more porosity and specific surface area the MOF may have; the structural elements of the MOF may be different metal ions or clusters and thus have different coordination structures; organic ligands also have different sizes, coordination structures, and organic ligands can carry various functional groups with reactivity, so MOFs show some modifiability. Based on the advantages, the MOF material has potential application value in the fields of gas adsorption and separation, catalysis, sensing, biological medicine and the like.
MOF materials as CO2Have achieved some success.
For example, -NH in the ligand2The introduction of functional groups will make the corresponding MOF materials towards CO2Has certain specific adsorption performance. However, in the ligand-NH2Functional groupThe introduction of the group makes the ligand difficult to synthesize, causes the ligand price to be higher, and is not beneficial to industrial application; and, the ligand has introduced-NH2The functional groups lead to a low chemical stability of the ligand and the corresponding MOFs are also not easily synthesized.
In addition, a large number of MOFs are unstable in air due to the presence of water molecules, and UiO-66 with a stable structure is an ideal CO2Adsorbent, UiO-66 measured on CO reported in literature2Has specific adsorption, and the maximum adsorption capacity is about 1.7 mmol-g-1. However, the metal source Zr of UiO-66 is expensive, and strong acid HCl is needed as an inhibitor during synthesis, which has certain influence on the environment and human health.
Therefore, the research and research have stable chemical property, low price and CO resistance2Specific adsorption of MOFs remains one of the challenges for those skilled in the art.
The rare earth element has a unique 4f electronic structure, so that the rare earth element is widely applied to the fields of light, electricity, magnetism, catalysis and the like. Of all rare earth elements, the abundance of cerium in the earth crust is 68ppm, which accounts for the first place of the total content of rare earth. The chemical property of cerium element is stable, and the electronic filling mode of the outer layer is 4f1，5d1，6s2Thus, cerium may be stably present in positive trivalent and tetravalent states. This variability in valence state allows the cerium element to behave differently than the other rare earth elements. Although China is the export country with the largest rare earth elements, the application of the rare earth elements is still short of results. Therefore, the cerium-based metal organic framework structure has great strategic significance and development prospect.
There are reports of CeO2As a catalyst for catalytic conversion of CO and elimination of volatile organic pollutants and the like, however, the report of Ce-MOF on CO is not available at present2Specific adsorption performance of (1).
Disclosure of Invention
In view of the above technical situation, the inventors of the present invention found that cerium-based metal organic framework (Ce-MOF) material can interact with CO after a large number of long-term experimental searches2Has high selective adsorption performance. Under the conditions of 1 atmosphere pressure and 0 ℃ temperature,to CO2The adsorption amount of (B) is 1.9 mmol/g-1Above, even 2.5 mmol/g-1And with CH4、N2In contrast, the adsorptive separation factor of the gas reaches over 10. Thus, Ce-MOF materials can be used for CO2The adsorption separation application of (1).
The adsorptive separation factor is determined by the following formula:
Sads＝q1p2/q2p1
wherein SadsTo adsorb the separation factor, qiAs the adsorption capacity (mmol. g) of component i-1)，piThe partial pressure (bar) of component i.
The Ce-MOF material is in a powder shape, and the particle size is preferably 0.5-10 μm, and more preferably 1-5 μm.
Preferably, the Ce-MOF powder has a specific surface area of 650-900m2/g。
Preferably, the Ce-MOF powder is in a regular octahedral microstructure.
In the present invention, the method for producing the Ce-MOF powder is not limited. Currently, a hydrothermal method is generally adopted to prepare the Ce-MOF, namely, a mixed solution containing cerium and an organic ligand is put into a reaction kettle, and is reacted for a certain time at a certain temperature to obtain a reaction product, and then the reaction product is washed, filtered and dried to obtain the Ce-MOF. However, the hydrothermal method requires a long reaction time, generally 24 hours or more, and thus consumes a high amount of energy, and the production rate of Ce-MOF powder having a good morphology is low.
Therefore, the inventors have conducted research and study on a method for producing Ce-MOF powder and found that: the reaction time can be greatly shortened by placing the mixed solution containing the cerium source and the organic ligand in a microwave reactor for reaction, the reaction product can be generated only in 1-2 hours, and the prepared Ce-MOF powder has good regular octahedron morphology, so that the synthesis efficiency of the Ce-MOF is effectively improved, and the energy consumption is reduced. The method is called as microwave method in the invention.
