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Cyclodextrin supramolecular polymer/Fe3O4 magnetic nanoparticle complex

A technology of supramolecular polymers and magnetic nanoparticles, applied in alkali metal compounds, water/sludge/sewage treatment, alkali metal oxides/hydroxides, etc., can solve the lack of selectivity and kinetics, separation and recovery difficulties and other problems, to achieve the effect of excellent adsorption capacity, simple operation and easy recovery

Inactive Publication Date: 2017-06-16
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The adsorption efficiency of conventional adsorbents, such as activated carbon, diatomaceous earth, resin, etc., is usually limited by conditions such as specific surface area, difficulty in separation and recovery, lack of selectivity, and kinetics

Method used

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  • Cyclodextrin supramolecular polymer/Fe3O4 magnetic nanoparticle complex
  • Cyclodextrin supramolecular polymer/Fe3O4 magnetic nanoparticle complex
  • Cyclodextrin supramolecular polymer/Fe3O4 magnetic nanoparticle complex

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1: Preparation of β-CDSP-MNPs

[0027] (1) Preparation of β-CDSP: Add 2g of β-CD into 8mL dimethyl sulfoxide (DMSO) to dissolve and stir, then add 2mL of triethylamine, after 5 minutes, add 1.345g of cross-linking agent pyromellitic acid di anhydride (PMA), react at room temperature, and the reaction solution gradually gels. After 16 hours, the reaction was complete, and it became a block, which was ground with a mortar, washed with double distilled water and acetone, and filtered with suction, washed with secondary water three times, and freeze-dried to obtain a white powder β-CDSP.

[0028] (2) Preparation of β-CDSP modified MNPs: 1 g FeCl 3 ·6H 2 O, 0.45g FeCl 2 4H 2 O and 0.9g β-CDSP are placed in the reactor, add 200mL of secondary water, heat and stir until dissolved under nitrogen protection, keep the temperature at 80°C for 5 minutes, add concentrated ammonia water dropwise to adjust the pH of the reaction solution to 10, and stir mechanically Af...

Embodiment 2

[0037] Example 2: Adsorption of β-CDSP-MNPs to malachite green dye

[0038] (1) Effect of pH on the adsorption performance of β-CDSP-MNPs

[0039] Determination of adsorption of malachite green (2×10 -5 M) Absorbance before and after to explore the effect of pH on the adsorption performance of β-CDSP-MNPs.

[0040] (2) Effect of ionic strength on the adsorption performance of β-CDSP-MNPs

[0041] The adsorption of malachite green (2×10 -5 M) Absorbance before and after to explore the effect of ionic strength on the adsorption performance of β-CDSP-MNPs.

[0042] (3) Malachite green standard curve and its linear range

[0043] Measure malachite green stock solution (2×10 -3 M) 2μL, 10μL, 20μL, 30μL, 40μL, 50μL, 60μL, 70μL, 80μL, 90μL, 100μL, dilute to 4mL with secondary water, measure the absorbance of the sample solution at 617nm. Draw the standard curve with the concentration (mol / L) of malachite green substance as the abscissa and the absorbance as the ordinate.

[00...

Embodiment 3

[0054] Embodiment 3: investigation of desorption and reuse situation

[0055] The complex uses absolute ethanol as the eluent, after ultrasonic oscillation for 10 minutes, hysteresis separation, and then washes three times with secondary water and absolute ethanol respectively, and vacuum-dries at 60°C to obtain the desorbed magnetic nanocomposite, which is then recycled. use. This cycle was repeated three times, and the adsorption amount of malachite green by β-CDSP-MNPs in each cycle was calculated.

[0056] Depend on Figure 13 It can be seen that after recycling 3 times, β-CDSP-MNPs still has a high adsorption capacity, indicating that β-CDSP-MNPs is a reusable dye adsorption material. It shows that the complex has a good application prospect in the field of dye pollutant adsorption.

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Abstract

The invention provides a cyclodextrin supramolecular polymer / Fe3O4 magnetic nanoparticle complex. The complex is prepared by the following steps: firstly, crosslinking beta-cyclodextrin with pyromellitic dianhydride to synthesize a cyclodextrin supramolecular polymer (beta-CDSP); coprecipitating the beta-CDSP and FeCl3.6H2O and FeCl2.4H2O under an alkaline condition by a one-pot method, so as to obtain the complex. An X-ray diffraction (XRD) method, a transmission electron microscope (TEM) method, a Fourier transform infrared spectroscopy (FTIR) method and a thermogravimetric analysis (TGA) method are applied for characterizing to verify that the beta-CDSP is grafted to Fe3O4 magnetic nanoparticles. The complex has the advantages of low synthesis cost, environment friendliness, no toxicity, abundant hydroxide radicals, free carboxyl and better magnetic properties, and can be used as an adsorption material for adsorption cation type triphenylmethane dye pollutants; malachite green serves as a model molecule for study on adsorption properties, and results show that the complex has a good adsorption effect on the malachite green and has a potential application prospect on the aspect of the adsorption material of environmental pollutants.

Description

technical field [0001] The invention relates to the technical field of magnetic nano-adsorbent and water treatment, in particular to a cyclodextrin supramolecular polymer / Fe 3 o 4 Magnetic nanoparticle complex and its preparation method and application. Background technique [0002] Cationic triphenylmethane dyes are the third most used dyes after azo dyes and anthraquinone dyes, and a large amount of waste water is generated during production and use. This type of wastewater is dark in color, difficult to biodegrade, and seriously pollutes the environment. Among them, the most typical malachite green is used as an industrial dye in pottery, textile, leather and cytochemical dyeing; because of its antibacterial and insecticidal effects, it is also often used as a fungicide. However, malachite green has high toxicity, high residue, carcinogenic, teratogenic and mutagenic effects, and because it is easily soluble in water and widely used, it is very easy to enter water bodi...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C02F101/30
CPCB01J20/265B01J20/28009C02F1/285C02F2101/308
Inventor 梁文婷李丹范丽芳董文娟李勇杨振华董川
Owner SHANXI UNIV
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