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A kind of mil-101 ​​material with high water stability and preparation method thereof

A stable and high-water technology, applied in the field of materials, can solve problems such as structural collapse, and achieve the effects of improved stability, high material yield, and reduced costs

Active Publication Date: 2022-03-29
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the carboxylic acid-based metal-organic framework series has high thermal stability, but when exposed to water at room temperature, the structure is very prone to collapse.

Method used

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  • A kind of mil-101 ​​material with high water stability and preparation method thereof
  • A kind of mil-101 ​​material with high water stability and preparation method thereof
  • A kind of mil-101 ​​material with high water stability and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Transition metal-doped bimetallic Ni / MIL-101 (Cr) material was prepared by the following method: Weigh 2.5mmol of organic ligand BDC into a 200mL glass beaker, add 70mL of distilled water, weigh chromium nitrate and nickel nitrate The solid is dissolved in the above distilled water, where Cr 3+ and Ni 2+ The total amount of is 2.5mmol, and the Ni / (Cr+Ni) molar ratio is 0.2. Add 0.35mmol of citric acid, and stir to mix the materials evenly. Afterwards, the mixed solution in the above system was transferred to a 100mL lined polytetrafluoroethylene autoclave reactor, and the reactor was placed in an oven for reaction, the temperature was adjusted to 220°C, and the time was set to 8h. After the reactor was cooled to room temperature, the resulting green solid was separated with a high-speed centrifuge. In order to remove the residual BDC in the solid, under the agitation of an electric stirrer, the obtained solid was washed twice with N,N-dimethylformamide, each washing ...

Embodiment 2

[0033]According to the synthesis method in Example 1, change the type and ratio of doped metal ions, under the condition that other conditions remain unchanged, when Ni / (Cr+Ni) is 0, the synthetic material is marked as MIL-101 (Cr), in When Ni / (Cr+Ni) is 0.2, the synthetic material is marked as Ni / MIL-101(Cr), when Cu / (Cr+Cu) is 0.2, the synthetic material is marked as Cu / MIL-101(Cr), and three The total amount of metal ions in each material is 2.5mmol. Weigh 1g of the obtained materials MIL-101(Cr), Cu / MIL-101(Cr) and Ni / MIL-101(Cr) respectively in a 50mL centrifuge tube, add 40mL Distilled water, stirred evenly, and left at room temperature. Take 0.15 g of solids at the bottom of the centrifuge tube on the 2nd, 4th, 6th, and 15th day respectively, and dry them in vacuum at 80°C for 16 hours. The obtained solid materials were subjected to characterization analysis. The XRD pattern of the sample is shown in Figure 2.

[0034] Such as Figure 2a As shown, the material MIL-101...

Embodiment 3

[0036] Synthesize materials MIL-101(Cr), Ni / MIL-101(Cr)-1, Ni / MIL-101(Cr)-2 according to the steps in Example 1, weigh 1g of the above three materials in 100mL saline bottle , add 50mL of distilled water and mix well, then let it stand at room temperature. Take the supernatant liquid on the 1st, 3rd, 5th, 7th, 10th, and 15th day respectively, filter through a 0.22 μm filter membrane and measure its chromium ion content by ion chromatography, which is the chromium ion leaching concentration of the material in distilled water, which is used to reflect Material stability in water.

[0037] The chromium ion leaching concentration of MIL-101(Cr), Ni / MIL-101(Cr)-1, Ni / MIL-101(Cr)-2 in distilled water changes with the leaching time as image 3 As shown, it can be seen that the chromium ion leaching concentration of the three materials increases with the prolongation of the leaching time, and the chromium ion leaching concentration of MIL-101(Cr) material is much higher than that of ...

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Abstract

The invention discloses a high water stability MIL-101 material and a preparation method thereof. The method introduces transition metal ions (such as Co 2+ 、Ni 2+ 、Cu 2+ , Zn 2+ etc.) as doping metals, with metal ions (Fe 3+ 、Cr 3+ 、Al 3+ ) to form competitive coordination, and add organic acids (such as citric acid, acetic acid, tartaric acid) as doping accelerators and take into account the role of mineralizers to synthesize bimetallic MIL‑101 materials doped with transition metal ions. After washing, use The acid solution with a pH value of (2~5) removes the coordination defect structure, and obtains a stable bimetallic MIL-101 material after drying. This method is green and convenient, and the synthesized bimetallic MIL-101 material has remarkable stability in water Improvement, and good synthesis reproducibility.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a highly water-stable MIL-101 material and a preparation method thereof. Background technique [0002] Metal-organic frameworks (MOFs) are crystalline porous materials with regular pore or hole structures formed by the self-assembly of inorganic metal centers and organic ligands. Due to its structural designability, diversity, tailorability and high specific surface area, this material has become a research hotspot of new materials in recent years, and has shown a wide range of applications in the fields of catalysis, separation, gas storage, bioconduction, and medical research. prospect. [0003] The stability of MOFs, especially water stability, has always been a bottleneck hindering their industrial application. For example, the carboxylic acid-based metal-organic framework series has high thermal stability, but when exposed to water at room temperature, the structure is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
Inventor 王艳韩劲椰万金泉马邕文
Owner SOUTH CHINA UNIV OF TECH