Method for preparing mixed-valent-state iron doped zeolite imidazate skeleton nano-material

A zeolite imidazolate and mixed valence technology, which is applied in the field of preparation of mixed valence iron-doped metal organic framework nanomaterials, can solve problems such as difficulty in regulating the concentration of iron ions, and achieves fewer synthesis regulation parameters, mild conditions, and high production efficiency. simple method effect

CN110724272AInactive Publication Date: 2020-01-24BEIJING UNIV OF CHEM TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2020-01-24
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a method for preparing a mixed-valent-state iron doped zeolite imidazate skeleton nano-material. The method comprises the steps of simultaneously dispersing bivalent and trivalent iron salts and zinc nitrate into a methanol solvent to form an iron-zinc precursor solution, mixing a 2-methylimidazole methanol solution with the precursor solution, placing the mixture in an oil bath with the temperature of 40 DEG C to 100 DEG C, carrying out a sustained magnetic stirring reaction, and then, subjecting a product to centrifugation, washing and drying treatment, thereby obtaining the mixed-valent-state iron doped zeolite imidazate skeleton nano-material. The mixed-valent-state iron doped zeolite imidazate skeleton nano-material with relatively high yield and uniform and controllable particle size is obtained. According to the method disclosed by the invention, the total iron doped amount can reach 50% to the maximum through adjusting a ratio of bivalent iron salts totrivalent iron salts, and conversion ratios of zinc ions and iron ions can separately reach up to 78% and 60%. The method is simple and economical, and reacted mother liquor can be reused. The obtained nano-material has a relatively high active oxygen generating efficiency under ultrasonic induction, has a tremendous application value in degradation of environmental pollutants and sonodynamic therapy of tumors and can be applied to preparation of high-concentration monoatomic iron-carbon based catalysts.
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Description

Technical field:

[0001] The invention belongs to the technical field of functional nanometer materials, and in particular relates to a preparation method of mixed valence iron doped metal organic framework nanomaterials. Background technique:

[0002] Metal-organic frameworks (MOFs) are porous materials with a three-dimensional spatial network structure formed by transition metal ions and organic ligands through coordination self-assembly, and the formed porous structure materials exhibit unique physical properties of nanomaterials at the nanoscale. Chemical properties (such as controllable size, large specific surface area, high chemical stability, etc.). In particular, using the space confinement effect of metal-organic frameworks, transition metal single-atom carbon-based nanomaterials with high catalytic activity can be prepared under high-temperature pyrolysis conditions, showing broad applications in the fields of energy, catalysis, and biomedicine. Value. For exampl...

Examples

Embodiment 1

[0034] Weigh 11.65mmol zinc nitrate, 0.124mmol ferrous ammonium sulfate and 0.124mmol ferric ammonium sulfate and disperse in 600mL methanol solvent to form zinc-iron metal cation precursor A solution; weigh 56mmol 2-methylimidazole ligand and disperse in 600mL methanol A solution B is formed in a solvent; the two solutions A and B are mixed, and placed in an oil bath at 60°C, and after 24 hours of magnetic stirring at 300 rpm, the formed product is centrifuged, washed, and vacuum-dried to prepare The final mixed valence iron doping-ZIF-8 nanomaterial, the prepared sample TEM picture is shown in figure 1 . Compared with other embodiments, two metal salts with similar properties are used in this example to obtain a higher iron doping amount. Quantitative analysis of elemental indications shows that the total iron doping amount is calculated to be 50%.

Embodiment 2

[0036] Weigh 11.65mmol zinc nitrate, 0.124mmol ferrous sulfate and 0.062mmol ferric nitrate and disperse in 300mL methanol solvent to form zinc-iron metal cation precursor A solution; weigh 56mmol 2-methylimidazole ligand and disperse in 300mL methanol solvent Form B solution; mix A and B solutions, place them in an oil bath at 40°C, and react with magnetic stirring at 400 rpm for 36 hours, then centrifuge, wash, and vacuum-dry the formed product to prepare the final Mixed valence iron-doped-ZIF-8 nanomaterial, the XRD pattern of the obtained sample is shown in figure 2 .

Embodiment 3

[0038] Weigh 11.65mmol zinc nitrate, 0.124mmol ferrous sulfate and 0.248mmol ferric chloride and disperse in 200mL methanol solvent to form zinc-iron metal cation precursor A solution; weigh 56mmol 2-methylimidazole ligand and disperse in 200mL methanol solvent Form B solution; mix A and B solutions, put them in an oil bath at 100°C, and react with magnetic stirring at 200 rpm for 16 hours, then centrifuge, wash, and vacuum-dry the formed product to prepare the final product The mixed valence state iron-doped-ZIF-8 nanometer material, the XRD pattern of the obtained sample is shown in figure 2 .