Method for preparing metal organic framework material UiO-66 in ethanol phase

A metal-organic framework and organic framework technology are applied in the preparation of metal-organic framework material UiO-66, and in the field of preparation of metal-organic framework material UiO-66 in ethanol phase under normal temperature conditions, which can solve the limitation of amplification reaction, increase production cost, Difficulty and other problems, to achieve the effect of reducing synthesis cost, reducing usage and overcoming low yield

Active Publication Date: 2017-09-15
TONGJI UNIV
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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
[0008] However, the synthesis methods of UiO-66(Zr) reported above all need to be carried out under heating conditions, organic solvents such as N,N-dimethylformamide will be used in the synthesis and preparation process, and the washing and activation process is cumbersome. Increased production costs and limited scale-up reactions

Method used

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  • Method for preparing metal organic framework material UiO-66 in ethanol phase
  • Method for preparing metal organic framework material UiO-66 in ethanol phase
  • Method for preparing metal organic framework material UiO-66 in ethanol phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 0.291 gZrCl respectively 4, 0.208 g of terephthalic acid in a mortar, grind vigorously for 10 minutes to make it evenly mixed, then transfer the mixture into a 10 mL ball milling jar, the volume ratio of large, medium and small ball milling beads is 1:6:3, the ball milling beads Accounting for 1 / 2 of the volume of the ball milling jar, the ball milling beads and the ball milling jar are made of alumina ceramics, milled at 420rpm for 2 h, take out the ball-milled mixture, add 5 mL of ethanol, and ultrasonicate for 15 minutes, at 600 The reaction was carried out at a stirring speed of rpm for 48 h.

[0036] The crude product after the reaction was obtained by centrifugation, washed with ethanol several times, and the washed crude product was vacuum-dried to obtain 0.157 g of the product with a yield of 51%. Through XRD analysis, its characteristic peak (see figure 2 ) and theoretically simulated characteristic peaks of UiO-66(Zr) (see figure 1 ) are consistent, ...

Embodiment 2

[0039] Weigh 0.402 gZrOCl respectively 2 •8H 2 O. 0.208 g of terephthalic acid was placed in a mortar, ground vigorously for 10 min to make it evenly mixed, and then the mixture was transferred into a 10 mL ball milling jar, the volume ratio of large, medium and small ball milling beads was 1:6:3, and ball milling Beads accounted for 1 / 2 of the volume of the ball milling jar, and the materials of both the ball milling beads and the ball milling jar were alumina ceramics. They were ball-milled for 2 h at a speed of 420 rpm, and the mixture that had been ball-milled was taken out, and 5 mL of ethanol was added. After ultrasonication for 15 minutes, the The reaction was carried out for 48 h at a stirring speed of 600 rpm.

[0040] The reacted crude product was obtained by centrifugation, washed with ethanol several times, and the washed crude product was vacuum-dried to obtain 0.160 g of the product with a yield of 52%. Through XRD analysis, its characteristic peak (see Figur...

Embodiment 3

[0042] Weigh 0.444gZr(SO 4 ) 2 • 4H 2 O. 0.208 g of terephthalic acid was placed in a mortar, ground vigorously for 10 min to make it evenly mixed, and then the mixture was transferred into a 10 mL ball milling jar, the volume ratio of large, medium and small ball milling beads was 1:6:3, and ball milling Beads accounted for 1 / 2 of the volume of the ball milling jar, and the materials of both the ball milling beads and the ball milling jar were alumina ceramics. They were ball milled for 2 h at a speed of 420 rpm, and the mixture that had been ball milled was taken out, and 5 mL of ethanol was added. After ultrasonication for 15 minutes, the The reaction was carried out for 48 h at a stirring speed of 600 rpm.

[0043] The reacted crude product was obtained by centrifugation, washed with ethanol several times, and the washed crude product was vacuum-dried to obtain 0.165 g of the product with a yield of 52%. Through XRD analysis, its characteristic peak (see Figure 5 ) an...

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Abstract

The invention relates to a method for preparing a metal organic framework material UiO-66 (Zr) in an ethanol phase. The method comprises the following steps: (1) uniformly mixing a zirconium source and an organic ligand, and pretreating for 1-3 hours so as to obtain an intermediate; (2) adding the intermediate into ethanol, stirring under a normal temperature condition, and centrifuging so as to obtain a crude product; and (3) washing the crude product for multiple times with ethanol, and drying, thereby obtaining the metal organic framework material UiO-66 (Zr). Compared with the prior art, the method is not involved with toxic organic solvents such as N,N-dimethyl formamide used in a conventional solvent thermal method, after the raw materials are pretreated, the UiO-66 (Zr) can be synthesized by using the ethanol as a solvent under the room temperature condition, the condition is gentle, the yield is relatively high, and large-scale synthesis of metal organic framework materials is possible.

Description

technical field [0001] The invention belongs to the field of metal-organic framework material preparation, and relates to a method for preparing metal-organic framework material UiO-66(Zr), in particular to a method for preparing metal-organic framework material UiO-66(Zr) in ethanol phase at normal temperature . Background technique [0002] Metal-organic framework materials (Metal-Organic Frameworks, referred to as MOFs) is a new type of porous material with a periodic 3D framework structure formed by self-assembly with metal ions as connection points with organic ligands, and has a mobilized pore structure. , huge specific surface area and modifiable functional functional groups, etc., the skeleton structure of the material can be adjusted according to the target requirements, and it is widely used in the fields of gas adsorption and storage, sensing and detection, drug delivery and reaction catalysis. Extensive research and application. [0003] UiO-66(Zr) is composed ...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 李风亭吴一楠侯书亮王颖李杰冯凌宇
Owner TONGJI UNIV
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