CN113441114A - Mixed metal MOF and preparation method and application thereof - Google Patents
Mixed metal MOF and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a mixed metal MOF and a preparation method and application thereof. The technical scheme is as follows: weighing zirconyl nitrate solution and ceric ammonium nitrate solution, mixing uniformly, adding terephthalic acid, N-dimethylformamide and formic acid in sequence, and mixing uniformly to obtain mixed solution; placing the obtained mixed solution in an ultrasonic reactor, and performing ultrasonic action at 323 +/-10K for 20-40 min; cooling to room temperature, centrifuging, washing with N, N-dimethylformamide and acetone in sequence, and drying to obtain the target product. The mixed metal MOF prepared by the invention has excellent adsorption effect on carbon dioxide. Compared with a liquid phase synthesis method, the preparation method of the mixed metal MOF has the characteristics of mild conditions, high yield, large-scale production and the like.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a preparation method and application of mixed metal MOF (Metal organic framework), namely Zr/Ce-UiO-66.
Background
Mofs (metal Organic framework) refers to a crystalline porous material with a periodic network structure formed by metal ions and Organic ligands. The MOFs have a nano-scale pore channel and cage structure similar to those of the traditional zeolite materials, and have the advantages of various structures, easily adjustable pore diameter, large specific surface area and the like. Most MOFs have limited kinds of structural units which are periodically and repeatedly arranged, so that the channel structure and the environment are relatively single. This uniqueness makes its own functionality unable to meet the rapidly increasing demands of practical applications. And the mixed metal MOFs enriches the pore channel structure and environment of the MOFs material by introducing various construction units. The possible synergy between different building blocks of mixed metal MOFs provides superior properties and functions more readily than mechanical mixing of the unit MOFs materials. At present, the metal-mixed MOFs are highly concerned by researchers in the application fields of adsorption and separation, energy storage and conversion, heterogeneous catalysis and the like.
Environmental issues and energy shortages are major challenges facing the world at present and are also major issues that must be prioritized in our country for implementing the strategy of sustainable development. Carbon dioxide is a greenhouse gas that can cause the greenhouse effect. With economic development and advances in industry, the level of carbon dioxide in the atmosphere is further increased by burning the gases emitted mainly from coal, oil and natural gas. The global warming and climate change caused by energy depletion and greenhouse gases all over the world are obvious in developing countries, so effective control and reduction of carbon dioxide emission are one of the problems to be solved urgently, and therefore, the development of CO with large adsorption capacity2Adsorbents are particularly important.
Disclosure of Invention
The invention aims to synthesize mixed metal MOF (metal organic framework), namely Zr/Ce-UiO-66, by a simple and rapid method and research the performance of the mixed metal MOF as a carbon dioxide adsorption material.
The technical scheme adopted by the invention is as follows: a mixed metal MOF, which is a metal organic framework material Zr/Ce-UiO-66 loaded with metal zirconium and cerium, wherein the molar ratio of Zr to Ce is (1-5) to (5-1).
A method for preparing a mixed metal MOF, comprising the steps of:
1) weighing zirconyl nitrate solution and ceric ammonium nitrate solution, mixing, and sequentially adding terephthalic acid (H)2DBC)、NN-Dimethylformamide (DMF) and formic acid (HCOOH) are uniformly mixed to obtain a mixed solution;
2) placing the obtained mixed solution in an ultrasonic reactor, and performing ultrasonic action at 323 +/-10K for 20-40 min;
3) cooling to room temperature, centrifuging, washing with DMF and acetone sequentially, and drying to obtain the target product.
Preferably, in the above preparation method, the sum of the zirconium ion and the cerium ion is 1:1 in terms of molar ratio.
The invention provides application of mixed metal MOF as an adsorption material in carbon dioxide adsorption.
Preferably, the method is as follows: putting the mixed metal MOF into a container, controlling the temperature at 273-298K, and introducing CO2And standing for adsorption. More preferably, the control temperature is 273K.
The invention has the beneficial effects that:
1. the mixed metal MOF prepared by the invention has the advantages of simple preparation method, high yield and great application prospect. The mixed metal MOF enriches the pore structure and environment of the MOF material by introducing various construction units, and has good carbon dioxide adsorption effect.
2. According to the preparation method of the mixed metal MOF material, an ultrasonic method is adopted in the whole process, and the rapid synthesis of the mixed metal MOF under mild conditions is realized. Such material is on CO2Has high adsorption capacity, and can be used for industrial CO2High-efficiency adsorption.
