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Preparation of superparamagnetic mesoporous molecularly imprinted polymer of core-shell structure and application as solid phase extractant

A technology of magnetic molecular imprinting and core-shell structure, applied in alkali metal compounds, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of reduced binding force, mass transfer hindrance, time and labor waste, etc.

Inactive Publication Date: 2017-06-23
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Considering that the binding sites are distributed in different phases, the mass transfer of target molecules from the solution to the cavity is hindered by the adsorption of templates on the surface of MIPs, which leads to the decrease of binding force and waste of time and labor.

Method used

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  • Preparation of superparamagnetic mesoporous molecularly imprinted polymer of core-shell structure and application as solid phase extractant
  • Preparation of superparamagnetic mesoporous molecularly imprinted polymer of core-shell structure and application as solid phase extractant
  • Preparation of superparamagnetic mesoporous molecularly imprinted polymer of core-shell structure and application as solid phase extractant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Fe 3 o 4 Preparation of Magnetic Nanoparticles

[0057] Add 0.86g FeCl to 30mL ethylene glycol 3 ·6H 2 O and 2.16g of sodium acetate, magnetically stirred to a uniform yellow solution, transferred to a reaction kettle, placed in an oven at 200°C for a constant temperature reaction for 12 hours, taken out and cooled to room temperature, and washed three times with ethanol and secondary water respectively to obtain Fe 3 o 4 The magnetic nanoparticles were dried in an oven at 60°C, and then ground for later use.

[0058] (2) Preparation of magnetically imprinted polymer MMIPs-TBBPS

[0059] Dissolve 0.5mmol (0.283g) of tetrabromobisphenol S and 2mLAPTES (3-aminopropyltriethoxysilane) into 10mL of anhydrous methanol solution and keep at room temperature for 2h to obtain solution I;

[0060] Accurately weigh 0.2gFe 3 o 4 Disperse the nanoparticles in 60mL of methanol and 10mL of distilled water, sonicate until completely dissolved; then add 4mLTEOS, 1mL of ammon...

Embodiment 2

[0065] (1) Fe 3 o 4 Preparation of magnetic nanoparticles: same as Example 1;

[0066] (2) Preparation of magnetically imprinted polymer MMIPs-TBBPS

[0067] Dissolve 0.5mmol (0.283g) tetrabromobisphenol S and 1.9mLAPTES (3-aminopropyltriethoxysilane) in 10mL of anhydrous methanol solution, and keep at room temperature for 2h to obtain solution I;

[0068] Accurately weigh 0.17gFe 3 o 4 Disperse the nanoparticles in 60mL of methanol and 10mL of distilled water, sonicate until completely dissolved; then add 3mLTEOS, 1mL of ammonia (28%), and stir for 5min to obtain solution II;

[0069] Add solution II to the above solution I, and stir mechanically at room temperature for 1 h; after the reaction product is taken out, wash with ethanol and deionized water for 5 times, and dry at 60°C to obtain a magnetic molecularly imprinted polymer;

[0070] The magnetic molecularly imprinted polymer was placed in a Soxhlet extractor, and was eluted with a mixed solution of methanol / aceti...

Embodiment 3

[0073] (1) Fe 3 o 4 Preparation of magnetic nanoparticles: same as Example 1;

[0074] (2) Preparation of magnetically imprinted polymer MMIPs-TBBPS

[0075] Dissolve 0.5mmol (0.283g) tetrabromobisphenol S and 2.1mLAPTES (3-aminopropyltriethoxysilane) into 10mL methanol solution and keep at room temperature for 2h to obtain solution I;

[0076] Accurately weigh 0.23gFe 3 o 4 Disperse the nanoparticles in 60mL of methanol and 10mL of distilled water, sonicate until completely dissolved; then add 5mLTEOS, 1mL of ammonia water (28%), and stir for 5min to obtain solution II;

[0077] Add solution II to the above solution I, and stir mechanically at room temperature for 1 h; after the reaction product is taken out, wash with ethanol and deionized water for 5 times, and dry at 60°C to obtain a magnetic molecularly imprinted polymer;

[0078] The magnetic molecularly imprinted polymer was placed in a Soxhlet extractor, and eluted with a mixed solution of methanol / acetic acid (9:...

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Abstract

The invention provides a preparation method of a superparamagnetic mesoporous molecularly imprinted polymer MMIPs-TBBPS. The preparation method comprises the following steps: preparing a polymer-coated Fe3O4 nanoparticle magnetic molecularly imprinted polymer by means of a one-pot process by taking tetraethoxysilane as a crosslinking agent, 3-aminopropyltriethoxysilane as a functional monomer and tetrabromobisphenol S as a template molecule; and finally, eluting a template by means of Soxhlet extraction to obtain the superparamagnetic mesoporous molecularly imprinted polymer MMIPs-TBBPS. The molecularly imprinted polymer has a uniform core-shell structure, a large specific surface area, a highly ordered mesoporous structure and relatively high saturation magnetization strength, has a fast combining capacity, excellent magnetic response and specific preferential adsorption capacity, and has a relatively high removal efficiency and equilibrium absorption capacity on a common brominated flame retardant, and in particular, the adsorption capacity on TBBPS reaches up to 1626.8[mg] / g. Therefore, the molecularly imprinted polymer can be used for effectively removing the brominated flame retardant in waste water.

Description

technical field [0001] The invention relates to the preparation of a novel superparamagnetic core-shell structure mesoporous molecularly imprinted polymer; the invention also relates to the application of the composite material as a solid phase extraction agent in the treatment of complex wastewater samples, belonging to the field of composite materials and wastewater treatment . Background technique [0002] Brominated flame retardants (BFRs) are a class of additives and reactive substances and technical mixtures widely used in printed circuit boards, the production of plastics, etc. Due to the widespread use of BFRs, potential environmental and health risks arise. Tetrabromobisphenol S (TBBPS), as a new type of BFRs, has been widely used in the preparation of various heat-resistant products. TBBPS and its commercial analogs such as tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bis(allyl ether) (TBBPA-ae), tetrabromobisphenol A bis(2,3-dibromopropyl ) ether (TBBPA...

Claims

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Application Information

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IPC IPC(8): C08G77/26C08G77/06C08J9/26B01J20/26B01J20/28B01J20/30C02F1/28C08L83/08C08K3/22C08K7/26
CPCB01J20/262B01J20/28009B01J20/28021B01J20/28083C02F1/285C08G77/06C08G77/26C08J9/26C08J2201/0424C08J2383/08C08K7/26C08K2003/2275
Inventor 王雪梅黄鹏飞王欢马晓敏王娟杜彤彤
Owner NORTHWEST NORMAL UNIVERSITY
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