As one implementation, the method for preparing Ce-MOF powder employed in the present invention comprises the following steps:
1) dissolving ammonium ceric nitrate in water, and stirring to prepare liquid A; dissolving terephthalic acid in N, N-dimethylformamide, and stirring to prepare liquid B;
2) mixing the liquid A and the liquid B, slowly adding glacial acetic acid to prepare a mixed solution, and uniformly stirring;
preferably, the liquid A and the solution B are mixed and then placed in an ice bath for stirring, and then glacial acetic acid is slowly added;
3) pouring the mixed solution into a reaction kettle, placing the reaction kettle into a microwave reactor, and reacting for a certain time under a certain temperature condition to obtain a reaction product; then, the reaction product was washed, filtered and dried to obtain Ce-MOF powder.
Preferably, in the step (3), the power of the microwave reactor is 500-800W.
Preferably, in the step (3), the reaction temperature is 80-140 ℃.
Preferably, in the step (3), the reaction time is 0.5 to 6 hours, and more preferably 1 hour to 1.5 hours.
Preferably, in the step (1), the concentration of the cerium ammonium nitrate in the liquid A is 0.5 to 1 mol.L-1。
Preferably, in the step (1), the concentration of terephthalic acid in the liquid B is 0.05 to 0.1 mol.L-1。
Preferably, in the step (2), the volume ratio of the liquid A to the liquid B in the mixed solution is 1:5 to 1: 10.
Preferably, in the step (2), the amount ratio of the cerium ammonium nitrate to the glacial acetic acid in the mixed solution is 1:5-1: 50.
Compared with the prior art, the invention discovers that the Ce-MOF powder is used for treating CO2Has high selective adsorption performance, and can be used for CO2Adsorption and separation. In addition, the invention preferably adopts a microwave method to prepare the Ce-MOF powder, so that the reaction time can be greatly shortened, the energy consumption is reduced, the cost is saved, and the prepared Ce-MOF powder has good crystal form, high repeatability and excellent performance.
Drawings
FIG. 1 is an SEM photograph of octahedral Ce-MOF powder prepared by microwave and hydrothermal methods.
FIG. 2 is an XRD pattern of Ce-MOF powder prepared by microwave method and hydrothermal method.
FIG. 3 is a gas adsorption performance diagram of Ce-MOF powder synthesized by microwave method under different pressure conditions at 0 ℃.
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings, which are intended to facilitate the understanding of the present invention and are not intended to limit the present invention in any way.
Example 1:
(1) dispersing 5.18g of ammonium ceric nitrate in 20g of water, and uniformly stirring to obtain liquid A; dissolving 1.45g of terephthalic acid in 80ml of N, N-dimethylformamide and uniformly stirring to obtain a solution B; mixing the liquid A and the solution B, and then placing the mixture in an ice bath for stirring to obtain an orange yellow clear solution; 30ml of glacial acetic acid is added continuously and stirred to be uniform, so as to obtain a mixed solution.
(2) And transferring the mixed solution into a microwave reaction kettle, carrying out microwave reaction for 1h at 100 ℃, wherein the synthesis power is 800W, taking out a reaction product after the reaction is finished, washing the reaction product for multiple times by using N, N-dimethylformamide, and drying the washed powder in a drying oven at the temperature of 80 ℃ for 48h to obtain the Ce-MOF powder.
The obtained Ce-MOF powder is bright yellow, and an SEM picture of the powder is shown as a picture (a) in figure 1, so that the particle size of the powder is uniform and about 2 mu m, the powder has a regular octahedral shape, and the powder is good in stability in air and water.
The XRD pattern of the prepared Ce-MOF powder is shown as a curve marked by a microwave method in figure 2, and the Ce-MOF powder is highly crystallized and has no mixed crystal.
Experimental example 2:
(1) same as in step (1) in example 1;
(2) transferring the mixed solution into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 100 ℃ for 24h, taking out a reaction product after the reaction is finished, washing the reaction product for multiple times by using N, N-dimethylformamide, and drying the washed powder in a drying oven at 80 ℃ for 48h to obtain the powder.
The obtained Ce-MOF powder is bright yellow, and an SEM picture of the powder is shown in a (b) picture in figure 1, so that the particle size of the powder is uniform and about 2.5 mu m, the powder has a regular octahedral shape, and the powder is good in stability in air and water.
The XRD pattern of the prepared Ce-MOF powder is shown as a curve labeled 'hydrothermal method' in figure 2, and shows that the Ce-MOF powder is highly crystallized and has no mixed crystal.
Example 3:
(1) dispersing 2.59g of ammonium ceric nitrate in 20g of water, and uniformly stirring to obtain liquid A; dissolving 1.45g of terephthalic acid in 80ml of N, N-dimethylformamide and uniformly stirring to obtain a solution B; mixing the liquid A and the solution B, and then placing the mixture in an ice bath for stirring to obtain an orange yellow clear solution; 30ml of glacial acetic acid is added continuously and stirred to be uniform, so as to obtain a mixed solution.
