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Preparation method and application of porous magnetic superstructure nanocomposite

A nanocomposite material and superstructure technology, which is applied in the preparation and application of porous magnetic superstructure nanocomposite materials, can solve problems that have not yet been discovered, and achieve the effects of promoting electron transfer, mild reaction conditions, and good electrochemical activity

Active Publication Date: 2015-01-28
ANHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method and application of porous magnetic superstructure nanocomposite
  • Preparation method and application of porous magnetic superstructure nanocomposite
  • Preparation method and application of porous magnetic superstructure nanocomposite

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Embodiment 1

[0040] Ni / Ni(OH) 2 Preparation of Porous Magnetic Composite Superstructures:

[0041] 0.713g nickel chloride hexahydrate (NiCl 2 ·6H 2 O) Dissolve in 30 mL of the mixed system formed by ethylene glycol (EG) and N,N-dimethylformamide (DMF) (EG / DMF=18 / 12), stir sufficiently with magnetic force to form a homogeneous solution, then add 0.038 g sodium borohydride (NaBH 4 ), and then magnetically stirred for 10 minutes; the mixed solution was transferred to the polytetrafluoroethylene liner of a 40 mL autoclave, and the stainless steel reaction kettle was tightly sealed, and heated to 170°C for 8 hours. After the reaction, when the temperature of the reactor was lowered to room temperature, the black product was collected with a magnet, and the product was centrifuged and washed several times with deionized water. Finally, it was dried under vacuum at 60° C. for 5 hours.

[0042] The product (Cu Kα ray, λ=0.154060 nm, scan speed 0.02 o / s) for phase identification, figure 1 I...

Embodiment 2

[0045] Under ultrasonic stirring, the Ni / Ni(OH) prepared in 20 mg embodiment 1 2 The porous composite superstructure is dispersed in 50ml of Pb with a concentration of 10mg / L 2+ 、Cu 2+ and Cd 2+ In the mixed solution of ions, after mechanical stirring for 30 minutes, the concentration of remaining ions was measured with an inductively coupled plasma (ICP) atomic emission spectrometer, and it was found that: Pb 2+ The ion concentration dropped from 10mg / L before adsorption to 4.84mg / L. At this time, 51.6% of Pb 2+ ions are removed. Adsorbent to Pb 2+ The adsorption capacity of ions is 12.9 mg / g (see Figure 6 ). Cu 2+ The ion concentration dropped from 10mg / L before adsorption to 4.25mg / L, 57.5%Cu 2+ ions are removed (see Figure 7 ), adsorbed Cu 2+ The ion capacity is 14.4mg / g. But in the same system Cd 2+ The measured concentration of ions did not change significantly (see Figure 8 ).

[0046] The above results show that the porous magnetic Ni / Ni(OH) 2 Select...

Embodiment 3

[0048] 10 mg of the product obtained in Example 1 was added to 50 milliliters of 10 mg / L of Cd 2+ , Pb 2+ and Cu 2+ In the mixed solution of ions, stirring and adsorbing for different time, using ICP atomic emission spectrometer to measure, the results show that the adsorbent has a good effect on Pb after adsorption for 50 minutes. 2+ 、Cu 2+ The adsorption reaches saturation, and its adsorption effect is ~65% and ~70% (such as Figure 9 ).

[0049] The adsorbent whose adsorption reaches saturation is separated from the waste water by applying an external magnetic field, and the separated adsorbent is put into 50ml of deionized water, and ultrasonically washed several times to remove the heavy metal ions adsorbed on the surface. Figure 10 Adsorb Pb for adsorbent reuse 3 times 2+ adsorption map. The results show that the adsorbent still has a good adsorption effect after repeated three times.

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Abstract

The invention discloses a preparation method and application of a porous magnetic superstructure nanocomposite. The porous magnetic superstructure nanocomposite is prepared by using a soluble nickel salt as a raw material and a mixed solution of N,N-dimethyl formamide and glycol or glycol containing a dissolved surfactant as a medium, uniformly mixing the raw material and the medium under stirring at room temperature, adding a strong reducing agent, carrying out stirring for 5 min, reacting the obtained mixture in a reaction vessel for 1h to 10h at a temperature of 150 to 170 DEG C, cooling an obtained product to room temperature, rinsing the product with deionized water several times and drying the product under vacuum until the product has a constant weight. Compared with the prior art, the invention has the following advantages: morphology of the magnetic nanocomposite is controlled through the soluble nickel salt and hydroboron so as to obtain porous microspheres with a uniform size; the porous magnetic superstructure nanocomposite has a large specific surface area; during application, since the prepared porous superstructure nanocomposite is magnetic, the nanocomposite can be easily separated from waste water through an applied magnetic field after adsorption of heavy metals; meanwhile, the nanocomposite has good electrochemical performance and can be used for electrochemical detection of small molecules.

Description

technical field [0001] The invention relates to a preparation method and application of a porous magnetic superstructure nanocomposite material Background technique [0002] With the development of science and technology, people's lives are changing with each passing day, but they are also facing severe environmental problems. In recent years, China's annual discharge of industrial wastewater is about 8×10 8 m 3 , and the emissions are increasing year by year, which contains a large number of heavy metal ions such as chromium, zinc, copper, and mercury. Due to its high stability and strong toxicity, industrial wastewater should be strictly treated before discharge. However, neither activated carbon nor graded metal oxides can be effectively separated from large water bodies and are difficult to regenerate for practical applications. In this way, further post-processing must be carried out, which increases the cost of the application. It can be seen that these problems m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/02B01J20/28B01J20/30C02F1/28C02F1/62
Inventor 曹磊王曼倪永红
Owner ANHUI NORMAL UNIV