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Preparation and application of di(2-ethyl hexyl) phthalate surface molecular imprinting magnetic nanometer material

A technology of phthalic acid two and surface molecular imprinting, which is applied in the preparation and application of nanomaterials, can solve the problems of easy agglomeration and small particle size of nanoparticles, and achieve large adsorption capacity, simple preparation process and good selectivity Effect

Active Publication Date: 2016-04-20
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ferric oxide is commonly used as a magnetic material, but its nanoparticles are small in size and easy to agglomerate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Dissolve 3.33g of polyethylene glycol (PEG) in 30mL of ultrapure water. Take 2.86g FeSO 4 ·7H 2 O and 8.10gFe(NO 3 ) 3 9H 2 O was dissolved in 75mL ultrapure water, and mixed to obtain a brown solution. After mixing the PEG solution with it, under the protection of nitrogen, slowly add ammonia water to adjust the pH to 11-12, and stir while ultrasonicating. Separate the flocculent magnetic fluid with a magnet, wash it twice with 200mL deionized water, wash it twice with 150mL95% ethanol, and disperse it with 95% ethanol to 100mL to obtain solution A.

[0025] (2) Dissolve 15mLTEOS in 30mL acetone, add 0.45mL concentrated hydrochloric acid and 1.2mL ultrapure water, heat and stir in a 58°C water bath. After 3 h, solution B was obtained. Mix solutions B and A evenly under ultrasonication, quickly add 6.0mL concentrated ammonia water, stir evenly, and form a black gel. After aging the black gel in a ventilated place for 30 minutes, dry it in a vacuum oven at 60...

Embodiment 2

[0030] Carry out various index experiments to the material obtained in Example 1.

[0031] 50 mg of the material obtained in Example 1 was added to 100 mL of solutions containing 1 mg / LDEHP at different pH values ​​to investigate the effect of pH value on the adsorption effect of DEHP. The results showed that the recovery rate was close to 100% when the pH was around 7, so other adsorption experiments were carried out under neutral conditions.

[0032] 50 mg of the material obtained in Example 1 was added to 100 mL of a pH=7 solution containing 1 mg / LDEHP, and the effect of adsorption time on the adsorption effect of DEHP was investigated. The results showed that after 20 min, the adsorption equilibrium was reached.

[0033] 50 mg of the material obtained in Example 1 was added to solutions with different initial DEHP concentrations, and was adsorbed in a constant temperature oscillator at 25°C for 3 hours to study the variation of the adsorption amount of the material with t...

Embodiment 3

[0038] The material obtained in Example 1 was used for the solid phase extraction separation and enrichment of trace DEHP in the solution.

[0039] Add 50mg of the material to 100mL of a solution containing a certain concentration of DEHP (environmental water sample, beverage sample, etc.), adjust the pH to 7, and shake at 200rpm for 20min. The material adsorbed by DEHP was separated with a magnet, then 5 mL of chloroform was added, desorbed by shaking at 300 rpm for 5 min, the content of DEHP in the eluent was measured by gas chromatography-mass spectrometer, and the recovery rate was calculated.

[0040] The material can be reused 8 times.

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Abstract

The invention relates to preparation and application of a di(2-ethyl hexyl) phthalate surface molecular imprinting magnetic nanometer material, and belongs to the technical field of nanometer materials. The preparation method includes the steps of conducting ultrasonic stirring under protection of N2, adding a polyethylene glycol solution to a mixed solution of Fe(NO3)3 and FeSO4, regulating pH, separating out flocculent magnetic fluid through a magnet, dispersing the flocculent magnetic fluid in ethyl alcohol, evenly mixing the mixture with an acetone solution of tetraethyl orthosilicate, and adding strong ammonia water to form black gel; obtaining an Fe3O4-SiO2 material after ageing and drying are conducted on the gel; dissolving DEHP and phenyl trimethoxy silane in methyl alcohol, adding the activated Fe3O4-SiO2 material, tetraethyl orthosilicate and acetic acid after oscillation, and conducting stirring at the room temperature; obtaining the DEHP imprinting magnetic nanometer material after trichloromethane washing, magnetic separation and vacuum drying, wherein the average grain diameter is about 33 nm, and the saturation magnetization strength is 14.9 emu.g<-1>. When the material is added to an environment water sample or a beverage sample containing DEHP, DEHP can be efficiently enriched, the processing speed is high, and selectivity is good; the material can be repeatedly used.

Description

technical field [0001] The invention relates to the preparation and application of a nano material, in particular to a method for preparing a molecularly imprinted magnetic nano material on the surface of bis(2-ethylhexyl) phthalate, and the preparation of the material in a solution sample (such as an environmental water sample) , beverage samples, etc.), and belongs to the technical field of composite materials. Background technique [0002] Bis(2-ethylhexyl) phthalate (DEHP) is a plasticizer used in large quantities. Studies have shown that DEHP is now widely present in water, soil, air, food, beverages, and vegetables. Since DEHP is an endocrine disruptor and carcinogen, the analysis method and removal technology of phthalic acid plasticizers including DEHP have become a research hotspot in the fields of environment, food and hygiene in recent years. [0003] The content of DEHP in environmental water samples, beverages and other samples is usually at trace or even trac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/20G01N30/02G01N27/62
CPCB01D15/203B01J20/06B01J20/103G01N27/62G01N30/02B01J20/268B01J20/28009B01J2220/46G01N2030/025
Inventor 马晓国李春英
Owner GUANGDONG UNIV OF TECH
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