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Magnetic core-shell mesoporous surface molecular imprinting composite nano material and preparation method thereof

A technology of surface molecular imprinting and composite nanomaterials, applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., can solve problems such as difficult magnetic separation, weakened magnetic properties, and slow adsorption equilibrium speed

Active Publication Date: 2021-05-18
合肥海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]By synthesizing a specific magnetic mesoporous carrier material, and imprinting phthalate target molecules on the surface of the carrier material by surface molecular imprinting technology, the material is The selectivity, adsorption capacity and kinetic properties of phthalates have been greatly improved, but the surface molecularly imprinted polymer materials synthesized using magnetic mesoporous carbon materials as carriers are only suitable for PAEs in drinking water and environmental water. Due to the large cavity between the mesoporous shell and the magnetic core, the adsorption equilibrium speed is slow, which takes about 20 minutes, and the magnetic performance is greatly weakened (saturation magnetic susceptibility is only 21.5 emu / g), and it is difficult to achieve magnetic separation.

Method used

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  • Magnetic core-shell mesoporous surface molecular imprinting composite nano material and preparation method thereof
  • Magnetic core-shell mesoporous surface molecular imprinting composite nano material and preparation method thereof
  • Magnetic core-shell mesoporous surface molecular imprinting composite nano material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation steps of a magnetic core-shell mesoporous surface molecularly imprinted composite nanomaterial are as follows:

[0050] (1) Synthesis of Fe 3 o 4 magnetic nanoparticles

[0051] 0.5 g Fe 3 o 4 , 150 mL of absolute ethanol, and 150 mL of deionized water were added to a 500 mL three-necked flask, and ultrasonically dispersed for 10 min; 0.6 g of resorcinol and 4.8 mL of concentrated ammonia water with a mass concentration of 28% were added, and stirred at 30°C for 1 h; Add 0.8 mL of formaldehyde with a mass concentration of 37% and 1.4 mL of TEOS dropwise, stir at 30 °C for 6 h, then stir at 80 °C for 10 h, wash the product three times with deionized water and ethanol, and dry in a 60 °C oven 10 h, get Fe 3 o 4 magnetic nanoparticles.

[0052] (2) Preparation of magnetic core-shell mesoporous nanocomposite particles

[0053] Magnetic core-shell mesoporous nanocomposite particles were synthesized by the improved Stöber method, and 1.0 g Fe 3 o 4 M...

Embodiment 2

[0068] The preparation steps of a magnetic core-shell mesoporous surface molecularly imprinted composite nanomaterial are as follows:

[0069] (1) Synthesis of Fe3O4 magnetic nanoparticles, same as in Example 1.

[0070] (2) Preparation of magnetic core-shell mesoporous nanocomposite particles, same as in Example 1.

[0071] (3) Preparation of amino-modified magnetic core-shell mesoporous nanocomposite particles

[0072] Add 1.2 g of magnetic core-shell mesoporous nanocomposite particles prepared in step (2) and 60 mL of toluene into a three-neck flask, disperse uniformly by ultrasonic for 5 min, and slowly add 5 mL of 3-(2-aminoethyl)-aminopropyl Trimethoxysilane (TSD), reflux reaction at 85°C for 4 h, so that the silane reagent can be adsorbed onto SiO 2 In the mesoporous channel, cooled to room temperature, separated by magnet, and washed twice with toluene and deionized water successively to remove unreacted or unadsorbed SiO 2 The silane reagent in the mesoporous chann...

Embodiment 3

[0077] The application of the magnetic core-shell mesoporous surface molecularly imprinted composite nanomaterial of the present invention as a magnetic solid-phase extraction agent for adsorbing phthalates has excellent specific adsorption performance and high adsorption capacity (saturation) for six PAEs The adsorption capacity is 523.9 mg / g), the adsorption kinetics is fast, and the adsorption equilibrium is reached in 5 minutes. The material can be reused. It is an ideal magnetic solid-phase extraction material for the extraction and purification of phthalates.

[0078] In order to evaluate the selective adsorption performance of the material of the present invention, two analogues, butyl benzoate (BB) and dodecylbenzene (DB), which are similar in structure to PAEs, were selected to compare the adsorption capacity. Adsorption performance comparison. Accurately weigh 10 mg of the product of the present invention or non-molecularly imprinted composite (Fe 3 o 4 @SiO 2 @mS...

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Abstract

The invention relates to a magnetic core-shell mesoporous surface molecularly imprinted composite nano material and a preparation method thereof, and belongs to the technical field of molecularly imprinted polymers. The material is black powder, the average particle size of powder particles is 200-300 nm, the specific surface area is 327.6 cm<2> / g, and the saturation magnetization is 54.9 emu / g. The preparation method comprises the following steps: synthesizing double-layer silicon dioxide coated magnetic core-shell mesoporous nano composite particles as a carrier through an improved Stober method, bonding amino groups on the carrier, taking diisononyl phthalate as a virtual template, and preparing a novel magnetic core-shell mesoporous surface molecularly imprinted composite nano material through a surface molecular imprinting technology; a matrix dispersion-magnetic solid phase extraction-gas chromatography-mass spectrometry method established on the basis that the material disclosed by the invention is a magnetic solid phase extraction agent is used for detecting phthalic acid ester substances, and the method is low in detection limit, high in precision and suitable for detecting trace phthalic acid ester in liquid drinks such as water, wine and drinks.

Description

technical field [0001] The invention belongs to the technical field of molecularly imprinted polymers, in particular to a method for preparing a magnetic core-shell mesoporous surface molecularly imprinted composite nanomaterial, and at the same time relates to the use of the composite material as a magnetic solid-phase extraction agent for phthalate compounds in food Applications in extraction testing. Background technique [0002] Phthalates (PAEs) are plasticizers widely used in food packaging, plastic processing and other industries, and have become widespread pollutants in food. Studies have found that phthalates have estrogen-like effects, can interfere with the endocrine system, cause lesions in the human reproductive system, and have potential health risks. There is no covalent bond between phthalates and plastic molecules, so they are easy to migrate from packaging materials to food and the environment during use and contact. At present, the detection process of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/26B01J20/30B01J20/285
CPCB01J20/28009B01J20/268B01J20/06B01J20/28083B01J20/28007B01J20/28021B01J20/285B01J2220/46
Inventor 刘宇欣韩芳丁磊吕亚宁周典兵宋伟郑平赵琳
Owner 合肥海关技术中心
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