CN117772121A - Ag-loaded MOF composite material and preparation method and application thereof - Google Patents
Ag-loaded MOF composite material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 239000012924 metal-organic framework composite Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052704 radon Inorganic materials 0.000 claims abstract description 40
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- OYFRNYNHAZOYNF-UHFFFAOYSA-N 2,5-dihydroxyterephthalic acid Chemical compound OC(=O)C1=CC(O)=C(C(O)=O)C=C1O OYFRNYNHAZOYNF-UHFFFAOYSA-N 0.000 claims abstract description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
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- 239000007787 solid Substances 0.000 claims abstract description 3
- 239000012265 solid product Substances 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000012621 metal-organic framework Substances 0.000 abstract description 6
- 230000003993 interaction Effects 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 239000002131 composite material Substances 0.000 description 12
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- 206010058467 Lung neoplasm malignant Diseases 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
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- 239000004566 building material Substances 0.000 description 2
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
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- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to the technical field of gas adsorption materials, in particular to an Ag-loaded MOF composite material and a preparation method and application thereof, wherein the preparation method comprises the steps of pouring nickel nitrate hexahydrate and 2, 5-dihydroxyterephthalic acid into a mixed solution of DMF, ethanol and deionized water, stirring at 100-130 ℃, refluxing, reacting for 24-48 hours, centrifuging after the reaction is finished, and drying the obtained solid product in a vacuum oven to obtain MOF-74Ni; placing MOF-74Ni in a vacuum oven, performing first activation for 12-24 h at 150-200 ℃, then soaking the activated MOF-74Ni in silver nitrate solution for 24-48 h, and placing the filtered solid in the vacuum oven for second activation to obtain the MOF composite material. According to the invention, silver is loaded on the MOF, and the strong dipole-induced dipole interaction exists among the Ag clusters, so that the adsorption capacity to radon is remarkably improved, and the application of the adsorption material in the radon adsorption field is widened.
Description
Technical Field
The invention relates to the technical field of gas adsorption materials, in particular to an Ag-loaded MOF composite material, and a preparation method and application thereof.
Background
Radon gas is the only one of the common radon gases with half-life of 3.8235 daysGases, which are all composed of radioactive isotopes under normal conditions, are constantly released from uranium-containing minerals in rock and soil. The radon gas with higher concentration is accumulated in the environments such as underground array land and underground engineering, near-ground floors and basements of urban low-lying areas in mountain cities, mining and metallurgy, rock, building materials and the like, and causes health hazard to practitioners. It is reported that in closed spaces such as underground mines or houses, the dose of ionizing radiation generated by radon gas is about 52% of the dose of ionizing radiation received by individuals. Epidemiological studies provide a great deal of evidence that indoor radon exposure can lead to lung cancer even at relatively low radon levels. Radon is considered to be the first cause of lung cancer in non-smokers, and the world health organization ranks radon as one of 19 major environmental carcinogens and recommends indoor use 222 Reference level of Rn is now 200Bqm -3 Down to 100Bqm -3 。
At present, three methods of reducing the radon precipitation, ventilating dilution and adsorption enrichment are mainly adopted in domestic and foreign radon reduction measures. Spraying radon-proof paint on building materials, floors or walls with high radon exhalation rate to block radon release, but cannot guarantee long-term effectiveness of sealing; the indoor radon concentration can be effectively reduced by increasing the air circulation quantity and diluting the indoor radon concentration, but the energy consumption is higher and the implementation operation in an underground closed space is more difficult; the method can be used for reducing the indoor radon concentration through activated carbon adsorption enrichment, fiber filtration purification technology, biological filtration technology, electrostatic dust collection technology and the like, and the activated carbon is the earliest material for radon adsorption research and is the radon absorbing material which is commercially available at present. Although the activated carbon has a certain effect on adsorbing radon, the adsorption of radon gas is mainly physical adsorption, and the saturated adsorption capacity is not high, mainly because micropores (< 2 nm) with actual adsorption blocking effect on radon account for the limited effective volume mass fraction of the activated carbon. In the prior art, although the activated carbon has a certain effect on adsorbing radon, the adsorption of the activated carbon on radon gas is mainly physical adsorption, and the saturated adsorption capacity is not high, mainly because micropores (< 2 nm) with an actual adsorption blocking effect on radon account for the limited effective volume mass fraction of the activated carbon. The metal-organic framework Material (MOFs) is a novel material, is rich in variety, and has high porosity, large specific surface area and adjustable pore size structure. Therefore, the MOFs material with different pore sizes or different pore structures is designed and prepared by utilizing the coordination of the connecting ligands with different lengths and the metal ions, and the MOFs material is hopeful to provide a new material selection for radon adsorption.
