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Four co(ii)-based metal-organic frameworks and their preparation methods and applications

A metal-organic framework and reaction technology, applied in the field of Co-based metal-organic frameworks and their preparation, can solve the problems of poor stability, inability to recycle, and complicated preparation steps.

Inactive Publication Date: 2018-03-23
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing metal-organic frameworks have problems as a Lewis acid catalyst: poor stability, cumbersome preparation steps, low activity, and non-recyclability

Method used

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  • Four co(ii)-based metal-organic frameworks and their preparation methods and applications
  • Four co(ii)-based metal-organic frameworks and their preparation methods and applications
  • Four co(ii)-based metal-organic frameworks and their preparation methods and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] The preparation of organic ligand L, the specific preparation steps are as follows:

[0068] N 2 Under protection, 2,5-dibromopyridine (2.37g, 10mmol), 1,2,4-triazole (1,66g, 24mmol), cesium carbonate (13.03g, 40mmmol), cuprous iodide (0.76g, 4mmol) was placed in a 100mL three-necked flask, 20mL DMF was used as a solvent, heated to 120°C, followed by TLC, poured into 400mL water after the reaction was completed, left to stand, suction filtered, and after the solid was dried, it was subjected to silica gel column chromatography (dichloromethane: methanol =20:1), 1.49 g of white solid was obtained with a yield of 75%.

[0069]

[0070] Structural characterization of the organic ligand L prepared in this example, its 1 HNMR, IR respectively as Figure 11 , 12 shown.

Embodiment 2

[0071] Embodiment 2: Synthesis of Co-MOF-1

[0072] The L (3.0mg, 0.014mmol) prepared in Example 1, isophthalic acid (2.5mg, 0.015mmol) Co(CH 3 COO) 2 4H 2 O (3.7mg, 0.015mmol) was dissolved in 2mL of methanol, placed in a 5mL small test tube, kept at 120°C for 72 hours, then cooled down to room temperature for 48 hours to obtain pink blocky crystals [Co(C 9 h 7 N 7 )(C 8 h 4 o 4 )0.75MeOH] n , yield 3.3 mg, yield 46.5% (based on L).

[0073] The compound was characterized by IR, and the results are shown in Figure 13 .

Embodiment 3

[0074] Example 3: Synthesis of Co-MOF-2

[0075] L (3.0mg, 0.014mmol), 5-methylisophthalic acid (2.7mg, 0.015mmol) Co(CH 3 COO) 2 4H 2 O (3.7mg, 0.015mmol) was dissolved in 2mL of methanol and dimethylacetamide, the volume ratio of methanol and dimethylacetamide was (1-2): (1-2), placed in a 5mL small test tube, 120 Keep the temperature at ℃ for 72 hours, then cool down to room temperature for two days after 48 hours to get pink blocky crystals [Co 2 (C 9 h 7 N 7 ) 2 (C 9 h 6 o 4 ) 2 ] n , the yield was 3.1 mg, and the yield was 41% (based on L).

[0076] The compound was characterized by IR, and the results are shown in Figure 14 .

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Abstract

The invention discloses four metal organic frames based on Co (II) and a preparation method and application of the four metal organic frames. The prepared metal organic frames can be adopted as a lewis acid catalyst for catalyze a chemical reaction, a Knoevenagel condensation reaction is efficiently catalyzed, a weak base catalyst reaction is not needed, corrosion of reaction liquid to a reaction container is reduced, reaction temperature is moderate, reaction time is short, the amount of the adopted catalyst is small, no other additives are needed, and compared with homogeneous catalysis, the metal organic frames can be repeatedly utilized five times or above.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, in particular to four Co(II)-based metal-organic frameworks and their preparation methods and applications Background technique [0002] Metal-organic framework (Metal-organic Framework, MOF) is a research hotspot in recent years. It has similarities with traditional metal-organic complexes, and is the combination product of organic molecules and metals; however, it shows different characteristics. MOF has porosity, large specific surface area and pore volume in the framework, and is more difficult to dissolve in most organic solvents than metal-organic complexes. As a porous functional material, it shows great advantages in the application of heterogeneous catalysis. . The Knoevenagel condensation reaction is a dehydration condensation reaction of carbonyl compounds and active methylene compounds. It is used for the formation of carbon-carbon double bonds and can directly synthesiz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/06B01J31/22C07C253/30C07C255/34
CPCB01J31/1691B01J2531/845C07C253/30C07F15/065C07C255/34
Inventor 董育斌丁凤文王建成刘启奎
Owner SHANDONG NORMAL UNIV
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