Drawings
FIG. 1 is a PXRD spectrum of mixed metal MOFs prepared with different Zr and Ce molar ratios.
FIG. 2 is an infrared spectrum of mixed metal MOFs prepared with different Zr and Ce molar ratios.
FIG. 3 is a mixed metal MOF Zr prepared with a Zr to Ce molar ratio of 1:51Ce5PXRD pattern after 24 hours of treatment of ulio-66 soaked in different solvents.
FIG. 4 is a mixed metal MOF Zr prepared with a 2:4 molar ratio of Zr to Ce2Ce4PXRD pattern after 24 hours of treatment of ulio-66 soaked in different solvents.
FIG. 5 isMixed metal MOF Zr prepared by using Zr and Ce in molar ratio of 3:33Ce3PXRD pattern after 24 hours of treatment of ulio-66 soaked in different solvents.
FIG. 6 is a graph of mixed metal MOFs prepared with different Zr and Ce molar ratios at 273K vs. CO2Adsorption isotherm of (1).
FIG. 7 is a graph of mixed metal MOFs prepared with different Zr and Ce molar ratios at 298K vs. CO2Adsorption isotherm of (1).
Detailed Description
Example 1 Mixed Metal MOF (Zr)5/Ce1-UiO-66)
The preparation method comprises the following steps:
1.0mL of an aqueous zirconium oxynitrate solution (0.5M), 0.2mL of an aqueous cerium ammonium nitrate solution (0.5M), and 128.0mg of terephthalic acid (H)2DBC), 4mL of N, N-Dimethylformamide (DMF) and 1mL of formic acid are added into a glass bottle with the volume of 20mL, and after uniform mixing, the mixture is placed in an ultrasonic reactor and is subjected to ultrasonic treatment at 323K for 25min to obtain a white solid. Centrifuging, washing with DMF and acetone sequentially, and drying to obtain the target product, wherein the molar ratio of Zr to Ce is 5:1 and is recorded as Zr5/Ce1-UiO-66, yield 62.5%. (yield-mass of actual product/mass of theoretical product).
Example 2 Mixed Metal MOF (Zr)4/Ce2-UiO-66)
The preparation method comprises the following steps:
0.8mL of an aqueous zirconium oxynitrate solution (0.5M), 0.4mL of an aqueous cerium ammonium nitrate solution (0.5M), and 128.0mg of terephthalic acid (H)2DBC), 4mL of N, N-Dimethylformamide (DMF) and 1mL of formic acid are added into a glass bottle with the volume of 20mL, and after uniform mixing, the mixture is placed in an ultrasonic reactor and is subjected to ultrasonic treatment at 323K for 25min to obtain a white solid. Centrifuging, washing with DMF and acetone sequentially, and drying to obtain the target product, wherein the molar ratio of Zr to Ce is 4:2, and the molecular weight is recorded as Zr4/Ce2-UiO-66, yield 61.7%. (yield-mass of actual product/mass of theoretical product).
Example 3 Mixed Metal MOF (Zr)3/Ce3-UiO-66)
The preparation method comprises the following steps:
0.6mL of an aqueous zirconium oxynitrate solution (0.5M), 0.6mL of an aqueous cerium ammonium nitrate solution (0.5M), and 128.0mg of terephthalic acid (H)2DBC), 4mL of N, N-Dimethylformamide (DMF) and 1mL of formic acid are added into a glass bottle with the volume of 20mL, and after uniform mixing, the mixture is placed in an ultrasonic reactor and is subjected to ultrasonic treatment at 323K for 25min to obtain a white solid. Centrifuging, washing with DMF and acetone sequentially, and drying to obtain the target product, wherein the molar ratio of Zr to Ce is 3:3 and is recorded as Zr3/Ce3-UiO-66, yield 62.2%. (yield-mass of actual product/mass of theoretical product).
Example 4 Mixed Metal MOF (Zr)2/Ce4-UiO-66)
The preparation method comprises the following steps:
0.4mL of an aqueous zirconium oxynitrate solution (0.5M), 0.8mL of an aqueous cerium ammonium nitrate solution (0.5M), and 128.0mg of terephthalic acid (H)2DBC), 4mL of N, N-Dimethylformamide (DMF) and 1mL of formic acid are added into a glass bottle with the volume of 20mL, the mixture is uniformly mixed and placed in an ultrasonic reactor, ultrasonic treatment is carried out for 25min at 323K to obtain a white solid, the white solid is centrifuged, washed by DMF and acetone in sequence and dried to obtain a target product, and the molar ratio of Zr to Ce is 2:4 and is recorded as Zr2/Ce4-UiO-66, yield 60.7%. (yield-mass of actual product/mass of theoretical product).
