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Method for synthesizing pure metal organic skeleton MIL-101 by one-step process

A technology of metal-organic frameworks and synthesis methods, applied in organic chemistry, chemical instruments and methods, compounds containing elements of group 6/16 of the periodic table, etc., can solve the problem of time-consuming and energy-consuming consumables, unfavorable synthesis and application of MIL-101 , Subsequent activation method to deal with complex problems, to achieve the effect of large specific surface area

Inactive Publication Date: 2014-01-08
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The follow-up activation method of this sample purification is complicated to deal with, and the consumables are time-consuming and energy-consuming, which is not conducive to the synthesis and application of MIL-101

Method used

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  • Method for synthesizing pure metal organic skeleton MIL-101 by one-step process
  • Method for synthesizing pure metal organic skeleton MIL-101 by one-step process
  • Method for synthesizing pure metal organic skeleton MIL-101 by one-step process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] According to the molar ratio: 1 terephthalic acid: 1 chromium nitrate: 50 water: 0.02 lithium acetate, add 0.82g terephthalic acid, 2g chromium nitrate, 0.01g lithium acetate to 5ml water in turn, stir evenly for 30min, then transfer into polytetrafluoroethylene The lined high-pressure hydrothermal reaction kettle was sealed and then crystallized at a constant temperature of 220°C for 8 hours. The crystallized product was washed with water and filtered to obtain a green sample. Through X-ray powder diffraction analysis (XRD), the crystals synthesized in this embodiment have the characteristic peaks of MIL-101 at 2.9°, 3.4°, 5.3°, 8.5°, and 9.2°, indicating that MIL-101 has been successfully synthesized. , and there is no characteristic peak of terephthalic acid at 2θ of 17.5°, indicating that the obtained crystal is pure MIL-101. Its BET specific surface area is 3102m 2 / g.

Embodiment 2

[0049] According to the molar ratio: 1 terephthalic acid: 1 chromium chloride: 150 water: 0.05 sodium acetate, add 0.82g terephthalic acid, 1.33g chromium chloride, 0.02g sodium acetate to 25ml water in turn, stir evenly for 30min, then move into poly Seal the tetrafluoroethylene-lined high-pressure hydrothermal reactor and crystallize at a constant temperature of 190°C for 24 hours. The crystallized product is washed with water and filtered to obtain a green sample. According to X-ray powder diffraction analysis (XRD), the crystal synthesized in this embodiment has a 2θ value of 2.9. , 3.4°, 5.3°, 8.5°, and 9.2°, the characteristic peaks of MIL-101 appeared, indicating that MIL-101 was successfully synthesized, and there was no characteristic peak of terephthalic acid at 2θ of 17.5°, indicating that the obtained crystal For pure MIL-101. Its BET specific surface area is 3093m 2 / g.

Embodiment 3

[0051] According to the molar ratio: 1 terephthalic acid: 1 chromium nitrate: 220 water: 0.15 potassium acetate, add 0.82g terephthalic acid, 2g chromium nitrate, and 0.12g potassium acetate to 20ml water in sequence, stir evenly for 30min, then transfer to polytetrafluoroethylene The lined high-pressure hydrothermal reaction kettle was sealed and then crystallized at a constant temperature of 200°C for 16 hours. The crystallized product was washed with water and filtered to obtain a green sample. Through X-ray powder diffraction analysis (XRD), the crystals synthesized in this embodiment have the characteristic peaks of MIL-101 at 2.9°, 3.4°, 5.3°, 8.5°, and 9.2°, indicating that MIL-101 has been successfully synthesized. , and there is no characteristic peak of terephthalic acid at 2θ of 17.5°, indicating that the obtained crystal is pure MIL-101. Its BET specific surface area is 3342m 2 / g.

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Abstract

The invention belongs to a synthesis method of metal organic framework, and discloses a one-step method for synthesizing pure metal organic framework MIL-101. In this method, the mineralizer is added to water, dissolved, then organic ligands are added, stirred, and then metal chromium salts are added. After the resulting mixture is stirred evenly, it is crystallized at a constant temperature, filtered, washed, and dried to obtain a pure MIL-101 sample; wherein : The mineralizer is a substance that provides acetate; the organic ligand is terephthalic acid; the metal chromium salt is a water-soluble chromium salt. The present invention does not require cumbersome subsequent activation processes, and can synthesize pure MIL-101 in one step. The obtained MIL-101 has a larger specific surface area, and is simple, easy to operate, time-saving and energy-saving compared to the existing technology.

Description

technical field [0001] The invention belongs to a method for synthesizing a metal-organic framework, and relates to a method for synthesizing a pure metal-organic framework MIL-101 in one step. Background technique [0002] Metal-Organic Frameworks (MOFs), also known as Metal-Organic Networks or Organic-Inorganic Hybrid Materials. This type of material is a new type of zeolite-like porous material formed by the self-assembly of transition metals and multi-dentate organic ligands. Due to the characteristics of high porosity, high specific surface area, adjustable pore size and structure, and structural and functional diversity, MOFs have attracted more and more attention from researchers in recent years. [0003] Metal-organic framework MIL-101 is a new type of MOF material first synthesized and reported by the French Ferey research group. The material has a large specific surface area (Langmuir specific surface area: 4500-5500m 2 / g) and pore volume (702000A3), and can ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F11/00
Inventor 郭金涛孙贻白马正飞陈勇李金锋
Owner NANJING TECH UNIV