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Metal-organic frameworks based on co(ii) and their preparation methods and applications

A technology of metal-organic frameworks and organic ligands, applied in organic chemistry, cobalt-organic compounds, chemical instruments and methods, etc., can solve the problems of non-recyclable catalysts, complicated operations, and high costs

Inactive Publication Date: 2017-10-03
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above method has the problems of non-recyclable catalyst, high cost and complicated operation.

Method used

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  • Metal-organic frameworks based on co(ii) and their preparation methods and applications
  • Metal-organic frameworks based on co(ii) and their preparation methods and applications
  • Metal-organic frameworks based on co(ii) and their preparation methods and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Embodiment 1: the preparation of organic ligand L

[0060] Concrete preparation steps are as follows:

[0061] (1) 4,4-dibromobenzil (10.00g, 27.17mmol), ammonium acetate (41.89g, 543.45mmol), paraformaldehyde (1.63g, 54.34mmol), join in 100mL glacial acetic acid solution, stir Heat to reflux for 5 hours, adjust to neutral with saturated sodium carbonate solution after the reaction, extract with 200mL ethyl acetate, wash with sodium carbonate solution, extract the aqueous phase with ethyl acetate, combine the organic phases, and wash with anhydrous magnesium sulfate Dry, filter, and remove the solvent under reduced pressure to obtain 10.07 g of a yellow solid with a yield of 98.00%.

[0062]

[0063] (2)N 2 Under protection, intermediate A (10.58mmol, 4.00g) and sodium hydride (11.64mmol, 0.28g) were placed in a 100ml three-necked flask, and 50ml of anhydrous THF was slowly added as a solvent, heated to 80°C, and stirred at a constant temperature of 80°C for 1h , ...

Embodiment 2

[0068] Embodiment 2: Synthesis of Co-MOF-1

[0069] The organic ligand L (4.06mg, 0.01mmol) prepared in Example 1, terephthalic acid (1.66mg, 0.01mmol), cobalt acetate (0.01mmol, 2.13mg), were dissolved in 2mL of methanol, placed in a 5ml small In the test tube, the temperature was kept at 120°C for 72 hours, and the temperature was lowered to room temperature after 50 hours of programming to obtain purple-red blocky crystals {Co 3 L(BDC) 2.5 (OAc)(MeOH)}, yield 3.3 mg, yield 34% (based on L).

[0070] We characterized the compound by IR, TGA, and the infrared spectrum results of Co-MOF-1 are shown in Figure 7 , see the TGA spectrum Figure 8 .

Embodiment 3

[0071] Example 3: Synthesis of Co-MOF-2

[0072] The crystal of Co-MOF-1 prepared in Example 2 was placed in the air at room temperature for 24 hours, and then kept at 70°C for 2 hours to obtain the compound Co-MOF-2. We characterized the compound by IR and TGA, and the results are shown in Figure 9 , 10 .

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Abstract

The invention discloses an organic ligand L for synthesizing a Co(II)-based metal-organic framework, a Co(II)-based metal-organic framework Co-MOF-1, and a Co(II)-based metal-organic framework Co- MOF‑2. Firstly, the metal-organic framework Co‑MOF‑1 was synthesized by the organic ligand L, and then the crystal of Co‑MOF‑1 was placed in the air at room temperature for 24 hours, and then kept at 70°C for 2 hours to obtain a new type with active sites. Point Catalyst Co‑MOF‑2. The catalyst can effectively catalyze the oxidation reaction of cyclohexane, does not require heavy metals as catalysts, reduces the harm of heavy metals to the environment, has mild reaction temperature, short reaction time, less catalyst consumption, no other additives, and compared with free heavy metal salts , can be reused more than five times.

Description

technical field [0001] The invention relates to a metal organic framework based on Co(II) and its preparation method and application, belonging to the technical field of catalyst preparation. Background technique [0002] Metal-organic framework (Metal-organic Framework, MOF) is a research hotspot in recent years. Compared with traditional porous materials, MOF has porosity, larger specific surface area and pore volume in the framework, and is used as a porous functional material. Applications in catalysis show great advantages. [0003] The oxidation reaction of cyclohexane to prepare cyclohexanol and cyclohexanone (commonly known as KA oil) is an important reaction in industry. However, due to the low conversion rate and selectivity of this reaction process, serious pollution of three wastes and high energy consumption, this field has always been a hot and difficult point of research at home and abroad. At present, for the preparation of cyclohexanol and cyclohexanone by...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/06B01J31/22C07D401/14
Inventor 董育斌王建成马建平丁凤文刘启奎
Owner SHANDONG NORMAL UNIV
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