Disclosure of Invention
In view of the above, the invention aims to provide an Ag-loaded MOF composite material, and a preparation method and application thereof, so as to at least solve the problem that the effective volume mass fraction of micropores (< 2 nm) of the prior active carbon with actual radon adsorption blocking effect is limited.
The invention solves the technical problems by the following technical means:
one aspect of the present invention is to provide a method for preparing an Ag-loaded MOF composite, comprising the steps of:
pouring nickel nitrate hexahydrate and 2, 5-dihydroxyterephthalic acid into a mixed solution of DMF, ethanol and deionized water, stirring at 100-130 ℃, refluxing, reacting for 24-48 hours, centrifuging after the reaction is finished, and drying the obtained solid product in a vacuum oven to obtain MOF-74Ni;
placing 3-7 parts by weight of MOF-74Ni into a vacuum oven, performing first activation for 12-24 hours at 150-200 ℃, then soaking the activated MOF-74Ni into silver nitrate solution for 24-48 hours, and placing the filtered solid into the vacuum oven for second activation to obtain the MOF composite material.
Optionally, ni in the nickel nitrate hexahydrate 2+ The molar ratio of the catalyst to the 2, 5-dihydroxyterephthalic acid is (5-7): (1-3).
Optionally, the volume ratio of DMF, ethanol, and deionized water is 4: (3.5-5.8): (0.7-1.2).
Optionally, the rotational speed of the centrifugation is 8000-10000 r/min.
Optionally, the drying condition is that the temperature is 60-80 ℃ and the drying time is 6-12 hours.
Optionally, the concentration of the silver nitrate is 5-100 mmol/L.
Optionally, the condition of the second activation is that the temperature is 200-250 ℃ and the activation is carried out for 12-15 h.
The invention further provides the Ag-loaded MOF composite material prepared by the preparation method.
Still another aspect of the present invention is to provide the use of the Ag-loaded MOF composite described above in radon adsorption.
According to the preparation method of the Ag-loaded MOF composite material, the MOF-74Ni is prepared by a one-step solvothermal method, and silver nano particles are successfully loaded in the porous material MOF-74Ni by a deposition method. On the basis of maintaining the surface area of the dispersed silver-loaded MOF, the strong dipole-induced dipole interaction exists among the Ag clusters, so that the adsorption capacity of radon is remarkably improved, the application of the adsorption material in the radon adsorption field is widened, and a feasible scheme is further provided for the radon adsorption material.
According to the Ag-loaded MOF composite material, on one hand, MOF-74Ni is adopted as a matrix material, and the aperture structure with larger specific surface area and rich unsaturated metal active sites of the MOF-74Ni are utilized, so that the composite material has a good radon adsorption effect; on the other hand, ag is loaded on the MOF-74Ni, and the interaction force between the adsorption material and radon is enhanced by utilizing the polarization effect of the Ag on the radon, so that the adsorption capacity is improved.
Drawings
FIG. 1 is an XRD pattern of an Ag@MOF-74Ni material obtained at different mass fractions of silver nitrate solutions;
FIG. 2 is a 10mmolAg loaded Ag@MOF-74Ni and MOF-74Ni N 2 Adsorption graph.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following examples were conducted under conventional conditions or conditions recommended by the manufacturer, without specifying the specific conditions. The raw materials, equipment or instruments used are conventional products commercially available without identifying the manufacturer.
Specifically, please refer to the following examples:
example 1
The preparation method of the Ag-loaded MOF composite material of the embodiment is as follows:
9.6g of nickel nitrate hexahydrate and 1.98g of 2, 5-dihydroxyterephthalic acid (DHTA) were poured into a mixed solution of 40ml of DMF, 40ml of ethanol and 10ml of deionized water, and the mixture was stirred at 100℃and reacted under reflux for 24 hours. After the reaction, the product was separated by centrifugation at 8000r/min and dried in a vacuum oven at 60℃for 8 hours. 3.3g of the synthesized MOF-74Ni is placed in a vacuum oven and is pretreated for 12 hours at 150 ℃; then, soaking the activated MOF-74Ni in 5mmol/L, 10mmol/L and 100mmol/L of silver nitrate solution for 24 hours to obtain an Ag@MOF-74Ni composite material; and finally, placing the prepared Ag@MOF-74Ni composite material in a vacuum oven and activating for 12 hours at 200 ℃ to obtain the MOF composite material.
