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Zirconium-based metal organic framework material UiO-66 (Zr) as well as room-temperature rapid preparation method and application thereof

An organic framework, uio-66 technology, applied in the field of metal-organic framework materials, can solve the problems of cumbersome washing and activation process, difficult microwave-assisted heating, and high cost

Active Publication Date: 2021-09-07
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is time-consuming, but it needs to add acetic acid and water as additives, and microwave-assisted heating is difficult to carry out scale-up experiments, and it is difficult to realize industrial production
[0009] The synthesis methods of UiO-66(Zr) reported above all require heating or pretreatment of the reactants. The synthesis process is complicated, the conditions are harsh, the reaction time is long, reaching more than 24h, and toxic organic substances such as N,N-dimethylformamide are used. solvent
Moreover, the washing and activation process is cumbersome and costly, making it difficult to scale up production

Method used

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  • Zirconium-based metal organic framework material UiO-66 (Zr) as well as room-temperature rapid preparation method and application thereof
  • Zirconium-based metal organic framework material UiO-66 (Zr) as well as room-temperature rapid preparation method and application thereof
  • Zirconium-based metal organic framework material UiO-66 (Zr) as well as room-temperature rapid preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Weigh 0.996g of terephthalic acid and 1.932g of zirconium oxychloride octahydrate into a 150ml beaker, add 100ml of methanol, and stir for 1 hour under magnetic stirring conditions and 350rpm. After the reaction is finished, centrifuge the white emulsion liquid obtained after stirring, and discard the transparent gel state intermediate product obtained after the supernatant liquid is discarded. The intermediate product was transferred to a blast oven, and heated and dried at 80° C. for 1 h to obtain 1.421 g of the final product with a yield of 85%. Characterized by XRD analysis ( figure 2 ), indicating that the product synthesized in this example is a typical zirconium-based metal-organic framework material UiO-66(Zr).

Embodiment 2

[0050] Weigh 0.996g of terephthalic acid and 1.932g of zirconium oxychloride octahydrate respectively into a 150ml beaker, add 100ml of methanol, and stir for 1h under magnetic stirring conditions at 350rpm. After the reaction, the white emulsion obtained after stirring was centrifuged, and the supernatant was discarded to obtain an intermediate product in a transparent gel state. The intermediate product was transferred to a blast oven, and heated and dried at 40° C. for 4 h to obtain 1.036 g of the final product with a yield of 62%. Characterized by XRD analysis ( image 3 ), indicating that the product synthesized in this example is a typical zirconium-based metal-organic framework material UiO-66(Zr).

Embodiment 3

[0052] Weigh 1.992g of terephthalic acid and 1.932g of zirconium oxychloride octahydrate into a 150ml beaker, add 100ml of methanol, and stir for 1 hour under magnetic stirring conditions at 350rpm. After the reaction, the white emulsion obtained after stirring was centrifuged, and the supernatant was discarded to obtain an intermediate product in a transparent gel state. The intermediate product was transferred to a blast oven, and heated and dried at 80° C. for 4 h to obtain 1.487 g of the final product with a yield of 89%. Characterized by XRD analysis ( Figure 4 ), indicating that the product synthesized in this example is a typical zirconium-based metal-organic framework material UiO-66(Zr).

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Abstract

The invention relates to a zirconium-based metal organic framework material UiO-66 (Zr) as well as a room-temperature rapid preparation method and application thereof. The preparation method comprises the following steps of: (1) uniformly mixing a zirconium source and an organic ligand, placing the mixture in methanol, stirring the mixtureat room temperature, performing centrifuging, and discarding clear liquid to obtain a transparent gel-state intermediate product; and (2) heating and drying the intermediate product to obtain the UiO-66 (Zr). Compared with the prior art, the UiO-66 (Zr) can be synthesized only by performing stirring in methanol at room temperature and performing drying without using toxic organic solvents such as N, N-dimethylformamide and the like in a traditional solvothermal method, the conditions are mild, the yield is higher, the synthesis time is greatly shortened, the product purity is extremely high, the step of activating the product can be omitted, the large-scale synthesis of the metal organic framework material is highly possible; and the material has good adsorption performance on fluorine ions in water, and can be applied to adsorption treatment of fluorine-containing wastewater.

Description

technical field [0001] The invention belongs to the technical field of metal-organic framework materials, and relates to a zirconium-based metal-organic framework material UiO-66(Zr), in particular to a zirconium-based metal-organic framework material UiO-66(Zr) and a rapid preparation method thereof at room temperature and Application of defluoridation in water. Background technique [0002] Metal-organic framework (Metal-organic framework), also known as metal-organic complexes or organic-inorganic hybrid materials, is a type of porous material formed by the self-assembly of metal salts and organic ligands. Due to the characteristics of high porosity, high specific surface area, adjustable pore size and structure, and structural and functional diversity, MOFs materials have attracted more and more attention from researchers in recent years. They are used in gas adsorption and storage, sensing and detection. , drug delivery and reaction catalysis have been widely studied a...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/22C02F1/28B01J20/30C02F101/14
CPCC08G83/008B01J20/226C02F1/285C02F2101/14C07F7/003
Inventor 吴一楠李风亭张彦星符家瑞
Owner TONGJI UNIV
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