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A kind of preparation method of nano antimony trioxide

A technology of antimony trioxide and antimony trichloride, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxyacid, nanotechnology, etc., can solve the problem of high implementation conditions, complicated process, induced dermatitis, etc. question

Active Publication Date: 2020-07-28
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Antimony trioxide is not very toxic, but it has irritating effects on the nose, eyes, throat and respiratory tract and other organs, and it can induce dermatitis if it contacts the skin
Although this method can prepare antimony trioxide superfine powder, its implementation conditions are relatively high, the process is complicated, and the cost is high, which is not conducive to large-scale implementation and use.

Method used

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  • A kind of preparation method of nano antimony trioxide
  • A kind of preparation method of nano antimony trioxide

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Take 16.0mmol SbCl 3 , dissolved in 40ml of ethylene glycol, added 20ml of distilled water and stirred for 20 minutes (the purpose of adding distilled water and stirring is to make SbCl 3 Hydrolysis, the reaction is 2SbCl 3 + 3H 2 O==Sb 2 o 3 + 6HCl), and then adjusted the pH of the solution to 9 with 6mol / L sodium hydroxide, stirred evenly, and transferred it to a 120°C reactor for 15 hours. After the reaction, cool the system to room temperature, filter it with suction, wash (ethanol and distilled water) several times, and dry at 60°C to obtain micron antimony trioxide; then dissolve micron antimony trioxide in ethylene glycol, and add Distilled water was reacted at 110°C for 1 hour (to hydrolyze it to obtain antimony trioxide), followed by suction filtration and drying to obtain nano antimony trioxide with an average particle size of 300nm. Yield: 99.5%.

Embodiment 2

[0021] Take 16.0mmol SbCl 3 , dissolved in 40ml of ethanol (EA), added 40ml of distilled water and stirred for 20 minutes, then adjusted the pH of the solution to 9 with 6mol / L sodium hydroxide, stirred evenly, and moved it into a 60°C reactor to react for 15h. After the reaction, cool the system to room temperature, filter it with suction, wash (ethanol and distilled water) several times, and dry at 60°C to obtain micron antimony trioxide; then dissolve micron antimony trioxide in ethylene glycol, and add Distilled water (hydrolyzed to obtain antimony trioxide) was reacted at 110°C for 1 hour, followed by suction filtration and drying to obtain nano antimony trioxide with an average particle size of 300nm. Yield: 99.6%.

Embodiment 3

[0023] Take 16.0mmol SbCl 3 , dissolved in 40ml of methanol, added 40ml of distilled water and stirred for 20 minutes, then adjusted the pH of the solution to 9 with 6mol / L sodium hydroxide, stirred evenly and moved into a 60°C reactor for 15 hours. After the reaction, cool the system to room temperature, filter it with suction, wash (ethanol and distilled water) several times, and dry at 60°C to obtain micron antimony trioxide; then dissolve micron antimony trioxide in ethylene glycol, and add 20ml of distilled water was reacted at 110°C for 1 hour, followed by suction filtration and drying to obtain nanometer antimony trioxide with an average particle size of 300nm. Yield: 99.6%.

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Abstract

The invention discloses a preparation method of nano antimony trioxide. The preparation method comprises the following steps: dissolving antimony trichloride into an alcohol solvent and regulating thepH (Potential of Hydrogen) of an alkaline solution to 8 to 9; after uniformly stirring, transferring a mixture into a reaction kettle and reacting; reacting at 60 to 150 DEG C for 6 to 12h; after reaction is finished, cooling a system to room temperature; filtering, washing and drying to obtain micron antimony trioxide; dissolving the micron antimony trioxide into ethylene glycol; adding distilled water, filtering and drying to obtain the nano antimony trioxide. An SEM (Scanning Electron Microscope) shows that the grain diameter of a product, i.e., Sb2O3 particles, is about 200 to 500nm and the product is nano-grade Sb2O3; nanoparticles have no agglomeration phenomenon and are uniformly dispersed. The preparation method takes the antimony trichloride as a raw material and the high-puritynano antimony trioxide is directly obtained through a solvothermal method; a preparation technology is simple, the cost is low and the efficiency is high, so that large-scale production is facilitated.

Description

technical field [0001] The invention relates to the preparation and application of nano antimony trioxide. It specifically relates to a method for preparing nano antimony trioxide by hydrothermal method using antimony trichloride as a raw material, an alcohol dissolution and desorption method and application as a lithium ion battery electrode material, which belongs to the field of nanometer material preparation and application. Background technique [0002] Antimony trioxide, antimony tetroxide, and antimony pentoxide are three compounds formed by antimony and oxygen that have industrial applications. Antimony and oxygen can form a series of oxides, including Sb 2 o 3 , Sb 2 o 4 , Sb 2 o 5 , Sb 6 o 13 , Sb 2 O and gaseous SbO, but only the first three are meaningful in industrial production, and most of the other oxides are transition products in different production processes of antimony. [0003] Antimony trioxide (Sb 2 o 3 , Mr291.50) is a dual-type substance,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00B82Y40/00
CPCB82Y40/00C01G30/005C01P2002/72C01P2004/03C01P2004/62
Inventor 周小中王武强张正锋
Owner NORTHWEST NORMAL UNIVERSITY
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