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Magnetic carboxylated covalent organic framework nanocomposite material and its preparation method and application

A technology of covalent organic framework and nanocomposite materials, applied in chemical instruments and methods, alkali metal compounds, inorganic chemistry, etc., can solve the problems of large solution consumption, time-consuming, single action mode of the extraction target, etc., and achieve pore Large, improved adsorption efficiency, good stability

Active Publication Date: 2022-04-01
HENAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solid-phase extraction method has disadvantages such as time-consuming, large solution consumption, and a single mode of action for the extracted target.

Method used

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  • Magnetic carboxylated covalent organic framework nanocomposite material and its preparation method and application
  • Magnetic carboxylated covalent organic framework nanocomposite material and its preparation method and application
  • Magnetic carboxylated covalent organic framework nanocomposite material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1. Preparation of magnetic carboxylated covalent organic framework nanocomposites

[0043] A method for preparing a magnetic carboxylated covalent organic framework nanocomposite material, comprising the following steps:

[0044] (1) Magnetic Fe 3 o 4 Synthesis of nanoparticles:

[0045] Weigh 2.7g FeCl 3 ·6H 2 O solid in a 100mL beaker, add 80mL of ethylene glycol, ultrasonic to FeCl 3 ·6H 2 O solid dissolved solution is a transparent liquid, then add 7.2g of anhydrous sodium acetate and 2.0g of polyethylene glycol, ultrasonic 20min, the solution is yellowish brown, and contains a large amount of yellow flocs; the resulting mixture is transferred to the autoclave , reacted at 200 ° C for 12 h, cooled to room temperature, and washed the Fe produced by the reaction with ethanol and double distilled water in sequence. 3 o 4 , repeated three times, stored in absolute ethanol for later use.

[0046] (2) Magnetic Fe 3 o 4 @SiO 2 Synthesis of nanoparticles...

Embodiment 2

[0058] Example 2. Adsorption performance test of magnetic carboxylated covalent organic framework nanocomposites for polycyclic aromatic hydrocarbons

[0059] Weigh 4 mg magnetic carboxylated covalent organic framework nanocomposites, add 0.2 μg / mL polycyclic aromatic hydrocarbons mixed standard (naphthalene, fluorene, anthracene, phenanthrene, pyrene, )5mL, ultrasonically adsorbed for 2min, 3min, 4min, 5min, 7min, 9min, and 11min respectively, and the supernatant was filtered through a 0.2μm water filter membrane, and then injected for analysis to investigate the effect of adsorption time on the adsorption efficiency of polycyclic aromatic hydrocarbons. from Figure 5 It can be seen that with the increase of adsorption time, the adsorption efficiency gradually increases, and when the adsorption time is 5 min, the adsorption efficiency can reach more than 95%.

Embodiment 3

[0060] Example 3, Test of Adsorption Performance of Magnetic Covalent Organic Framework Composite Materials on Tetracycline

[0061] Weigh 4mg of magnetic carboxylated covalent organic framework nanocomposite, add 0.2μg / mL tetracycline mixed standard (oxytetracycline, tetracycline, methacycline, doxycycline) 5mL, ultrasonic adsorption for 2min, 4min, 6min respectively , 8min, 10min, 12min, 15min, the supernatant was filtered through a 0.2μm water filter membrane, and the sample was analyzed to investigate the influence of the adsorption time on the tetracycline adsorption efficiency. from Image 6 It can be seen that with the increase of adsorption time, the adsorption efficiency gradually increases, and when the adsorption time is 8 min, the adsorption efficiency can reach more than 93.5%.

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Abstract

The invention discloses a magnetic carboxylated covalent organic framework nanocomposite material and its preparation method and application. The composite material is Fe with carboxylated covalent organic framework externally modified 3 o 4 @SiO 2 ‑NH 2 Nanoparticles. The outer layer of the composite material of the present invention has a variety of functional groups, such as benzene rings with conjugated structures, abundant ‑NH‑, carbonyl, carboxyl and other groups, which can not only provide hydrophobic interaction, hydrogen bond interaction, π‑π It can also provide a weak cation exchange effect, so that the material has multiple modes of action, and can treat substances with different properties such as non-polar polycyclic aromatic hydrocarbons, polar substances tetracyclines, and strong alkalis with quaternary ammonium salt structures. Substances such as paraquat, diquat, malachite green and crystal violet were extracted simultaneously. The composite material synthesized by the invention has the advantages of large specific surface area, large pores, strong magnetism, good stability, reusability, etc., and can meet the requirements of rapid separation and analysis.

Description

technical field [0001] The invention relates to a separation material, in particular to a magnetic carboxylated covalent organic framework nanocomposite material and its preparation method and application. Background technique [0002] With the development of society, problems such as environmental pollution and food safety are becoming more and more serious. The severe situation leads to more types of samples and more complex sample matrices that need to be monitored and analyzed. Rapid and accurate analysis of the content of trace components in complex samples at a lower cost is the most requested by people for analytical laboratories. The analysis process of a sample mainly includes: sample collection, sample pretreatment, data collection and result analysis. Among them, sample pretreatment is the most time-consuming and cumbersome step in the entire analysis process, and it is also the most important link in the analysis. Moreover, errors generated in sample pretreatme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/30C02F101/32C02F101/38
CPCB01J20/22B01J20/28009B01J20/28007C02F1/285C02F2101/306C02F2101/308C02F2101/327C02F2101/38
Inventor 胡锴史艳梅陈志红罗晓
Owner HENAN UNIV OF CHINESE MEDICINE
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