Hierarchical heterogeneous covalent organic framework material, preparation method and application thereof
A covalent organic framework and organic framework technology, applied in the field of hierarchical heteroporous covalent organic framework materials and their preparation, can solve the problems of cumbersome operation and incomplete purification, save operation time, improve adsorption efficiency, and realize The effect of full recycling
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Embodiment 1
[0062] 1. Synthesis method of hierarchical heteroporous covalent organic framework:
[0063] (1) Synthesis of metal-organic frameworks;
[0064] Dissolve 0.0272-0.0816g of anhydrous copper acetate, 0.042-0.1260g of D / L-malic acid and 0.0234-0.0702g of 4,4'-bipyridine in 3-9mL of water / methanol mixed solution (1:1, v / v), the mixture is sealed in a glass bottle and left at room temperature for 3-24 hours.
[0065] The blue crystals were collected and washed with methanol, and then vacuum-dried at 70°C for 3 hours to obtain copper metal-organic frameworks (CuMOFs).
[0066] (2) Synthesis of composite materials:
[0067]Disperse 50-1000mg of Cu MOFs prepared in step (1) in a round-bottomed flask filled with 3-10mL 1,4-dioxane and sonicate for 0.5-2h, then add 64.2-256.8mg of tetrakis-(4- Aminophenyl) ethylene, 60-240mg of 4,4'-biphenyldicarbaldehyde, ultrasonic and mechanical stirring to disperse evenly, then add 0.3-1.0mL 4-7M acetic acid, continue stirring for 0.5-1h, transf...
experiment example 1
[0079] Experimental example 1: SEM analysis
[0080] The heteroporous covalent organic frameworks, metal organic frameworks, composite materials and hierarchical heteroporous covalent organic frameworks prepared in Example 1 of the present invention were analyzed by scanning electron microscopy of JEOL model JSM-7500F and AEMC , see the result Figure 4 , it can be seen that the metal-organic framework ( Figure 4 A-C) Rhombohedral / rectangular crystals with heteroporous covalent organic frameworks ( Figure 4 D-F) is a planar lamellar structure, the composite material ( Figure 4 H-G) The core-shell structure of COFs coated on the surface of MOFs crystals, hierarchical heteroporous covalent organic framework ( Figure 4 L-N) are hollow rhomboid and spherical particle structures.
experiment example 2
[0081] Experimental Example 2: Transmission Electron Microscopy Analysis
[0082] The Tecnai G2 F20 transmission electron microscope produced by FEI was used to analyze the hierarchical heteroporous covalent organic framework prepared in Example 1 of the present invention. The results are shown in Figure 5 , it can be seen that the composite material MOFs@COFs has a rhombohedral and spherical particle structure, and a hierarchical heteroporous covalent organic framework ( Figure 5 C, 5D) are hollow diamond and spherical particle structures.
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