Method for preparing nanometer zero-valent iron grain using improved liquid phase reduction method

A technology of nano-zero-valent iron and reduction method is applied in the field of preparation of nano-zero-valent iron particles, which can solve the problems of easy agglomeration and uneven particle distribution, and achieve the effects of low production cost, easy operation and fast preparation.

Inactive Publication Date: 2006-12-13
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] Aiming at the problems of uneven particle distribution, easy agglomeration, and the need for nitrogen protection during the process of preparing nano-zero-valent iron particles by liquid phase reduction method
The invention provides a met

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  • Method for preparing nanometer zero-valent iron grain using improved liquid phase reduction method
  • Method for preparing nanometer zero-valent iron grain using improved liquid phase reduction method

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Weigh 0.139 g FeSO 4 .7H 2 O, dissolved in distilled water, made into 0.01M FeSO 4 .7H 2 O aqueous solution 50ml, electromagnetic stirring to make it fully mixed. The solution was then poured into an Erlenmeyer flask and placed on a mechanical stirrer. Weigh 0.0567g NaBH 4 , dissolved in distilled water, made into 0.03M NaBH 4 Aqueous solution 50ml. Under the condition of mechanical stirring, the NaBH 4 The aqueous solution is rapidly added to the FeSO 4 .7H 2 O aqueous solution, continue stirring for 5-15 seconds, and stop stirring when the solution turns black. Selected by magnetic separation, first washed three times with distilled water, then fully washed three times with acetone, and stored in acetone.

[0040] The test results of TEM show that the particle size range is 10-100nm, and the particle size distribution is not uniform.

[0041] The XRD test results show that: when the scanning diffraction angle (2θ) is 30°-100°, the corresponding 2θ when the ...

Embodiment 2

[0044] Weigh 0.139 g FeSO 4 .7H 2 O, dissolved in distilled water, made into 0.01M FeSO 4 .7H 2 O aqueous solution 50ml, then add 0.1g polyvinylpyrrolidone (PVP K-30), electromagnetic stirring to make it fully mixed. The solution was then poured into an Erlenmeyer flask and placed on a mechanical stirrer. Weigh 0.0567g NaBH 4 , dissolved in distilled water, made into 0.03M NaBH 4 Aqueous solution 50ml. Under the condition of mechanical stirring, 50mlNaBH 4 The aqueous solution was quickly poured into the FeSO 4 .7H 2 O aqueous solution, continue to stir for a few seconds, stop stirring when the solution turns black. Selected by magnetic separation, first washed three times with distilled water, then fully washed three times with acetone, and stored in acetone.

[0045] The test result of TEM shows that: the particle size range is 44-96nm, and the average particle size is 780nm.

[0046] The XRD test results show that: when the scanning angle (2θ) is 30°-100°, the co...

Embodiment 3

[0049] Weigh 0.139 g FeSO 4 .7H 2 O, dissolved in distilled water, made into 0.01M FeSO 4 .7H 2 O aqueous solution 50ml, then add 0.2g polyvinylpyrrolidone (PVP K-30), electromagnetic stirring to make it fully mixed. The solution was then poured into an Erlenmeyer flask and placed on a mechanical stirrer. Weigh 0.0567g NaBH 4 , dissolved in distilled water, made into 0.03M NaBH 4 Aqueous solution 50ml. Under the condition of mechanical stirring, 50mlNaBH 4 The aqueous solution was quickly poured into the FeSO 4 .7H 2 O aqueous solution, continue to stir for a few seconds, stop stirring when the solution turns black. Selected by magnetic separation, first washed three times with distilled water, then fully washed three times with acetone, and stored in acetone.

[0050] The test result of TEM shows that: the particle size range is 43-76nm, and the average particle size is 60nm.

[0051] The XRD test results show that: when the scanning angle (2θ) is 30°-100°, the cor...

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Abstract

The invention discloses a method for preparing nanometer iron particle with a modified liquid phase reduction method. The main steps comprise: preparing soluble ferric salt solution and NaBH4 or KBH4 solution; adding polyethylene pyrrolidone into said soluble ferric salt solution according to a certain proportion, stirring evenly; adding NaBH4 or KBH4 solution into said soluble ferric salt solution under continuous stirring condition, stirring continuously until solution changes into black; selecting nanometer iron particle with magnetic method; washing with distilled water firstly, then washing with acetone or alcohol, storing in acetone or alcohol. The invention needs no nitrogen protective device, process is easy for operation, production cost is low; the distribution of got nanometer iron particle is homogenous (40-80nm), average particle size is 60 nm, specific surface area is 45-56m2/g, and there is no ferric oxide.

Description

1. Technical field [0001] The invention relates to a method for preparing nanometer zero-valent iron particles, in particular to a method for preparing nanometer zero-valent iron particles by using an improved liquid phase reduction method. 2. Background technology [0002] Zero-valent ferroelectricity is relatively large and has strong reducibility. It can be used to treat certain trace organic pollutants in water bodies, and can act as a catalyst to accelerate the reaction process. Both indoor experiments and field tests have shown that zero-valent iron particles can degrade halogenated aliphatic hydrocarbons, halogenated aromatic hydrocarbons, and some polychlorinated biphenyl chemical pollutants, that is, when pollutants such as halogenated hydrocarbons or halogenated aromatic hydrocarbons After the halogen atoms on the surface get the electrons provided by the zero-valent iron, the halogens will fall off from the molecules, and the halogenated pollutants will be transf...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 王晓栋高树梅王海燕刘洋刘树深王连生
Owner NANJING UNIV
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