Method for preparing zerovalent iron nanoparticles by improved liquid phase reduction method

A technology of zero-valent nano-iron and reduction method, which is applied in the field of synthesis of nano-materials by chemical reduction method, to achieve the effect of convenient operation, uniform distribution and good dispersion

Inactive Publication Date: 2011-01-26
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] By consulting the relevant literature and patents related to the synthesis of nano-iron at home and abroad, the results show that before the completion of the present invention, there has been no need to add...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 0.5952mol / L of Fe in a 250mL three-necked flask 3+ 3mL of aqueous solution and 20mL of distilled water were stirred to make them fully mixed, and then 0.59g of NaF and 20mL of THF were added in sequence to adjust the pH to 4. Weigh 0.4gKBH 4 Dissolve in the mixed system of 20mL THF and water (volume ratio is 1: 1), finally add potassium borohydride solution in the three-necked flask at the speed of 2-3 drops / second, control the reaction time after dropping is completed After 30 min, the nano-iron particles were washed three times with distilled water and absolute ethanol, and then the nano-iron particles were stored in absolute ethanol.

[0037] The test result of TEM shows that the range of particle size is about 30-80m, and the average particle size is 58nm.

[0038]The XRD test results show that: from the XRD test results, when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 44.68°, 64.23°, and 81.45°, r...

Embodiment 2

[0041] Add 0.5952mol / L of Fe in a 250mL three-necked flask 3+ 3mL of aqueous solution and 13mL of distilled water were stirred to make them fully mixed, and 0.59gNaF and THF27mL were added in turn to adjust the pH to 5. Weigh 0.4g KBH 4 Dissolve in 20mL of THF and water (1:1) mixed system, and finally add the alcoholic aqueous solution of potassium borohydride into the three-necked flask at a rate of 2 to 3 drops / second, and control the reaction time to 45min after the addition is completed , after washing the nano-iron particles with distilled water and absolute ethanol three times respectively, the nano-iron particles were stored in absolute ethanol.

[0042] The test result of TEM shows that the range of particle size is about 42-75nm, and the average particle size is 52nm.

[0043] The XRD test results show that: from the XRD test results, when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 44.08°, 64.56°, and 81...

Embodiment 3

[0046] Add 0.5952mol / L of Fe in a 250mL three-necked flask 3+ 1.5mL of aqueous solution and 13mL of distilled water, stir to make them fully mixed, add 0.28gNaF and THF27mL in sequence, and adjust the pH to 4. Weigh 0.4g KBH 4 Dissolve in the mixed system of 20mL of THF and water (1:1), and finally add the aqueous solution of potassium borohydride into the three-necked flask at a rate of 2-3 drops / second, and control the reaction time to 30min after the addition is completed. After the nano-iron particles were washed three times with distilled water and absolute ethanol, the nano-iron particles were stored in absolute ethanol.

[0047] The test result of TEM shows that the range of particle size is about 45-60nm, and the average particle size is 50nm.

[0048] The XRD test results show that: from the XRD test results, when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 43.98°, 64.63°, and 81.36°, respectively. Compar...

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PUM

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Abstract

The invention discloses a method for preparing zerovalent iron nanoparticles by an improved liquid phase reduction method. The method comprises the following steps of: (1) preparing 0.03 to 0.07mol/L Fe3<+> solution in distilled water; (2) adding NaF in an amount which is 7 to 9 times that of the Fe3<+> into the solution in step (1) to form FeF63<-> solution; (3) adding tetrahydrofuran into the system in step (2), wherein the volume ratio of the tetrahydrofuran to the solution in step (1) is 1:2-2:1; (4) dissolving KBH4 into the mixed solution of tetrahydrofuran and water, and reacting under the stirring; and (5) washing iron nanoparticles with distilled water and ethanol respectively, and keeping the iron nanoparticles in absolute ethanol. In the process of synthesizing the iron nanoparticles, an organic macromolecule surfactant does not need to be added; nitrogen protection is not needed; the equipment is simple; and the operation is convenient. The prepared iron nanoparticles are uniformly distributed; the average grain diameter is 50nm; the dispersibility is relatively good; the specific surface area is 42 to 60m<2>/g; and an impurity, namely iron oxide, does not appear.

Description

technical field [0001] The invention relates to a preparation method of zero-valent nano-iron, which belongs to the technical field of synthesizing nano-materials by chemical reduction method. In particular, it relates to a method for preparing zero-valent nano-iron particles by using an improved liquid phase reduction method. Background technique [0002] Since the 1990s, nano-zero-valent iron has attracted more and more attention from the scientific community in the pollution control of organic chlorinated compounds. The physical and chemical properties of nano zero-valent iron particles, such as small volume, large specific surface area, and strong reducibility, can accelerate the reduction and degradation reaction process of pollutants. Studies have shown that organic pollutants including chlorinated alkanes, chlorinated alkenes, chlorinated aromatics and organochlorine pesticides can be reductively degraded in the presence of nano-sized zero-valent iron. [0003] At p...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 崔世海
Owner NANJING NORMAL UNIVERSITY
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