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

A nano-zero-valent iron and reduction method, applied in nanotechnology and other directions, can solve the problems of uneven particle shape, size, and particle agglomeration, and achieve the effects of simple equipment, uniform distribution, and convenient operation.

Inactive Publication Date: 2018-01-05
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main bottleneck of the liquid phase reduction method is that the shape and size of the particles are easy to be uneven in the preparation process, and the agglomeration between the particles is easy to occur. Therefore, some scholars improve the dispersion of iron particles by adding surfactants.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Measure 10mL 0.1mol·L respectively -1 FeCl 3 solution and 0.1mol·L -1 NaH 2 PO 4 Solution, adjust the pH value of the system to 4 after mixing, then add 20mL of tetrahydrofuran, stir to make it fully mixed. Weigh 0.32gNaBH 4 Dissolve in 10mL of tetrahydrofuran and water (volume ratio: 1:1) mixture, and finally drop the sodium borohydride solution into the complex iron salt solution at a rate of 2-3 drops / second, and control the reaction after the addition is complete The time is 15 min. After washing the nano-iron particles with anaerobic deionized water and absolute ethanol three times respectively, the nano-iron particles are stored in absolute ethanol.

[0041] The test result of TEM shows that the range of particle size is about 50-80m, and the average particle size is 66nm.

[0042] The XRD test results show that: when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 45.4453°, 65.0265°, and 82.1369°, wh...

Embodiment 2

[0045] Add 10mL 0.1mol·L respectively -1 FeCl 3 solution and 0.3mol·L -1 NaH 2 PO 4 Solution, adjust the pH value of the system to 5, then add 20mL of tetrahydrofuran, stir to make it fully mixed. Weigh 0.32gNaBH 4 Dissolve in 10mL of tetrahydrofuran and water (volume ratio: 1:1) mixture, and finally drop the sodium borohydride solution into the complex iron salt solution at a rate of 2-3 drops / second, and control the reaction after the addition is complete The time is 15 min. After washing the nano-iron particles with anaerobic deionized water and absolute ethanol three times respectively, the nano-iron particles are stored in absolute ethanol.

[0046] TEM test results show that: the range of particle size is about 50-80m, and the average particle size is 64nm.

[0047] The XRD test results show that: when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 45.1269°, 65.7531°, and 82.1568°, respectively, and compare...

Embodiment 3

[0050] Add 10 mL of 0.1 mol L to 28 mL of distilled water -1 Fe 2 (SO 4 ) 3 solution and 0.2mol·L - 1 NaH 2 PO 4 Solution, adjust the pH value of the system to 6, then add 12mL of tetrahydrofuran, stir to make it fully mixed. Weigh 0.32gNaBH 4 Dissolve in 10mL of tetrahydrofuran and water (volume ratio: 1:4) mixture, and finally drop the sodium borohydride solution into the complex iron salt at a rate of 2-3 drops / second, and control the reaction time after the addition is complete After 20 min, the nano-iron particles were washed three times with anaerobic deionized water and absolute ethanol, and then the nano-iron particles were stored in absolute ethanol.

[0051] The test result of TEM shows that the range of particle size is about 50-80m, and the average particle size is 63nm.

[0052] The XRD test results show that: when the scanning diffraction angle 2θ is 30°~100°, the corresponding 2θ when the diffraction peaks appear are 45.2568°, 65.1237°, and 82.5648°, re...

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Abstract

The invention relates to a method for preparing nanometer zero-valent iron on the basis of a liquid complexing reduction method. Iron salt and a phosphate solution are mixed to form a complex, and the pH value of a system is adjusted to 4-7; in mixed liquor of tetrahydrofuran and water, excessive NaBH4 or KBH4 is used as a reducing agent, a liquid phase reduction reaction is conducted under the condition of stirring, and iron ions in the complex are reduced to prepare nanometer zero-valent iron particles. According to the method, surfactants and other dispersing agents do not need to be added in the preparation process; the prepared nanometer particles are good in dispersity and uniform in particle size distribution, the particle sizes of the prepared nanometer particles range from 50 nm to 80 nm approximately, the specific surface area of the prepared nanometer particles is 70-90 m<2> / g, and the prepared products are free of an obvious oxidation phenomenon.

Description

technical field [0001] The invention relates to a method for preparing nanometer zero-valent iron particles, and belongs to the technical field of nanometer material synthesis technology. In particular, it relates to a method for preparing nanometer zero-valent iron through a liquid-phase complexation reduction method. Background technique [0002] Due to its small particle diameter, large specific surface area and strong surface activity, nano-iron has superior adsorption capacity, good chemical reduction activity and high catalytic activity. Its unique size effect and surface effect greatly improve the reactivity and degradation efficiency of pollutants; at the same time, as an environmentally friendly material, zero-valent iron has its unique advantages in the restoration of groundwater and drinking water . At present, there are more and more literature reports on the use of nano-iron to remove heavy metals, organic matter, inorganic salts and other pollutants in water....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B82Y40/00
CPCB22F9/24B82Y40/00
Inventor 崔世海杨静张大鹏陈慧慧
Owner NANJING NORMAL UNIVERSITY
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