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Preparation method of highly dispersed ultra-small zero-valence iron nano-cluster and application

A technology of nano-clusters and zero-valent iron, which is applied in nanotechnology, chemical instruments and methods, water/sludge/sewage treatment, etc., can solve the difficulty of recovery and circulation of nano-zero-valent iron, is easy to be oxidized, and cannot control nano-zero Iron valence crystal growth and other problems, to achieve high catalytic reduction performance, the effect of mild conditions

Active Publication Date: 2019-01-15
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, various modification materials reported so far cannot control the crystal growth of nano-ZVF to prepare ultra-small metal nanoclusters.
The reactivity and catalytic ability of ultra-fine metal nanoclusters are greatly improved compared with ordinary nanoscale particles. Some people have prepared highly dispersed noble metal nanoparticles with a particle size of less than 1nm, such as palladium and gold. However, due to the Zero-valent iron particles have strong van der Waals force and magnetic attraction, and the synthesis of zero-valent iron nanoclusters with extremely small particle sizes while maintaining their surface activity and avoiding agglomeration is a challenging problem
In addition, even under anoxic environment, nano-ZVI particles are easily oxidized after removal of pollutants, which makes the recovery and recycling of nano-ZVI very difficult.
[0003] So far, through searching, we have not found relevant reports on the preparation and application of zero-valent iron nanoclusters from the information we have.

Method used

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  • Preparation method of highly dispersed ultra-small zero-valence iron nano-cluster and application
  • Preparation method of highly dispersed ultra-small zero-valence iron nano-cluster and application
  • Preparation method of highly dispersed ultra-small zero-valence iron nano-cluster and application

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Experimental program
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Effect test

Embodiment 1

[0024] Step S1: Add the surfactant CTAB (10mmol) to deionized water and stir for 30 minutes to form a micelle solution (its concentration is greater than the critical micelle concentration 0.9mmol / L), and FeCl 3 ·6H 2 O (1mmol) is dissolved in hydrochloric acid solution to form Fe 3+ / Hydrochloric acid mixed solution, then Fe 3+ / Hydrochloric acid mixed solution was added dropwise to the micellar solution to obtain mixed solution A;

[0025] Step S2: Add thiourea (1mmol) to deionized water and stir for 30 minutes to form a thiourea solution, dissolve sodium hydroxide (5mmol) in deionized water to form a sodium hydroxide solution, and then add the sodium hydroxide solution dropwise to In the thiourea solution, stir and mix to obtain mixed solution B;

[0026] Step S3: Drop the mixed liquid B into the mixed liquid A and stir and mix uniformly to obtain the mixed liquid C, and add NaBH 4 (25mmol) was added to the mixture C to react to prepare a zero-valent iron nanocluster suspension. ...

Embodiment 2

[0029] In order to evaluate the reactivity of the synthesized zero-valent iron nanoclusters, the zero-valent iron nanoclusters were used to catalytically reduce and remove p-nitrophenol in the solution. The specific steps are as follows:

[0030] Step S1: Add 40 mL of prepared zero-valent iron nanocluster suspension (0.46 mM) and 0.005 g of NaBH into a 50 mL Erlenmeyer flask. 4 And 1.4mL of p-nitrophenol (4mM), the solution should be magnetically stirred at 20℃;

[0031] Step S2: After stirring for 1 min, take 1.4 mL of the reaction solution for filtration, and then scan and analyze with an ultraviolet-visible spectrophotometer;

[0032] Step S3: Add 0.005g of NaBH before proceeding to the next cycle experiment 4 , Then add 1.4:mL p-nitrophenol aqueous solution (4mM), NaBH 4 And the concentration of p-nitrophenol remains constant at the beginning of each cycle. In the same NaBH 4 At the same concentration, the same zerovalent iron nanoclusters were cyclically reacted 8 times.

[0033]...

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Abstract

The invention discloses a preparation method of a highly dispersed ultra-small zero-valence iron nano-cluster and application, and belongs to the technical field of environmental nanomaterial preparation and organic pollutant treatment. According to the technical scheme, the preparation method comprises the following steps that Fe<3+> is encapsulated in a surfactant CTAB micelle; the release of S<2-> from thiourea is controlled under alkaline condition to form a FeS nanocluster as an intermediate body; and the FeS nanocluster is reduced by NaBH4 to obtain the highly dispersed zero-valence ironnano-cluster with diameter less than 1mm. The invention further discloses application of the of zero-valent iron nanocluster as a catalyst in the catalytic reduction of organic reactions in the presence of the NaBH4. According to the preparation process of the zero-valence iron nano-cluster, condition is mild, operation is simple, and achievement is easy. The zero-valent iron nanocluster has remarkable catalytic reduction activity to nitrophenol in water, and can be reused in the presence of the NaBH4 and maintain high catalytic activity.

Description

Technical field [0001] The invention belongs to the technical field of environmental nanomaterial preparation and organic pollutant treatment, and specifically relates to a preparation method and application of highly dispersed ultra-small zero-valent iron nanoclusters. Background technique [0002] In recent years, nano-zero-valent iron has received extensive attention from scientific researchers due to its high reduction activity, environmental protection and low economic cost. Nano-zero-valent iron particles are often used in wastewater treatment and groundwater remediation. A large number of studies have shown that nano-zero-valent iron is an effective water treatment material that can be used to remove various pollutants, such as nitrite, selenate, antibiotics, aromatic halides and heavy metal pollutants. However, similar to other nanomaterials, nano-zero-valent iron particles are not only aggregated into larger-sized particles driven by strong magnetism and van der Waals fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B82Y40/00B01J23/745C02F1/70C02F101/34C02F101/38
CPCB82Y40/00C02F1/705B01J23/745B22F9/24C02F2101/345C02F2101/38B01J35/393
Inventor 樊静师东阳程萌张晓迪李想张霞吴甜时悦悦付元奇杨西通
Owner HENAN NORMAL UNIV
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