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Magnetic PAMAM dendrimer material modified by p-mercaptobenzoic acid

A technology of p-mercaptobenzoic acid and polymer materials, applied in the field of magnetic materials, can solve the problems of weak adsorption capacity, few adsorption types, easy aggregation, etc., and achieve the effect of good adsorption performance

Active Publication Date: 2020-09-22
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Commonly used magnetic materials are mostly Fe 3 o 4 , but the unmodified Fe 3 o 4 Easy to aggregate, weak adsorption capacity and relatively few adsorption types

Method used

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  • Magnetic PAMAM dendrimer material modified by p-mercaptobenzoic acid
  • Magnetic PAMAM dendrimer material modified by p-mercaptobenzoic acid
  • Magnetic PAMAM dendrimer material modified by p-mercaptobenzoic acid

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Experimental program
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Effect test

Embodiment 1

[0062] This embodiment provides a method for preparing a magnetic PAMAM dendritic polymer material (MNPs@G3.0@4-MBA) modified by p-mercaptobenzoic acid. The schematic flow chart is as follows figure 1 As shown, it includes the following steps:

[0063] (1) Synthesis of magnetic nanoparticles (MNPs):

[0064] 5.4g FeCl 3 ·6H 2 O and 2.78g FeSO 4 ·7H 2 O was dissolved in 100mL of deoxygenated water, and under nitrogen atmosphere, 18mL of 25%-28% ammonia water was added dropwise while stirring, and the temperature was raised to 80°C to continue stirring for 30min, and then cooled to room temperature. Washed with pure water several times, and dried overnight at 50°C in a vacuum oven to obtain magnetic nanoparticles MNPs.

[0065] (2) Amino-modified magnetic nanoparticles (MNPs-NH 2 )Synthesis:

[0066] Ultrasonic dispersion of 2 g of MNPs in 200 mL of ethanol, under the protection of nitrogen, 14 mL of 3-aminopropyltriethoxysilane (APTES) was added dropwise with stirring, a...

Embodiment 2

[0084] This embodiment provides a method for magnetic solid-phase extraction to detect polycyclic aromatic hydrocarbons in environmental water samples. The schematic flow chart is as follows figure 1 As shown, it includes the following steps:

[0085] The 80mg p-mercaptobenzoic acid modified magnetic PAMAM dendritic polymer material of the present invention (such as the MNP@G3.0@4-MBA prepared in Example 1) was dispersed in 60mL of polycyclic aromatic hydrocarbons as a solid phase extraction adsorbent. In the sample solution to be tested, the sample solution to be tested contains 5 kinds of polycyclic aromatic hydrocarbons: PHE, ANT, FLT, PYR and BaP, and the concentration of the 5 kinds of polycyclic aromatic hydrocarbons in the sample solution to be tested is 10 μg / L, and the control solution The pH is 7.0, shaken at 200rpm in a constant temperature oscillator at 20°C for 50min, and the solid phase extraction adsorbent and supernatant are separated by an external magnetic fi...

Embodiment 3

[0089] 1. Comparing the magnetic nanoparticles grafted by PAMAM dendritic polymers of different generations modified with p-mercaptobenzoic acid, the prepared PAMAM dendritic polymer grafted magnetic nanoparticles are used as solid phase extraction adsorbents for the extraction of target substances Efficiency impact.

[0090] The preparation process of MNPs@G3.0, MNPs@G1.0@4-MBA, MNPs@G2.0@4-MBA, MNPs@G3.0@4-MBA was carried out according to the operation of Example 1. The extraction was carried out according to the operation of Example 2, and the extraction efficiency of the target extract was compared, and the results were as follows: Figure 5a shown.

[0091] Depend on Figure 5a It can be seen that the recovery rate of PAHs is MNPs@G3.02 More than G1.0 and G2.0, so MNPs@G3.0@4-MBA contains more 4-MBA, which can get a relatively high recovery rate. Therefore, the present invention preferably uses MNPs@G3.0@4-MBA as the solid phase extraction adsorbent.

[0092] 2. The i...

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Abstract

The invention provides a magnetic PAMAM dendrimer material modified by p-mercaptobenzoic acid. The preparation method of the material comprises the following steps: preparing amino-modified magnetic nanoparticles, carrying out n-generation PAMAM grafting on the amino-modified magnetic nanoparticles, and modifying the grafted product with p-mercaptobenzoic acid to obtain the p-mercaptobenzoic acid-modified magnetic PAMAM dendritic polymer material. The 4-MBA modified magnetic PAMAM dendritic polymer material is obtained by modifying a magnetic PAMAM dendritic polymer with p-mercaptobenzoic acid, and the material can realize simple, rapid, sensitive and effective determination of polycyclic aromatic hydrocarbons (PAHs) in an environmental water sample. The material used as a solid phase adsorbent has better linearity within the range of 0.1-300mu g / L, and the detection limit range is 0.014-0.055 mu g / L. Compared with other conventional methods, the method has the advantages of simplicity, durability, easiness in separation and high enrichment efficiency.

Description

technical field [0001] The invention belongs to the technical field of magnetic materials, and relates to a magnetic PAMAM dendritic polymer material modified by p-mercaptobenzoic acid. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are considered typical persistent organic pollutants (POPs) because of their high bioaccumulation and harmfulness to health (such as carcinogenicity, mutagenicity, teratogenicity and toxicity), and can pass through the digestive tract, Enter the human body through respiratory and skin contact. Even a small amount may cause various diseases to the human body and cause serious harm to the human body. Therefore, it is very important to develop fast, simple, highly sensitive and reliable methods for the detection of PAHs. [0003] Currently, methods for detecting PAHs include gas chromatography-tandem mass spectrometry (GC-MS), high-performance liquid chromatography (HPLC), liquid chromatography-mass spectrometry (LC-MS) and ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/062
Inventor 周庆祥仝亚艳
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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