Example 2
The preparation method of the Ag-loaded MOF composite material of the embodiment is as follows:
7.58g of nickel nitrate hexahydrate and 2.17g of 2, 5-dihydroxyterephthalic acid (DHTA) were poured into a mixed solution of 30ml of DMF, 26ml of ethanol and 10ml of deionized water, and the mixture was stirred at 110℃and refluxed for 24 hours. After the reaction, the product was separated by centrifugation at 8000r/min and dried in a vacuum oven at 60℃for 8 hours. Placing 4g of the synthesized MOF-74Ni in a vacuum oven, and pre-treating for 12 hours at 200 ℃; then, soaking the activated MOF-74Ni in 5mmol/L, 10mmol/L and 100mmol/L of silver nitrate solution for 24 hours to obtain an Ag@MOF-74Ni composite material; and finally, placing the prepared Ag@MOF-74Ni composite material in a vacuum oven to activate for 12 hours at 220 ℃ to obtain the MOF composite material.
Example 3
The preparation method of the Ag-loaded MOF composite material of the embodiment is as follows:
10.58g of nickel nitrate hexahydrate and 4.15g of 2, 5-dihydroxyterephthalic acid (DHTA) were poured into a mixture of 100ml of DMF, 87ml of ethanol and 30ml of deionized water, and reacted under reflux with stirring at 120℃for 48h. After the reaction, the product was separated by centrifugation at 10000r/min and dried in a vacuum oven at 80℃for 12h. 5g of the synthesized MOF-74Ni is taken and placed in a vacuum oven, and is pretreated for 24 hours at 150 ℃; then, respectively soaking the activated MOF-74Ni in 10mmol/L, 20mmol/L and 120mmol/L of silver nitrate solution for 48 hours to obtain an Ag@MOF-74Ni composite material; and finally, placing the prepared Ag@MOF-74Ni composite material in a vacuum oven to activate for 12 hours at 240 ℃ to obtain the MOF composite material.
Example 4
The preparation method of the Ag-loaded MOF composite material of the embodiment is as follows:
14.54g of nickel nitrate hexahydrate and 4.08g of 2, 5-dihydroxyterephthalic acid (DHTA) were poured into a mixed solution of 80ml of DMF, 116ml of ethanol and 14ml of deionized water, and the mixture was stirred at 130℃and reacted under reflux for 24 hours. After the reaction, the product was separated by centrifugation at 8000r/min and dried in a vacuum oven at 80℃for 12h. 7g of the synthesized MOF-74Ni is taken and placed in a vacuum oven, and is activated and pretreated for 24 hours at 150 ℃; then, respectively soaking the activated MOF-74Ni in 15mmol/L, 50mmol/L and 150mmol/L of silver nitrate solution for 24 hours to obtain an Ag@MOF-74Ni composite material; and finally, placing the prepared Ag@MOF-74Ni composite material in a vacuum oven to activate for 15 hours at the temperature of 250 ℃ to obtain the MOF composite material.
Example 5
The preparation method of the Ag-loaded MOF composite material of the embodiment is as follows:
a mixed solution of 20.35g of nickel nitrate hexahydrate and 2.17g of 2, 5-dihydroxyterephthalic acid (DHTA) was poured into 30ml of DMF, 25ml of ethanol and 10ml of deionized water, and the mixture was stirred at 110℃and refluxed for 24 hours. After the reaction, the product was separated by centrifugation at 8000r/min and dried in a vacuum oven at 60℃for 8 hours. Placing 4g of the synthesized MOF-74Ni in a vacuum oven, and pre-treating for 12 hours at 200 ℃; then, soaking the activated MOF-74Ni in 5mmol/L, 10mmol/L and 100mmol/L of silver nitrate solution for 24 hours to obtain an Ag@MOF-74Ni composite material; and finally, placing the prepared Ag@MOF-74Ni composite material in a vacuum oven to activate for 12 hours at 220 ℃ to obtain the MOF composite material.
Comparative example 1
9.6g of nickel nitrate hexahydrate and 1.98g of 2, 5-dihydroxyterephthalic acid (DHTA) were poured into a mixed solution of 40ml of DMF, 40ml of ethanol and 10ml of deionized water, and the mixture was stirred at 100℃and reacted under reflux for 24 hours. After the reaction, the product was separated by centrifugation at 8000r/min and dried in a vacuum oven at 60℃for 8 hours to obtain MOF-74Ni.