Example 5 Mixed Metal MOF (Zr)1/Ce5-UiO-66)
The preparation method comprises the following steps:
0.2mL of an aqueous zirconium oxynitrate solution (0.5M), 1.0mL of an aqueous cerium ammonium nitrate solution (0.5M), and 128.0mg of terephthalic acid (H)2DBC), 4mL of N, N-Dimethylformamide (DMF) and 1mL of formic acid are added into a glass bottle with the volume of 20mL, the mixture is uniformly mixed and placed in an ultrasonic reactor, ultrasonic treatment is carried out for 25min at 323K to obtain a white solid, the white solid is centrifuged, washed by DMF and acetone in sequence and dried to obtain a target product, and the molar ratio of Zr to Ce is 1:5 and is recorded as Zr1/Ce5-UiO-66, yield 62.8%. (yield-mass of actual product/mass of theoretical product).
Using X-ray powder diffraction, as shown in FIG. 1The PXRD of the mixed metal MOF obtained in examples 1 to 5, i.e., Zr/Ce-UiO-66, was measured. As can be seen from FIG. 1, Zr1/Ce5-UiO-66、Zr2/Ce4-UiO-66、Zr3/Ce3-UiO-66、Zr4/Ce2-UiO-66、Zr5/Ce1The PXRD pattern of-UiO-66 shows characteristic peaks at 2 θ ═ 7.34 °, 8.51 °, 12.04 °, 14.08 °, 17.02 °, 22.11 °, 25.64 ° and 33.23 °, respectively, which are consistent with the diffraction peaks of UiO-66, thus indicating that mixed metal MOF, i.e. Zr/Ce-UiO-66, was successfully synthesized.
As shown in FIG. 2, the mixed metal MOF obtained in examples 1 to 5, namely Zr, was analyzed by Fourier Infrared spectrometer1/Ce5-UiO-66、Zr2/Ce4-UiO-66、Zr3/Ce3-UiO-66、Zr4/Ce2-UiO-66、Zr5/Ce1-UiO-66 by IR spectroscopy. 1580cm, as can be seen in FIG. 2-1And 1600cm-1The characteristic peak is caused by stretching vibration of the carbon skeleton of the benzene ring and is about 1400cm-1The characteristic peak is the symmetrical stretching vibration peak of carboxyl in the terephthalic acid ligand, 550cm-1The characteristic peaks on the left and right are the characteristic vibration peaks of Zr/Ce-O bonds, which indicates that the mixed metal MOF, namely Zr/Ce-UiO-66, is successfully synthesized.
Fig. 3-5 are PXRD patterns of mixed metal MOFs after 24 hours of treatment in different solvents. Adding Zr1Ce5-UiO-66，Zr2Ce4-UiO-66 and Zr3/Ce3And (3) soaking the-UiO-66 in 1, 4-dioxane, tetrahydrofuran, dichloromethane, methanol and DMA for 24 hours respectively, separating and drying, and performing PXRD test on the soaked mixed metal MOF to find that the structure is not changed, thereby indicating that the mixed metal MOF has excellent chemical stability.
Example 6 use of Mixed Metal MOFs as adsorbent materials for carbon dioxide adsorption
CO treatment of the Mixed Metal MOFs prepared in examples 1 to 52And (5) performing adsorption test.
The method comprises the following steps:
the mixed metal MOF prepared in example 1-example 5 was vacuum activated at 423K for 8-10 h.
CO regulation2The output pressure is about 0.34MPa, 200mg of the mixed metal MOF samples prepared in the example 1-the example 5 after activation are respectively placed in different sample tubes, and then CO is introduced into the sample tubes2Controlling the temperature of the sample tube to be 273K or 298K respectively, and determining the mixed metal MOF to CO2The amount of adsorption. The results are shown in table 1, fig. 6 and fig. 7.
