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Method for preparing antimony by in-situ reduction of antimonous oxide with eutectic solvent

The technology of antimony trioxide and deep eutectic solvent is applied in the field of non-ferrous metal metallurgy, which can solve the problems of high production temperature, long time and complicated equipment, and achieve the effects of low electrolytic reduction temperature, short time and lower production cost.

Inactive Publication Date: 2015-12-09
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

The invention aims to solve the problems of high production temperature, long time, long process, complex equipment, polluted environment and single product form in the existing metal antimony production method, and provides an in-situ deep eutectic solvent that adopts green economy and environmental protection. The method for reducing antimony trioxide to produce metal antimony, the present invention is realized through the following technical solutions

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  • Method for preparing antimony by in-situ reduction of antimonous oxide with eutectic solvent

Examples

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Effect test

Embodiment 1

[0015] The method for preparing antimony by in-situ reduction of antimony trioxide in the deep eutectic solvent, the specific steps are as follows:

[0016] (1) Under an inert atmosphere, mix the quaternary ammonium salt and the polyol according to the molar ratio of 1:2, and mix them uniformly at a temperature of 90°C (constant temperature oil bath) to prepare a deep eutectic solvent; the quaternary ammonium salt is chlorine choline, polyhydric alcohol is ethylene glycol;

[0017] (2) Use the graphite crucible as the cathode and the electrolytic cell, place 0.5g of antimony trioxide powder at the bottom of the graphite crucible, use the 20ml deep eutectic solvent obtained in step (1) as the electrolyte, and insert the graphite into the electrolyte However, it cannot touch the antimony trioxide powder at the bottom. It is electrolyzed for 3 hours at an electrolysis temperature of 80°C and a cell voltage of 3V. Finally, the bottom powder of the cathode graphite crucible is take...

Embodiment 2

[0019] The method for preparing antimony by in-situ reduction of antimony trioxide in the deep eutectic solvent, the specific steps are as follows:

[0020] (1) Under an inert atmosphere, mix the quaternary ammonium salt and the polyol according to the molar ratio of 1:3, and mix them uniformly at a temperature of 70°C (constant temperature oil bath) to prepare a deep eutectic solvent; the quaternary ammonium salt is chlorine choline, polyhydric alcohol is propylene glycol;

[0021] (2) Use the graphite crucible as the cathode and the electrolytic cell, place 0.5g of antimony trioxide powder at the bottom of the graphite crucible, use the 20ml deep eutectic solvent obtained in step (1) as the electrolyte, and insert the graphite into the electrolyte However, it cannot touch the antimony trioxide powder at the bottom. It is electrolyzed for 6 hours at an electrolysis temperature of 90°C and a cell voltage of 3.2V. Finally, the bottom powder of the cathode graphite crucible is t...

Embodiment 3

[0023] The method for preparing antimony by in-situ reduction of antimony trioxide in the deep eutectic solvent, the specific steps are as follows:

[0024] (1) Under an inert atmosphere, mix quaternary ammonium salts and polyols at a molar ratio of 2:3, and mix them uniformly at a temperature of 73°C (constant temperature oil bath) to prepare a deep eutectic solvent; the quaternary ammonium salts are tetra Methyl ammonium chloride, polyhydric alcohol is propylene glycol;

[0025] (2) Use the graphite crucible as the cathode and the electrolytic cell, place 0.5g of antimony trioxide powder at the bottom of the graphite crucible, use the 20ml deep eutectic solvent obtained in step (1) as the electrolyte, and insert the graphite into the electrolyte However, the antimony trioxide powder that cannot touch the bottom is electrolyzed for 5.5 hours at an electrolysis temperature of 70°C and a cell voltage of 2.8V. Finally, the powder at the bottom of the cathode graphite crucible is...

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Abstract

The invention relates to a method for preparing antimony by in-situ reduction of antimonous oxide with an eutectic solvent and belongs to the technical field of nonferrous metallurgy. The method comprises the steps of uniformly mixing quaternary ammonium salt and polyhydric alcohol to form the eutectic solvent in an inert atmosphere, putting antimonous oxide powder at the bottom in a graphite crucible as a cathode and an electrolyzer to form an electrolyte of the eutectic solvent, inserting graphite or an inert anode into the electrolyte without contact with the antimonous oxide powder at the bottom, carrying out electrolysis for 3-6h at electrolysis temperature of 25-100 DEG C and electrolyzer voltage of 2.2-3.5V, finally taking out the powder at the bottom of the cathode graphite crucible, and flushing and drying to form the metallic antimony. The method aims at solving the problems of high production temperature, long time and flow, complicated equipment, environment pollution, a single product form and the like existing in the existing metallic antimony production method, and the green, economic and environmentally-friendly method for preparing the metallic antimony by the in-situ reduction of antimonous oxide with the eutectic solvent is provided.

Description

technical field [0001] The invention relates to a method for preparing antimony by reducing antimony trioxide in situ with a deep eutectic solvent, and belongs to the technical field of nonferrous metallurgy. Background technique [0002] Metal antimony is different from general non-ferrous metals. It is brittle, brittle and non-ductile. It is precisely because of this characteristic of antimony that antimony is added to other metals to form alloys, which can improve the hardness and wear resistance of the alloy and improve the casting fluidity. Improved, improved mechanical properties, etc. Therefore, antimony and antimony alloys are widely used in bearings, solder, enamel, ammunition, battery grid materials and other fields. The production of antimony usually adopts pyrometallurgy, mainly volatilization roasting-reduction smelting method. This process first uses the characteristics of antimony sulfide ore to be easily oxidized and volatilized to roast to obtain enriched a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B30/02
Inventor 徐存英王蒙蒙华一新张启波李坚李艳
Owner KUNMING UNIV OF SCI & TECH
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