(2) Same as step (2) in example 1;
example 4:
(1) dispersing 5.18g of ammonium ceric nitrate in 20g of water, and uniformly stirring to obtain liquid A; dissolving 1.45g of terephthalic acid in 80ml of N, N-dimethylformamide and uniformly stirring to obtain a solution B; mixing the liquid A and the solution B, and then placing the mixture in an ice bath for stirring to obtain an orange yellow clear solution; 10ml of glacial acetic acid is added continuously and stirred until the mixture is uniform, and a mixed solution is obtained.
(2) Same as step (2) in example 1;
example 5:
(1) same as in step (1) in example 1;
(2) and transferring the mixed solution into a microwave reaction kettle, carrying out microwave reaction for 2h at 60 ℃, wherein the synthesis power is 800W, taking out a reaction product after the reaction is finished, washing the reaction product for multiple times by using N, N-dimethylformamide, and drying the washed powder in a drying oven at the temperature of 80 ℃ for 48h to obtain the Ce-MOF powder.
Example 6:
(1) same as in step (1) in example 1;
(2) and transferring the mixed solution into a microwave reaction kettle, carrying out microwave reaction for 1h at 100 ℃, wherein the synthesis power is 700W, taking out a reaction product after the reaction is finished, washing the reaction product for multiple times by using N, N-dimethylformamide, and drying the washed powder in a drying oven at the temperature of 80 ℃ for 48h to obtain the Ce-MOF powder.
Example 7:
(1) same as in step (1) in example 1;
(2) and transferring the mixed solution into a microwave reaction kettle, carrying out microwave reaction for 2h at 100 ℃, wherein the synthesis power is 600W, taking out a reaction product after the reaction is finished, washing the reaction product for multiple times by using N, N-dimethylformamide, and drying the washed powder in a drying oven at the temperature of 80 ℃ for 48h to obtain the Ce-MOF powder.
CO-TREATMENT OF Ce-MOF POWDERS MADE OF EXAMPLES 1-72、CH4、N2The adsorption performance is tested, and the test equipment is as follows: hitachi S-4800 field emission scanning electron microscope; a physical adsorption analyzer model ASAP 2020 available from Micrometrics corporation. The test results of examples 1 and 2 are shown in FIG. 3.
The Ce-MOF prepared in the embodiments 1-7 show good CO under the conditions of 0 ℃ and different pressures2The adsorption performance is as follows:
as shown in FIG. 1, Ce-MOF prepared by microwave method in example 1 is coupled to CO2、、CH4、N2The maximum adsorption amount of (a) is 2.25 mmol/g-1、0.67mmol·g-1、0.14mmol·g-1。
EXAMPLE 2 Ce-MOF vs. CO prepared by hydrothermal method2、CH4、N2The maximum adsorption amount of the adsorbent reaches 2.3 mmol/g-1、0.64mmol·g-1、0.17mmol·g-1。
Ce-MOF to CO prepared by microwave method in EXAMPLE 32、CH4、N2The maximum adsorption amount of (a) is 2.35 mmol/g-1、0.68mmol·g-1、0.15mmol·g-1。
Ce-MOF vs. CO prepared by microwave method in EXAMPLE 42、CH4、N2The maximum adsorption amount of (a) is 1.91 mmol/g-1、0.62mmol·g-1、0.13mmol·g-1。
Ce-MOF vs. CO prepared by microwave method in EXAMPLE 52、CH4、N2The maximum adsorption amount of (a) is 2.5 mmol/g-1、0.71mmol·g-1、0.20mmol·g-1。
Ce-MOF vs. CO prepared by microwave method in EXAMPLE 62、CH4、N2The maximum adsorption amount of (a) is 2.38 mmol/g-1、0.66mmol·g-1、0.16mmol·g-1。
Ce-MOF vs. CO prepared by microwave method in EXAMPLE 72、CH4、N2The maximum adsorption amount of (a) is 2.1 mmol/g-1、0.61mmol·g-1、0.13mmol·g-1。
Thus, the Ce-MOF prepared in examples 1-7 can be used for CO2Adsorption and separation.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. Application of cerium-based metal organic framework structure material in CO2The adsorption separation application of (1).
