Thorium-based metal organic framework material and preparation method and application thereof

An organic framework and base metal technology, applied in the field of thorium-based metal-organic framework materials and their preparation, can solve the problems of unfavorable MOFs crystal structure analysis, poor solubility of coordination products, rapid nucleation and other problems, and achieve a clear and stable crystal structure. Simple and fast method, high-purity effect

Active Publication Date: 2021-10-15
EAST CHINA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

At present, researchers have synthesized many types of metal-organic framework materials, among which researchers have conducted in-depth and extensive research on metal-organic frameworks with actinides as the coordination core, but the tetravalent metal clusters and multi-dentate carboxylic acid The strong affinity of the ligands often leads to problems such as poor solubility, rapid nucleation and easy precipitation of the coordination products, and finally produces polycrystalline powder or amorphous products instead of single crystal products, which is not conducive to the analysis of the crystal structure of MOFs

Method used

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  • Thorium-based metal organic framework material and preparation method and application thereof
  • Thorium-based metal organic framework material and preparation method and application thereof
  • Thorium-based metal organic framework material and preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0026] A method for preparing a thorium-based metal-organic framework material, comprising the following steps:

[0027] Step 1. Weigh 0.0121g (0.05mmol) of terphenyl dicarboxylic acid ligand and 0.0024g (0.05mmol) of thorium nitrate tetrahydrate metal salt using a ten-thousandth balance, and then add 3mL of N,N'-dicarboxylate Methylformamide and stir well; then slowly add the tetramethylguanidine chloride ionic liquid of 0.0076g (0.05mmol) in the mixed solution, and transfer to the polytetrafluoroethylene liner of hydrothermal reactor, at room temperature Ultrasonic treatment for 20min;

[0028] Step 2. Then seal the PTFE lining, then put it into the stainless steel outer tank, tighten the outer tank and put it in a muffle furnace for heating. The temperature is raised to 120 °C at a heating rate of 2 °C / min, and then the temperature is kept at 120 °C. React for 72 hours, then cool to room temperature at a cooling rate of 1°C / min, filter under reduced pressure to obtain bloc...

Embodiment 2

[0030] The structure of the thorium-based metal-organic framework material obtained in Example 1 is determined, and its scanning electron microscope photo is as follows: figure 2 As shown, the measured single crystal size of the material is 0.01mm×0.01mm×0.02mm.

[0031] Select moderately sized crystals under a microscope, and use Mo-Kα monochromated by a graphite monochromator using a RigakuSuperNova single crystal diffractometer at 293K Target collection data (CrysAlisPro software was used for data collection and reduction; the crystal structure was obtained using the SHELXTL-2104 program, and all non-hydrogen atoms were refined using the full-matrix least squares method; all non-hydrogen atoms were anisotropically refined ; the hydrogen atom on the ligand is produced by geometric symmetry and the C-H bond length is ). The obtained structure diagram is shown in Figure 3-Figure 6 . The specific crystallographic data are shown in Table 1.

[0032] Table 1

[0033] ...

Embodiment 3

[0037] The morphological characterization of the thorium-based metal-organic framework material obtained in Example 1 was determined. Specifically, the powder diffraction data was obtained by fitting the single crystal structure using the Mercury program, and compared with the actual measured powder diffraction data of the thorium-based metal-organic framework material. data for comparison. Such as Figure 7 As shown, after comparison, it can be found that the diffraction peak positions of the experimental data and the simulated data are basically consistent. and from Figure 8 In the shown Fourier transform infrared spectrum, it can be found that the peak intensity of the organic functional groups in the framework structure is well maintained. It can be seen that the purity and structure of the thorium-based metal organic framework material obtained in Example 1 are consistent with the experimental fitting structure.

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Abstract

The invention discloses a thorium-based metal organic framework material and a preparation method and application thereof. The structural unit of the material is [Th6O4(OH)4(tpda)6], and tpda represents terphenyl dicarboxylic acid anions without two hydroxyl H atoms. The method comprises the following steps: uniformly mixing terphenyl dicarboxylic acid ligand, thorium nitrate tetrahydrate metal salt and tetramethylguanidine chloride ionic liquid step by step, and reacting under a heating condition through self-generated pressure to obtain crystals of the thorium-based metal organic framework material. The preparation method is simple and rapid, metal thorium is not agglomerated with the polydentate carboxylic acid ligand tpda, abundant coordination geometric structures and more leading-edge electron orbits can be formed, formation of different secondary building units and topology types is promoted, and the prepared thorium-based metal organic framework material is clear and stable in crystal structure, high in purity and suitable for industrial production. The method can be better applied to analysis and research of MOFs crystal structures, and has a wide application prospect in the field of adsorption and separation of radionuclides.

Description

technical field [0001] The invention belongs to the field of crystalline materials, and in particular relates to a thorium-based metal-organic framework material and its preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs) are organic-inorganic hybrid materials with intramolecular voids formed by the self-assembly of organic ligands and metal ions. Since MOFs are usually connected by organic ligands and metal nodes, they have the advantages of clear spatial structure, uniform pore size, adjustable pore size, and large specific surface area. At present, researchers have synthesized many types of metal-organic framework materials, among which researchers have conducted in-depth and extensive research on metal-organic frameworks with actinides as the coordination core, but the tetravalent metal clusters and multi-dentate carboxylic acid The strong affinity of the ligands often leads to problems such as poor solubility, rapid nucleat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 徐珍珍陶源余峰涛范丽晶
Owner EAST CHINA UNIV OF TECH
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