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Preparation method and application method of phthalates molecular imprinted magnetic materials through dual-virtual template

A phthalate ester and virtual template technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problem of insufficient selectivity of solid phase extraction, complex matrix components, and unsatisfactory Requirements for the separation and enrichment of PAEs components and other issues, to achieve good specific recognition and selectivity, simple and convenient preparation process, and conducive to rapid separation

Active Publication Date: 2018-12-28
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because PAEs are not easily soluble in water, the content is usually at trace or even trace levels, and the matrix composition is complex, so pretreatment processes such as separation and enrichment are required before they can be used for analysis and detection
Due to the shortcomings of cumbersome operation, long cycle, low recovery rate, low enrichment factor and reproducibility, traditional sample pretreatment technology cannot meet the separation and enrichment requirements of PAEs components.
Due to its high enrichment factor, low cost and easy operation, solid phase extraction has been proven to be an effective method for water sample extraction, preconcentration and purification, but traditional solid phase extraction (such as bonded silica gel adsorbent, etc.) is selective Insufficient, it takes quite a long time when processing large volumes of water samples

Method used

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  • Preparation method and application method of phthalates molecular imprinted magnetic materials through dual-virtual template

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030](1) Mix 5g of graphite powder and 5g of sodium nitrate with 230mL of concentrated sulfuric acid in an ice bath, slowly add 40g of potassium permanganate, react for 2 hours, and control the temperature of the reaction solution not to exceed 10°C; remove the ice bath, and transfer the mixture to In a constant temperature water bath at 35°C, stir and react for 2 hours; raise the temperature of the water bath to 95°C and gradually add 230mL ultrapure water, keep the reaction for 40min to increase the degree of oxidation of the product; after the reaction, place it to cool to room temperature, then Add ultrapure water to 1000mL, and dropwise add hydrogen peroxide with a mass fraction of 30% until no bubbles are formed; let it settle, discard the supernatant, wash with deionized water and absolute ethanol three times respectively, and store at 70°C Vacuum drying yields graphene oxide (GO).

[0031] (2) 0.3g GO, 3.52g FeCl 3 ·6H 2 O and 1.81 g FeSO 4 ·7H 2 O was dissolved i...

Embodiment 2

[0037] Carry out various index experiments to the material obtained in Example 1.

[0038] 20 mg of the material obtained in Example 1 was added to 20 mL of solutions containing 20 mg / L PAEs at different pH values ​​to investigate the effect of pH value on the adsorption effect of PAEs. The results showed that the adsorption amount was the largest when the pH was around 7, so the subsequent adsorption experiments were all carried out under neutral conditions.

[0039] 20 mg of the material obtained in Example 1 was added to 20 mL of a pH=7 solution containing 20 mg / L PAEs, and an adsorption reaction occurred in a constant temperature oscillator at 25°C to investigate the effect of adsorption time on the adsorption effect. The results showed that after 120 minutes, the adsorption reached equilibrium, the adsorption process obeyed the second-order kinetics, and the mass transfer process of the adsorbed mass was mainly controlled by the chemical adsorption mechanism.

[0040] 20...

Embodiment 3

[0043] The material obtained in Example 1 was used for the solid phase extraction separation and enrichment of trace PAEs in the solution.

[0044] Add 20mg of the material to 100mL of PAEs solution containing 10μg / L, adjust the pH to 7, shake in a constant temperature oscillator at 25°C and 200rpm for 30min, and perform solid phase extraction. After the extraction, the material containing PAEs was sucked to the bottom of the reaction vessel with a magnet, and the supernatant was discarded. Then add 3mL absolute ethanol solution and shake and elute at 250rpm for 5min, magnetically separate, measure the concentration of PAEs in the upper eluent with GC-MS, do 3 groups of parallel experiments simultaneously, adopt internal standard method (with benzyl benzoate as internal standard) to calculate the recovery of PAEs.

[0045] The calculation formula of the recovery rate is as follows:

[0046]

[0047] where C 0 and C are the concentrations of PAEs in the solution before so...

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Abstract

The invention relates to a preparation method and application method of a phthalates molecular imprinted magnetic material through dual-virtual template. The preparation method comprises the followingsteps of preparing graphene oxide by a modified Hummer method; loading Fe3O4 granules to the surfaces; adding cetyl trimithyl ammonium bromide and tetraethylorthosilicate to obtain a magnetic graphene oxide-Meso-PS compound; using the compound as a carrier, using dipropyl phthalate and diisononyl phthalate as a virtual template, using Phenyltrimethoxysilane and 3-aminopropyl triethoxy silane as functional monomers, using tetraethylorthosilicate as a cross-linking agent, performing vibrating for stirring at room temperature, and performing sol-gel surface molecular imprinting; and eluting template molecules with a mixed solution of methyl alcohol and acetic acid, performing magnetic separation, and then performing vacuum drying to obtain the phthalates molecular imprinted magnetic materialthrough dual-virtual template. The material has favorable adsorptive selectivity on 6 priority-controlled phthalates, can be quickly separated from aqueous phases, is short in balance time and high in adsorbing capacity, can be reused for 6 times, can realize selective removal and enrichment of various PAEs in water, and has high practical application value.

Description

technical field [0001] The invention belongs to the field of new environmental functional materials and new water treatment technologies, and specifically relates to a preparation method of a double virtual template phthalate molecularly imprinted magnetic material, and the trace amount of phthalate in environmental water samples of the material Applications in the separation and enrichment of class compounds. Background technique [0002] Phthalate esters (PAEs) are esterified derivatives of phthalic acid. As a plasticizer, PAEs usually exist in a variety of environmental media, food, beverages, and pharmaceuticals in the form of free mobile phases, and are persistent. In addition, PAEs are endocrine disruptors and carcinogens, and human exposure to them may have potential harm to reproductive, liver and kidney systems. Therefore, using effective methods to analyze and remove PAEs in wastewater has become a research hotspot in recent years. [0003] In view of the hazard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/34
CPCB01J20/103B01J20/20B01J20/22B01J20/28009C02F1/288C02F2101/34
Inventor 马晓国郭丽慧谢晓纹
Owner GUANGDONG UNIV OF TECH
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