The materials prepared in example 1 and comparative example 1 were subjected to performance characterization or testing as follows:
(1) Structural characterization
The results of the test analysis of example 1 and comparative example 1 using an X-ray diffractometer are shown in fig. 1. The data of FIG. 1 shows that the Ag peak intensity at (111) in Ag@MOF-74Ni increases with increasing silver concentration in the material; at the same time (111) Ag diffraction peaks confirm the presence of Ag metal in the pores.
Characterization analysis was performed on example 1 and comparative example 1 using a BET specific surface area analyzer, and the results are shown in FIG. 2 and Table 1, wherein (5 mmol/L) Ag@MOF74 Ni represents MOF74 Ni immersed in 5mmol/L silver nitrate solution, and the prepared MOF composite material is composed of (10 mmol/L) Ag@MOF74 Ni and (100 mmol/L) Ag@MOF74 Ni.
Table 1:
the data of FIG. 2 and Table 1 show that the slave material is N 2 As a result of adsorption, the specific surface area of the Ag-supported MOF-74Ni material was found to be onlySlightly reduced, i.e., the reduced amplitude was small, less than 15%, indicating that the addition of Ag had little effect on the porosity of the MOF-74Ni material itself.
(2) Penetration experiment of Rn
First, all test samples were in an oil bath at 130℃N 2 Purging for 2h, degassing and activating for 12h under the vacuum condition of 10Pa, weighing 1g of each activated sample in a vacuum glove box, respectively loading into sample loading columns, and testing radon concentration change of a circulatory system every 10min as a period. After about 3 hours, on the premise of ensuring the stability of the instrument test, after the material is connected into a drying column, the dynamic adsorption data of the test material on radon is recorded. The results are shown in Table 2.
Table 2:
the data in Table 2 show that under the condition that the temperature and the humidity of the environment are controlled to be the same, the dynamic adsorption coefficient of the prepared Ag@MOF-74Ni composite material to radon is higher than that of the MOF-74Ni material without Ag, and the half penetration time is relatively longer, so that the adsorption capacity of the Ag to radioactive radon is obviously improved by adding the Ag. Therefore, the Ag-loaded MOF composite material can be applied to radon adsorption.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (10)
1. The preparation method of the Ag-loaded MOF composite material is characterized by comprising the following steps of:
pouring nickel nitrate hexahydrate and 2, 5-dihydroxyterephthalic acid into a mixed solution of DMF, ethanol and deionized water, stirring at 100-130 ℃, refluxing, reacting for 24-48 hours, centrifuging after the reaction is finished, and drying the obtained solid product in a vacuum oven to obtain MOF-74Ni;
placing 3-7 parts by weight of MOF-74Ni into a vacuum oven, performing first activation for 12-24 hours at 150-200 ℃, then soaking the activated MOF-74Ni into silver nitrate solution for 24-48 hours, and placing the filtered solid into the vacuum oven for second activation to obtain the MOF composite material.
2. The method for producing an Ag-supported MOF composite according to claim 1, wherein Ni in the nickel nitrate hexahydrate 2+ The molar ratio of the catalyst to the 2, 5-dihydroxyterephthalic acid is (5-7): (1-3).
3. The method for preparing an Ag-loaded MOF composite according to claim 2, wherein the volume ratio of DMF, ethanol and deionized water is 4: (3.5-5.8): (0.7-1.2).
4. The method for preparing an Ag-supported MOF composite according to claim 3, wherein the rotational speed of the centrifugation is 8000-10000 r/min.
5. The method for preparing an Ag-supporting MOF composite according to claim 4, wherein the drying condition is drying at 60-80℃for 6-12 h.
6. The method for producing an Ag-supported MOF composite according to claim 5, wherein the concentration of silver nitrate is 5 to 100mmol/L.
7. The method for preparing an Ag-supported MOF composite according to claim 6, wherein the second activation is performed at a temperature of 200 to 250 ℃ for 12 to 15 hours.
8. An Ag-loaded MOF composite material, wherein the MOF composite material is prepared by the preparation method according to any one of claims 1 to 7.
9. The Ag-loaded MOF composite according to claim 8, wherein the specific surface area of the MOF composite is 1301 to 1434m 2 /g。
10. Use of an Ag-loaded MOF composite according to claim 8 or 9 in radon adsorption.
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