2. The cerium-based metal organic framework material according to claim 1 for CO2The adsorption separation application is characterized in that: the cerium-based metal organic framework structure material can react with CO at the temperature of 0 ℃ under the pressure of 1 atmosphere2The adsorption amount of (B) is 1.9 mmol/g-1The above;
preferably, the cerium-based metal organic framework structure material is applied to CO at the temperature of 0 ℃ under the pressure of 1 atmosphere2The adsorption amount of (B) is 2.5 mmol/g-1。
3. The cerium-based metal organic framework material according to claim 1 for CO2Adsorption of (2)Separation application, which is characterized in that: and CH4、N2Compared with the cerium-based metal organic framework structure material, the cerium-based metal organic framework structure material has the advantages of CO2The adsorption separation factor of the gas reaches more than 10.
4. The cerium-based metal organic framework material according to claim 1 for CO2The adsorption separation application is characterized in that: the particle size of the cerium-based metal organic framework structure material is 0.5-10 μm, preferably 1-5 μm.
5. Use of a cerium-based metal organic framework material as claimed in any one of claims 1 to 4 for CO2The adsorption separation application is characterized in that: the cerium-based metal organic framework structure material is prepared by a hydrothermal method.
6. Use of a cerium-based metal organic framework material as claimed in any one of claims 1 to 4 for CO2The adsorption separation application is characterized in that: the preparation method of the cerium-based metal organic framework structure material comprises the following steps:
1) dissolving ammonium ceric nitrate in water, and stirring to prepare liquid A; dissolving terephthalic acid in N, N-dimethylformamide, and stirring to prepare liquid B;
2) mixing the liquid A and the liquid B, slowly adding glacial acetic acid to prepare a mixed solution, and uniformly stirring;
preferably, the liquid A and the solution B are mixed and then placed in an ice bath for stirring, and then glacial acetic acid is slowly added;
3) pouring the mixed solution into a reaction kettle, placing the reaction kettle into a microwave reactor, and reacting for a certain time under a certain temperature condition to obtain a reaction product; then, the reaction product was washed, filtered and dried to obtain Ce-MOF powder.
7. The cerium-based metal organic framework material according to claim 6 for CO2The adsorption separation application is characterized in that: in the step (3), the reaction time is 0.5h-6h, preferably 1h-1.5 h.
8. The cerium-based metal organic framework material according to claim 6 for CO2The adsorption separation application is characterized in that: in the step (3), the power of the microwave reactor is 500-800W.
9. The cerium-based metal organic framework material according to claim 6 for CO2The adsorption separation application is characterized in that: in the step (3), the reaction temperature is 80-140 ℃.
10. The cerium-based metal organic framework material according to claim 6 for CO2The adsorption separation application is characterized in that: in the step (1), the concentration of the ammonium ceric nitrate in the liquid A is 0.5-1 mol.L-1；
Preferably, in the step (1), the concentration of terephthalic acid in the liquid B is 0.05 to 0.1 mol.L-1；
Preferably, in the step (2), the amount ratio of the cerium ammonium nitrate to the glacial acetic acid in the mixed solution is 1:5-1: 50.
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|---|---|---|---|---|
| CN111450894A (en) * | 2020-05-02 | 2020-07-28 | 桂林理工大学 | Ce-based organic metal complex catalytic material and preparation and application thereof |
| CN111450894B (en) * | 2020-05-02 | 2023-10-13 | 桂林理工大学 | Ce-based organometallic complex catalytic material and preparation and application thereof |
| CN113087918A (en) * | 2021-03-04 | 2021-07-09 | 中国科学院宁波材料技术与工程研究所 | Zirconium-based metal organic framework material and preparation method and application thereof |
| CN113441114A (en) * | 2021-08-04 | 2021-09-28 | 辽宁大学 | Mixed metal MOF and preparation method and application thereof |
| CN114259837A (en) * | 2021-10-21 | 2022-04-01 | 江苏久亚机械科技有限公司 | Efficient capture method for carbon dioxide in flue gas |
| CN114259837B (en) * | 2021-10-21 | 2022-09-13 | 江苏久亚机械科技有限公司 | Efficient capture method for carbon dioxide in flue gas |
| CN114832012A (en) * | 2022-03-23 | 2022-08-02 | 复旦大学附属眼耳鼻喉科医院 | Ce-MOF nano material with oxidation resistance, preparation method and application |
| CN114832012B (en) * | 2022-03-23 | 2023-10-31 | 复旦大学附属眼耳鼻喉科医院 | Ce-MOF nano material with oxidation resistance, preparation method and application |
| CN115318284A (en) * | 2022-09-06 | 2022-11-11 | 上海应用技术大学 | Ru-based catalyst and preparation method and application thereof |
| CN115318284B (en) * | 2022-09-06 | 2024-02-27 | 上海应用技术大学 | Ru-based catalyst and preparation method and application thereof |
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