Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method

A technology of nano-zero-valent iron and reduction method, which is applied in the field of preparation of nano-zero-valent iron and nano-zero-valent iron particles by liquid-phase complexation reduction method, which can solve the problems of time-consuming operation, easy agglomeration, easy oxidation, etc. problems, to achieve the effect of convenient operation, simple equipment and uniform distribution

Inactive Publication Date: 2013-07-31
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Aiming at the problems that the particle size distribution of nano zero-valent iron prepared by the current liquid phase reduction method is uneven, easy to agglomerate, time-consuming in the operation process, and easily oxidized, the purpose of the present invention is to improve the liquid phase reduction method without the need for Under the condition of adding surfactant, nano-iron particles with better dispersion, uniform particles and smaller particle size (about 5~20nm) can be synthesized

Method used

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  • Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method
  • Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0042] In 20mL of distilled water, add 0.6934g FeSO 4 (NH 4 ) 2 SO 4 ·6H 2 0 and 0.8032g sulfosalicylic acid, adjust the pH of the solution to be 6, then add 20mL of THF, stir to make it fully mixed. Weigh 0.2gNaBH 4 Dissolve in the mixed system of 20mL THF and water (volume ratio 1:1), and finally drop the sodium borohydride solution into the complex ferrous salt solution at a rate of 2-3 drops / second, and control The reaction time is 15 min, and the nano-iron particles are washed three times with distilled water and absolute ethanol respectively, and then the nano-iron particles are stored in absolute ethanol.

[0043] The test result of TEM shows that the range of particle size is about 5-20m, and the average particle size is 16nm.

[0044] The XRD test results show that: when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 44.4732°, 65.8241°, and 82.9826°, respectively, and compared with the standard PDF card ...

Embodiment 2

[0047] In 13mL of distilled water, add 0.6986g FeSO 4 (NH 4 ) 2 SO 4 ·6H 2 0 and 0.8046g sulfosalicylic acid, adjust the pH of the solution to be 6, then add 27mL of THF, stir to make it fully mixed. Weigh 0.2gNaBH 4 Dissolve in the mixed system of 20mL THF and water (volume ratio 1:1), and finally drop the sodium borohydride solution into the complex ferrous salt solution at a rate of 2-3 drops / second, and control The reaction time is 15 min, and the nano-iron particles are washed three times with distilled water and absolute ethanol respectively, and then the nano-iron particles are stored in absolute ethanol.

[0048] The test result of TEM shows that the range of particle size is about 5-20m, and the average particle size is 15nm.

[0049] The XRD test results show that: when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 45.1752°, 65.0724°, and 82.1429°, respectively. Compared with the standard PDF card of i...

Embodiment 3

[0052] In 27mL of distilled water, add 0.7023g FeSO 4 (NH 4 ) 2 SO 4 ·6H 2 0 and 0.8174g sulfosalicylic acid, adjust the pH of the solution to be 6, then add 13mL of THF, stir to make it fully mixed. Weigh 0.2gNaBH 4 Dissolve in a mixed system of 20mL THF and water (volume ratio 1:1), and finally drop the sodium borohydride solution into the complex ferrous salt at a rate of 2-3 drops / second, and control the reaction after dropping The time is 15 minutes. After washing the nano-iron particles with distilled water and absolute ethanol three times respectively, the nano-iron particles are stored in absolute ethanol.

[0053] The test result of TEM shows that the range of particle size is about 5-20m, and the average particle size is 18nm.

[0054] The XRD test results show that: when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 44.2485°, 65.7484°, and 82.6836°, which are found by comparing the standard PDF card o...

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Abstract

Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method comprises the following steps of: dissolving soluble ferrous salt and complexing agent sulfosalicylic acid with water, adjusting pH value of the solution to be between 5 and 7 to obtain complexing ferrous solution; adding tetrahydrofuran into the complexing ferrous solution and mixing uniformly; adding NaBH4 solution or KBH4 solution into the complexing ferrous solution, proceeding liquid phase reduction reaction while stirring so that complexing-state ferrous ions are reduced to finally obtainnano zero-valent iron particles. According to the method for preparing the nano zero-valent iron particles, no surfactant is added during preparation process; the made nano zero-valent iron particle has good dispersibility and uniform distribution; the particle size range is about 5-20nm, average particle size is about 10-18nm and specific surface area is 70-90m<2> / g; has and no obvious oxidationphenomenon happens.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial synthesis technology, and relates to a method for preparing nanometer zero-valent iron particles, in particular to a method for preparing nanometer zerovalent iron through an improved liquid phase complexation reduction method. Background technique [0002] Due to its small particle diameter, large specific surface area and surface energy, nano-iron has excellent adsorption performance and high reduction activity. Utilizing its unique surface effect and small size effect, its reactivity and degradation efficiency can be greatly improved. At the same time, iron particles are also environmentally friendly substances, so they have unique advantages in groundwater remediation. At present, the use of nano-iron particles to remove inorganic salts, organic matter, and heavy metal pollutants in water has been reported in the literature. The strong decontamination and water purification capabilities a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24
Inventor 崔世海吉祖峰
Owner NANJING NORMAL UNIVERSITY
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