Preparation method of metal-organic framework material mil-88b(fe)

A metal-organic framework and organic ligand technology, applied in the preparation of metal-organic framework material MIL-88B, the preparation field of metal-organic framework material MIL-88B under normal temperature conditions, can solve the complicated washing and activation process, amplification reaction limitation, Improve production costs and other issues to achieve the effects of reducing synthesis costs, reducing usage, and reducing energy consumption

Active Publication Date: 2018-04-20
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] However, the synthesis methods of MIL-88B(Fe) 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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  • Preparation method of metal-organic framework material mil-88b(fe)
  • Preparation method of metal-organic framework material mil-88b(fe)
  • Preparation method of metal-organic framework material mil-88b(fe)

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Weigh 0.354g Fe(NO 3 ) 3 9H 2 O. Put 0.146g of terephthalic acid in a mortar, grind vigorously for 10min to make it evenly mixed, and then transfer the mixture into a 10mL ball mill jar. The volume ratio of large, medium and small ball milling beads is 1:6:3. Occupying 1 / 2 of the volume of the ball milling jar, the materials of the ball milling beads and the ball milling jar are both alumina ceramics, milled at a speed of 420rpm for 1 hour, took out the ball-milled mixture, transferred it to a 20mL glass bottle, added 5mL of ethanol, and ultrasonicated After 15 minutes, the reaction was carried out at a stirring speed of 600 rpm for 12 hours.

[0045] The reacted crude product was obtained by centrifugation, washed with ethanol several times, and the washed crude product was vacuum-dried to obtain 0.1568 g of the product with a yield of 51%. Through XRD analysis, its characteristic peak (see figure 2 ) and fitted MIL-88B(Fe) characteristic peaks (see figure 1 ) ar...

Embodiment 2

[0047] Weigh 0.354g Fe(NO 3 ) 3 9H 2 0.0.146g of terephthalic acid in a mortar, grind vigorously for 15min to make it evenly mixed, then move the mixture into a 10mL ball mill jar, the volume ratio of the large, medium and small ball mill beads is 1:6:3, Occupying 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 a speed of 420rpm for 2h, take out the ball-milled mixture, transfer it to a 20mL glass bottle, add 5mL of ethanol, and ultrasonically After 15 minutes, react at 600 rpm for 12 hours.

[0048] The reacted crude product was obtained by centrifugation, washed with ethanol for several times, and the washed crude product was vacuum-dried to obtain 0.1682 g of the product with a yield of 54%. Through XRD analysis, its characteristic peak (see Figure 4 ) and fitted MIL-88B(Fe) characteristic peaks (see figure 1 ) are consistent, indicating that the obtained crystals are pure MIL-88B(Fe), ...

Embodiment 3

[0050] Weigh 0.237g FeCl respectively 3 ·6H 2 O. Put 0.146g terephthalic acid in a mortar, grind vigorously for 10min to make it evenly mixed, then move the mixture into a 10mL ball mill jar, the volume ratio of large, medium and small ball mill beads is 1:6:3, accounting for 1 / 2 of the tank volume, the ball milling beads and the ball milling tank are made of alumina ceramics, milled at 420rpm for 1h, take out the ball-milled mixture, transfer it to a 20mL glass bottle, add 5mL of ethanol, and ultrasonicate for 15min , Reacted for 12h at a stirring speed of 600rpm.

[0051] The reacted crude product was obtained by centrifugation, washed several times with ethanol, and vacuum-dried the washed crude product to obtain 0.1864 g of the product with a yield of 60%. Through XRD analysis, its characteristic peak (see Figure 6 ) and fitted MIL-88B(Fe) characteristic peaks (see figure 1 ) are consistent, indicating that the obtained crystals are pure MIL-88B(Fe), and the results o...

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Abstract

The invention relates to a preparation method of a metal organic framework material MIL-88B(Fe). The preparation method comprises following steps: 1, an iron source and an organic ligand are mixed to be uniform, and are subjected to pretreatment for 1 to 3h so as to obtain an intermediate; 2, the intermediate is added into ethanol solvent, and an obtained mixture is stirred at room temperature, and then is subjected to centrifugation so as to obtain a crude product; 3, the crude product is washed with ethanol for a plurality of times, and then is dried so as to obtain the metal organic framework material MIL-88B(Fe). Compared with the prior art, toxic organic solvents such as N,N-dimethylformamide used in conventional solvothermal method is not used, ethanol is taken as a solvent, the raw material is subjected to pretreatment, synthesis of MIL-88B(Fe) is realized at room temperature, the conditions are mild, yield is relatively high, and it is possible to realize large-scale synthesis of metal organic framework materials.

Description

technical field [0001] The invention belongs to the field of preparation of metal organic framework materials, and relates to a preparation method of metal organic framework material MIL-88B(Fe), in particular to a preparation method of metal organic framework material MIL-88B(Fe) under normal temperature conditions. Background technique [0002] Metal-organic framework materials are porous materials with ordered pores and periodic grid structures formed by self-assembly of inorganic metal ion centers and organic ligands. MOFs materials have a huge specific surface area, adjustable pore size, and abundant unsaturated active sites to choose from, and have gradually become one of the research hotspots in the field of material synthesis. The outstanding structural features make MOFs have potential applications in the fields of gas storage, drug delivery, adsorption separation, and chemical catalysis. [0003] MIL-88B(Fe) is a three-dimensional framework structure with micropor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 吴一楠李风亭张冰如侯书亮马小亮
Owner TONGJI UNIV
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