TABLE 1 CO of Mixed Metal MOFs at 1bar, 273K and 298K2Adsorption capacity of
FIG. 6 is a graph of mixed metal MOFs for different Zr and Ce molar ratios prepared in example 1-example 5 at 273K vs. CO2Adsorption isotherm of (1). FIG. 7 is a comparison of mixed metal MOFs of example 1-example 5 with different Zr and Ce molar ratios at 298K for CO2Adsorption isotherm of (1). Analysis of FIG. 6 shows that at a temperature of 273K, the pressure P (actual pressure) reaches 760 mmHg (i.e., P/P)0Close to 1), mixed metal MOF Zr prepared in example 51/Ce5The highest adsorption capacity of the-UiO-66 to the carbon dioxide can reach 44.0cm3(ii) in terms of/g. Analysis of FIG. 7 shows that at a temperature of 298K, the pressure P (actual pressure) reaches 760 mmHg (i.e., P/P)0Close to 1), mixed metal MOF Zr prepared in example 51/Ce5The highest absorption capacity of the-UiO-66 to carbon dioxide can reach 24.6cm3/g。
As can be seen from table 1, fig. 6 and fig. 7, the mixed metal MOF showed excellent carbon dioxide adsorption performance, and the adsorption capacity of the same adsorbent to carbon dioxide at low temperature was much better than that at higher temperature. Mixing metals in different proportions at different temperatures, with Zr1/Ce5The best effect of the-UiO-66 on the adsorption of carbon dioxide is achieved.
The foregoing detailed description is only for the purpose of explaining the technical solutions of the present application in detail, and the present application is not limited to the foregoing embodiments, and it should be understood by those skilled in the art that all modifications, substitutions and alterations based on the above principles and spirit should be within the scope of the present application.
Claims (6)
1. The mixed metal MOF is a metal organic framework material Zr/Ce-UiO-66 loaded with metal zirconium and cerium, and the molar ratio of Zr to Ce is (1-5) to (5-1).
2. A preparation method of mixed metal MOF is characterized by comprising the following steps:
1) weighing zirconyl nitrate solution and ceric ammonium nitrate solution, mixing uniformly, adding terephthalic acid, N-dimethylformamide and formic acid in sequence, and mixing uniformly to obtain mixed solution;
2) placing the obtained mixed solution in an ultrasonic reactor, and performing ultrasonic action at 323 +/-10K for 20-40 min;
3) cooling to room temperature, centrifuging, washing with N, N-dimethylformamide and acetone in sequence, and drying to obtain the target product.
3. The method of claim 2, wherein: the sum of zirconium ion and cerium ion is 1:1 in terms of molar ratio.
4. Use of a mixed metal MOF of claim 1 as an adsorbent material for adsorbing carbon dioxide.
5. Use according to claim 4, characterized in that the method is as follows: placing the mixed metal MOF of claim 1 in a vessel, controlling the temperature at 273-2And standing for adsorption.
6. Use according to claim 5, wherein the control temperature is 273K.
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| CN115337915A (en) * | 2022-08-18 | 2022-11-15 | 中国科学院过程工程研究所 | Metal organic framework composite material with core-shell structure and preparation method and application thereof |
| CN115672402A (en) * | 2022-10-24 | 2023-02-03 | 河南大学 | Anion-cation co-doped modified UiO-66 and preparation method and application thereof |
| CN116239786A (en) * | 2023-03-17 | 2023-06-09 | 辽宁大学 | Metal organic framework material for separating carbon dioxide mixed gas, and preparation method and application thereof |
| CN116351405A (en) * | 2023-04-18 | 2023-06-30 | 大连中汇达科学仪器有限公司 | Gas-phase capillary column using UiO-66 as adsorbent and manufacturing method and application thereof |
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| CN115337915B (en) * | 2022-08-18 | 2023-12-12 | 中国科学院过程工程研究所 | Metal organic framework composite material with core-shell structure and preparation method and application thereof |
| CN115672402A (en) * | 2022-10-24 | 2023-02-03 | 河南大学 | Anion-cation co-doped modified UiO-66 and preparation method and application thereof |
| CN115672402B (en) * | 2022-10-24 | 2024-02-06 | 河南大学 | Anion-cation co-doping modified UiO-66 and preparation method and application thereof |
| CN116239786A (en) * | 2023-03-17 | 2023-06-09 | 辽宁大学 | Metal organic framework material for separating carbon dioxide mixed gas, and preparation method and application thereof |
| CN116351405A (en) * | 2023-04-18 | 2023-06-30 | 大连中汇达科学仪器有限公司 | Gas-phase capillary column using UiO-66 as adsorbent and manufacturing method and application thereof |
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