Magnetic metal-organic nanometer core-shell material with adjustable diameter and preparation method thereof

A nano core-shell, organic nanotube technology, applied in the directions of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., to achieve the effect of improving adsorption effect, improving contact area, and low detectability

Active Publication Date: 2019-08-30
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The magnetic-based metal-organic nano-core-shell material can effectively avoid problems such as the decline in adsorption efficiency caused by high pressure and blockage during the solid-phase extraction process, and through the control of the external magnetic field, the magnetic adsorbent and trihalomethane wastewater Rapid separation to achieve multiple recycling of materials and meet the requirements of green and efficient removal

Method used

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  • Magnetic metal-organic nanometer core-shell material with adjustable diameter and preparation method thereof
  • Magnetic metal-organic nanometer core-shell material with adjustable diameter and preparation method thereof
  • Magnetic metal-organic nanometer core-shell material with adjustable diameter and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0028] The silanized Fe of the present invention 3 o 4 The preparation can refer to [Magnetic metal-organic nanotubes: An adsorbent for magnetic solid-phase extraction of polychlorinated biphenyls from environmental and biological samples, J.Chromatogr.A 2016,1449,39-47].

[0029] Ag-based metal-organic nanotube material of the present invention ({[Ag 2 (Hbtc)(bpy) 2 ]·(H 2 O) 2} n) can be prepared with reference to the literature Syntheses, structures and properties of two unusual silver–organic coordination networks: 1D→1D tubular intertwinement and existence of an infinite winding water chain, Dalton Transactions 2011, 40, 788].

Embodiment 1

[0030] Embodiment 1: the preparation of the magnetic-based metal-organic nano-core-shell material with adjustable diameter, such as figure 1 Shown:

[0031] 1. Solvothermal Synthesis of Fe-Based Magnetic Nanoions 3 o 4 :

[0032] 2.6gFeCl 3 ·3H 2 O was added to 50mL of ethylene glycol, and stirred for 1h until the mixture was homogeneous. Add 5.75g of sodium acetate, continue to stir for 1h, transfer to 80mL reaction kettle, heat and react at 200°C for 8h, cool to room temperature naturally, wash with ethanol and deionized water alternately, and dry to obtain Fe 3 o 4 Nanoparticles.

[0033] 2. Magnetic nano-ion Fe 3 o 4 Surface hydroxylation modification:

[0034] 0.2gFe 3 o 4 Add it to 45mL sodium dodecylsulfonate solution and stir for 4h, and sonicate for 20min every hour of stirring, so as to disperse evenly. The samples were then washed and dried.

[0035] 3. Magnetic nano-ion Fe 3 o 4 Surface silanization modification:

[0036] 0.3 g of surface hydroxyla...

Embodiment 2

[0042] Embodiment 2: Adsorption experiment of magnetic base metal-organic nano core-shell material:

[0043] The adsorption material prepared in Example 1 carried out magnetic solid-phase extraction:

[0044] Add 10mL of the sample to be tested into a 20mL headspace vial, add the magnetic-based metal-organic nano core-shell material, and sonicate until the adsorption is complete. After the adsorption is completed, the adsorption material is separated from the water sample under the action of an external magnetic field. Add 5 mL of desorption solvent to the adsorbent core-shell material that has adsorbed trihalomethanes for desorption. After the desorption is completed, the desorption solution is concentrated to 50 μL and analyzed by the instrument.

[0045] Use Box-Behnken Design to optimize the important experimental conditions that affect the adsorption effect, such as: adsorption time, adsorbent quality, pH value, ionic strength ( image 3 ). The results showed that the...

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Abstract

The invention discloses a magnetic metal-organic nanometer core-shell material with an adjustable diameter and a preparation method thereof. The method comprises the following steps: adding 4,4'-bipyridine into an AgNO3 solution, carrying out uniform mixing under stirring, then adding 1,2,3-benzenetricarboxylic acid, adding KOH to adjust a pH value, carrying out a reaction at 140 DEG C to 170 DEGC so as to obtain an Ag-based metal-organic nanotube material, adding Fe3O4 with a surface modified by silane and the Ag-based metal-organic nanotube material into water, carrying out uniform ultrasonic dispersion, and adding 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 4-dimethylaminopyridine so as to prepare the magnetic metal-organic nanometer core-shell material. According tothe invention, through adjustment of the pH value, adjustment and control of the diameter and specific surface area of the material are achieved, and a maximum specific surface area can reach 177.42 m<2>/g; the contact area between an adsorbent and a trihalomethane pollutant is significantly improved; the effect of adsorption is effectively improved; the removal efficiency of adsorption reaches 90% or more; and the adsorbent can be recycled.

Description

technical field [0001] The invention relates to a magnetic-based metal-organic nano core-shell material with adjustable diameter and a preparation method thereof, which belongs to the technical field of adsorption material preparation. Background technique [0002] Although chlorination disinfection of drinking water can effectively prevent diseases, it will inevitably form disinfection by-products. Such by-products are formed by the reaction of free residual chlorine in water and natural organic matter in drinking water. Among various disinfection by-products, trihalomethanes are considered to be the main toxic carcinogens in drinking water, mainly including chloroform, monobromodichloromethane, monochlorodibromide and tribromomethane. [0003] At present, the common treatment methods for trihalomethanes in drinking water include ultrafiltration (Effects of membranehydrophilicity on the removal of a trihalomethane via micellar-enhanced ultrafiltration process, J.Membrane S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/36
CPCB01J20/22B01J20/223B01J20/06B01J20/28009C02F1/288C02F1/285C02F1/281C02F2101/36B01J2220/4812B01J2220/4806B01J2220/46
Inventor 姜炜李秋琳胡玉冰郝嘎子沃荣
Owner NANJING UNIV OF SCI & TECH
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