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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

Active Publication Date: 2021-04-27
NANKAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the QuEChERS technology developed specifically for the rapid screening and analysis of pesticide residues in a large number of food and agricultural product samples is cumbersome, time-consuming, and incompletely purified. In view of the above points, there is an urgent need for an efficient, fast, and selective method. It is an adsorbent for purifying the pigment interfering substances such as chlorophyll, lutein and carotene in the matrix of food samples, and does not adsorb pesticide residues, so as to obtain a clean solution on the machine, reduce the interference of the matrix on the determination of the target, and can further improve the pesticide residue content. Accurate qualitative and quantitative analysis

Method used

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  • Hierarchical heterogeneous covalent organic framework material, preparation method and application thereof
  • Hierarchical heterogeneous covalent organic framework material, preparation method and application thereof
  • Hierarchical heterogeneous covalent organic framework material, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention provides a hierarchical different-pore covalent organic framework material, a preparation method and application thereof. According to the invention, a composite material is prepared through the physical coating effect of a different-pore covalent organic framework and a metal organic framework, and takes the metal organic framework as a sacrificial template, and the metal organic framework is dissolved with a dissolving agent to synthesize the hierarchical heterogeneous covalent organic skeleton material; the hierarchical heterogeneous covalent organic framework material has excellent rapid purification ability on pigment molecules in food and agricultural products; and the pesticide residue content of food and agricultural product samples is detected and analyzed by combining a liquid chromatography or mass spectrometry analysis technology, so that the chemical hazard factors can be completely recycled.

Description

technical field [0001] The invention belongs to the field of nanomaterial synthesis, and in particular relates to a hierarchical heteroporous covalent organic framework material and its preparation method and application. Background technique [0002] Food safety is a major issue related to human health. At present, various pesticide and veterinary drug residues, food additives, and endocrine disruptors that exceed the standard in food and agricultural products may cause great harm to human health. Current analytical methods mainly focus on directed analysis, that is, the detection of known target analytes. Although directed analysis plays an important role in food safety analysis, in some cases, such as comprehensive assessment of food safety, emergency treatment of food poisoning and identification of emerging contaminants, the detection ability of this method is limited. is limited and cannot meet the requirements. Therefore, high-throughput non-targeted screening aimed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/282B01J20/28B01J20/30G01N30/02G01N30/72
CPCB01J20/282B01J20/2808B01J20/28085B01J20/28083B01J20/3057G01N30/02G01N30/72
Inventor 孔德明李薇唐安娜王晓涵陈燕王汭
Owner NANKAI UNIV
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