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A kind of preparation method of high-purity nano ferric oxide

A ferric tetroxide and nanotechnology, which is applied in the field of preparation of high-purity nano ferric tetroxide, can solve the problems of low rate performance, volume change particle agglomeration, poor cycle stability of negative electrode materials, etc. The effect of low cost and simple process

Active Publication Date: 2019-08-13
沈丽娜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Compared with carbon materials, some electrochemically active metals and metal oxides, such as tin, silicon, tin dioxide, cobalt tetroxide, etc., have higher theoretical capacity and are one of the negative electrode materials with great development potential. Good electronic conductivity, low price, abundant resources, non-toxicity and environmental friendliness, etc., but huge volume changes and serious particle agglomeration will occur during the intercalation and delithiation process, resulting in charge and Li + Poor transmission and diffusion performance, poor cycle stability and low rate performance as a negative electrode material

Method used

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Embodiment 1

[0043] A preparation method of high-purity nano ferric oxide, which comprises the following steps:

[0044] (1) Iron salt, ammoniacal liquor and oxidizing agent are joined in the reactor together, and at temperature is 235 ℃, and pressure is 1.8 atmospheres, and the pH of control reaction system is 7.55, and pH is the pH value under 25 ℃ of temperature, reacts An oxidation-reduction potential meter is installed on the kettle. When the ORP of the redox potential meter is 235mV, stop feeding, continue to react at high temperature for 2.5 hours, and observe the ORP value of the redox potential meter at the same time. When the ORP value is greater than 250mV, pass Inject hydrogen to reduce the ORP value to 235mV, then continue to increase the pressure to 3.2 atmospheres, maintain the pH of the reaction system at 8.03, the pH is the pH value at a temperature of 25°C, and the temperature is 168°C, and feed hydrogen to make the solution ORP value decreased to -25mV, and reacted for 2...

Embodiment 2

[0056] A preparation method of high-purity nano ferric oxide, which comprises the following steps:

[0057](1) Iron salt, ammoniacal liquor and oxidizing agent are joined in the reactor together, and at temperature is 245 ℃, and pressure is 1.89 atmospheric pressure, and the pH of control reaction system is 7.48, and pH is the pH value under 25 ℃ of temperature, reacts An oxidation-reduction potential meter is arranged on the kettle. When the ORP of the redox potential meter is 205mV, stop feeding, continue to react at high temperature for 2.5 hours, and observe the ORP value of the redox potential meter at the same time. When the ORP value is greater than 250mV, pass Inject hydrogen to reduce the ORP value to 205mV, then continue to increase the pressure to 3.68 atmospheres, maintain the pH of the reaction system at 7.99, the pH is the pH value at a temperature of 25°C, and the temperature is 168°C, and feed hydrogen to make the solution ORP value decreased to 25mV, and react...

Embodiment 3

[0068] A preparation method of high-purity nano ferric oxide, which comprises the following steps:

[0069] (1) Add iron salt, ammonia water and oxidant to the reaction kettle together, and control the pH of the reaction system to 7.55 at a temperature of 220-250°C and a pressure of 1.98 atmospheres, and the pH is the pH value at a temperature of 25°C , the reactor is equipped with an oxidation-reduction potential meter, when the ORP of the redox potential meter is 208mV, stop feeding, continue to react at high temperature for 2.3 hours, and observe the ORP value of the redox potential meter at the same time, when the ORP value is > 250mV , feed hydrogen to reduce the ORP value to 208mV, then continue to increase the pressure to 3.5 atmospheres, maintain the pH of the reaction system at 8.07, the pH is the pH value at a temperature of 25°C, and the temperature is 175°C, and feed hydrogen to make The ORP value of the solution was reduced to -10mV, and reacted for 23 minutes;

...

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Abstract

The invention discloses a preparation method of high-purity nano ferriferrous oxide. The preparation method comprises the following steps: adding ferric salt, ammonium hydroxide and oxidant into a reaction kettle for reaction, then introducing hydrogen, reacting at high temperature and high pressure, filtering, purifying materials with concentrated sulfuric acid and washing, then drying, crushing and performing vacuum packaging, concentrating, evaporating and crystalizing waste water obtained to recycle ammonium salt, condensing the evaporated water and recycling. The preparation method of high-purity nano ferriferrous oxide is simple in technology, zero emission of waste water can be realized, the cost is low, the particle size and purity of the finally prepared feriferrous oxide are respectively 30-50 nanometers and greater than 99.8%, the content of ferrous in the ferriferous oxide is higher than 23.9%, and the anti-oxidization capability is greatly enhanced.

Description

technical field [0001] The invention relates to a preparation method of high-purity nano ferric oxide, which belongs to the field of new materials. Background technique [0002] Ferric oxide, chemical formula Fe 3 o 4 . Commonly known as iron oxide black, magnet, magnet, and black iron, it is a black crystal with magnetic properties, so it is also called magnetic iron oxide. This substance is soluble in acid solution, insoluble in water, alkali solution and organic solvents such as ethanol and ether. Natural ferric ferric oxide is insoluble in acid solution, and is easily oxidized to iron oxide (Fe2O3) in air in a humid state. Usually used as pigments and polishes, it can also be used in the manufacture of audio tapes and telecommunications equipment. Iron tetroxide contains Fe 2+ and Fe 3+ , X-ray diffraction experiments show that Fe3O4 has a trans-spinel structure, the crystal Metaferrate ion FeO is never present in 2 2- . Iron tetroxide, also known as magnetic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08B82Y40/00
CPCB82Y40/00C01G49/08C01P2004/62C01P2004/64C01P2006/11C01P2006/12C01P2006/80
Inventor 沈丽娜
Owner 沈丽娜
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