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Preparation and separation method of monodisperse amorphous state nickel nano particle

A superparamagnetic and separation method technology is applied in the field of preparation and separation of monodisperse superparamagnetic iron nanoparticles, and can solve the problems of unsuitable large-scale industrial production, high price, and no domestic reagents.

Active Publication Date: 2009-01-07
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method with carbonyl iron as raw material has the following defects: (1) carbonyl iron is toxic, and its decomposition temperature is low, so it is very inconvenient to store and transport
Carbonyl iron is also a material controlled by the state. Although it is produced domestically, it is mainly used in military enterprises. Currently, there are no domestic reagents for sale on the market.
And buy foreign reagents, then the price is expensive; (2) reaction medium adopts expensive high-boiling point organic ethers reagents, such as: octyl ether, diphenyl ether etc.; Monodisperse nanoparticles require further screening of nanoparticles
Therefore, this method is only suitable for laboratory research and is not suitable for large-scale industrial production.

Method used

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  • Preparation and separation method of monodisperse amorphous state nickel nano particle
  • Preparation and separation method of monodisperse amorphous state nickel nano particle
  • Preparation and separation method of monodisperse amorphous state nickel nano particle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 2mmol of iron acetylacetonate, 6ml of trioctylphosphine, 6ml of oleylamine, 2mmol of 1,2-hexadecaneol, and 40ml of liquid paraffin were put into a 100ml stainless steel autoclave reactor, and high-purity nitrogen gas was introduced to remove oxygen. Pass hydrogen gas (purity 99.9%) into the autoclave, fill the pressure to 4.0MPa, adjust the stirring speed to 500rpm, then raise the temperature to 300°C, and react for 3 hours. After the reaction was completed, the reactor was opened, and the reaction solution was taken out and placed in a 250 ml beaker. Add 40 milliliters of ethanol and 10 milliliters of petroleum ether (60-90° C.) into the beaker, stir well and place it on the surface of the permanent magnet. The liquid in the beaker will separate into two layers, remove the supernatant. Repeat the above steps 3-5 times, the black nanoparticles will be enriched at the bottom of the beaker. The obtained nanoparticles are vacuum-dried at 100° C. for one hour, and then co...

Embodiment 2

[0027] 2mmol of iron acetylacetonate, 2ml of trioctylphosphine, 3ml of oleylamine, and 40ml of liquid paraffin were put into a 100ml stainless steel autoclave reactor, and high-purity nitrogen gas was introduced to remove oxygen. Pass hydrogen gas (purity 99.9%) into the autoclave, fill the pressure to 4.0MPa, adjust the stirring speed to 500rpm, then raise the temperature to 300°C, and react for 5 hours. After the reaction was completed, the reactor was opened, and the reaction solution was taken out and placed in a 250 ml beaker. Add 40 milliliters of ethanol and 10 milliliters of petroleum ether (60-90° C.) into the beaker, stir well and place it on the surface of the permanent magnet. The liquid in the beaker will separate into two layers, remove the supernatant. Repeat the above steps 3-5 times, the black nanoparticles will be enriched at the bottom of the beaker. The obtained nanoparticles are vacuum-dried at 100° C. for one hour, and then cooled to obtain nanoparticle...

Embodiment 3

[0029]2mmol of iron acetylacetonate, 2ml of trioctylphosphine, 3ml of oleylamine, and 40ml of liquid paraffin were put into a 100ml stainless steel autoclave reactor, and high-purity nitrogen gas was introduced to remove oxygen. Feed high-purity nitrogen (purity 99.99%) into the autoclave, fill the pressure to 4.0 MPa, adjust the stirring speed to 500 rpm, then raise the temperature to 300° C., and react for 5 hours. After the reaction was completed, the reactor was opened, and the reaction solution was taken out and placed in a 250 ml beaker. Add 40 milliliters of ethanol and 10 milliliters of petroleum ether (60-90° C.) into the beaker, stir well and place it on the surface of the permanent magnet. The liquid in the beaker will separate into two layers, remove the supernatant. Repeat the above steps 3-5 times, the black nanoparticles will be enriched at the bottom of the beaker. The obtained nanoparticles are vacuum-dried at 100° C. for one hour, and then cooled to obtain ...

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Abstract

A method for preparing and separating monodisperse superparamagnetic iron nanoparticles that can be completely dissolved in polar and non-polar organic solvents comprises the following steps: taking iron acetylacetonate as a raw material; taking whiteruss as a reaction medium; taking trioctyl phosphine and oleylamine as stabilizing agents (or: protective solutes, surface modifying agents); taking an organic ferric compound as a catalyzer; taking polylol as a morphological modifying agent; mixing the above substances in a kettle-type reactor according to a certain ratio; heating the substances with hydrogen to the reaction temperature (150 to 350 DEG C); reacting for 3 hours; obtaining iron nanoparticles of good crystallinity; and adopting an external applied magnetic field to assist the solvent fractionating method, so as to separate the iron nanoparticles from the reaction system. The powdery iron nanoparticles can once again disperse into organic solvents such as chloroform, sherwood oil, etc. without sedimentation.

Description

technical field [0001] The invention relates to a method for preparing and separating monodisperse superparamagnetic iron nanoparticles, which belongs to the improvement and innovation of the method for preparing and separating magnetic nanoscale materials. The prepared monodisperse superparamagnetic iron nanoparticles can be completely dissolved in polar and nonpolar organic solvents. Background technique [0002] Magnetic nanoparticles are an important part of nanoscale materials. The only magnetic elements at room temperature are iron, cobalt, and nickel, among which iron has the largest saturation magnetization. Iron is the most abundant metal element in nature, so the preparation of pure iron nanoparticles not only has important theoretical value, but also has broad application prospects. Since iron is a relatively active transition metal element and nanoscale ferrite is more stable, there are few reports on pure iron nanoparticles in the literature. The only methods...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/26
Inventor 张宏玉刘峰奎阙国和刘东邓文安沐宝泉金环年李庶峰文萍于建宁
Owner BC P INC CHINA NAT PETROLEUM CORP
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