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Preparation and application of a molecularly imprinted magnetic nanomaterial on the surface of bis(2-ethylhexyl) phthalate

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

Active Publication Date: 2018-07-03
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 3.33 g of polyethylene glycol (PEG) in 30 mL of ultrapure water. Take 2.86 g FeSO 4 ·7H 2 O and 8.10 gFe(NO 3 ) 3 9H 2 O was dissolved in 75 mL 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. Use a magnet to separate the flocculent magnetic fluid, wash it twice with 200 mL of deionized water, wash it twice with 150 mL of 95% ethanol, and disperse it with 95% ethanol to 100 mL to obtain solution A.

[0025] (2) Dissolve 15 mL of TEOS in 30 mL of acetone, add 0.45 mL of concentrated hydrochloric acid and 1.2 mL of ultrapure water, and heat and stir in a 58°C water bath. After 3 h, solution B was obtained. Mix solutions B and A evenly under ultrasound, quickly add 6.0 mL of concentrated ammonia water, stir well, and form a black gel. The black gel was aged in a ventilated place for 30 min, a...

Embodiment 2

[0030] Various index experiments were carried out on the materials obtained in Example 1.

[0031] Add 50 mg of the material obtained in Example 1 to 100 mL solutions containing 1 mg / L DEHP 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] Add 50 mg of the material obtained in Example 1 to 100 mL of pH=7 solution containing 1 mg / L DEHP, and investigate the effect of adsorption time on the adsorption effect of DEHP. 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 change of the adsorption amount of the material with the initial conc...

Embodiment 3

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

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

[0040] Material can be reused 8 times.

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Abstract

The invention relates to the preparation and application of a molecularly imprinted magnetic nanomaterial on the surface of bis(2-ethylhexyl) phthalate (DEHP), which belongs to the technical field of nanomaterials; the preparation method: ultrasonic stirring under the protection of N2, to Fe Add polyethylene glycol solution to (NO3)3, FeSO4 mixture, adjust the pH, separate the flocculent magnetic fluid with a magnet and disperse it in ethanol, mix evenly with the acetone solution of tetraethoxysilane, and add concentrated ammonia water , forming a black gel; after the gel is aged and dried, Fe3O4‑SiO2 material is obtained; DEHP and phenyltrimethoxysilane are dissolved in methanol, and after shaking, the activated Fe3O4‑SiO2 material, tetraethoxysilane and acetic acid, stirred at room temperature; washed with chloroform, magnetically separated, and vacuum-dried to obtain DEHP imprinted magnetic nanomaterials, with an average particle size of about 33 nm and a saturation magnetization of 14.9 emu g-1; the material was added to DEHP can be efficiently enriched in DEHP-containing environmental water samples or beverage samples, with fast processing speed and good selectivity; the material can be reused many times.

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 Patents(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