Method for preparing vanadic oxide from vanadium-containing raw materials through ball milling calcification and ammonification

A vanadium pentoxide and ball milling technology, which is applied in the field of vanadium chemical metallurgy, can solve the problems of high energy consumption, easy volatilization of acid liquid or ammonia gas, and long process flow, so as to reduce the water consumption of calcification, easy operation, and process flow The effect of simple equipment

Active Publication Date: 2018-07-10
HEBEI IRON AND STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] As can be seen from the above, there are many problems such as too long technical process, high energy consumption in the method for preparing high-purity vanadium pentoxide at present, and the use of acid solution or ammonia in the leaching process is volatile, so it is necessary to develop a new method for preparing high-purity vanadium pentoxide A method of pure vanadium pentoxide to overcome the above-mentioned problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Mix quicklime and water according to the liquid-solid ratio of 3:1 and then add them to the ball mill, add sodium vanadate solid according to the molar ratio of calcium to vanadium of 1.6, control the ball milling speed to 100r / min, and the ball milling time to 20min, quicklime The mass ratio of the total mass of the vanadium-containing raw material and the ball milling medium is 1:5, and the heat generated by lime digestion and ball milling activation are used to promote the calcification reaction, and the reaction is filtered after the completion of the reaction, and the obtained calcium vanadate is washed;

[0046] (2) according to the ammonium vanadium molar ratio is 1.2:1 the calcium vanadate that step (1) obtains and ammonium carbonate are mixed, at normal temperature, the mixture is joined in the ball mill and ball milling carries out ammonization reaction, and the control ball milling speed is 80r / min, the ball milling time is 30min, and the mass ratio of th...

Embodiment 2

[0051] (1) Quicklime and water are mixed according to the liquid-solid ratio of 5:1 and then added to the ball mill, and the ammonium polyvanadate solid is added according to the molar ratio of calcium to vanadium as 1.8, and the ball milling speed is controlled to be 150r / min, and the ball milling time is 40min. The mass ratio of the total mass of quicklime and vanadium-containing raw materials to the ball milling medium is 1:8, and the heat generated by lime digestion and ball milling activation are used to promote the calcification reaction. After the reaction is completed, filter and wash the obtained calcium vanadate;

[0052] (2) Mix the calcium vanadate obtained in step (1) with ammonium bicarbonate according to the ammonium vanadium molar ratio of 1.4:1, at normal temperature, join the mixture into the ball mill and carry out the ammonification reaction by ball milling, and the ball milling speed is controlled to be 100r / min, the ball milling time is 40min, and the mas...

Embodiment 3

[0057] (1) Mix quicklime and water according to the liquid-solid ratio of 6:1 and add them to the ball mill, add sodium vanadate solid according to the molar ratio of calcium to vanadium of 1.3, control the ball milling speed to 200r / min, and the ball milling time to 30min, quicklime The mass ratio of the total mass of the vanadium-containing raw material and the ball milling medium is 1:10, and the heat generated by lime digestion and ball milling activation are used to promote the calcification reaction. After the reaction is completed, filter and wash the obtained calcium vanadate;

[0058] (2) According to the ammonium vanadium molar ratio is 1.2:1 the calcium vanadate that step (1) obtains and ammonium carbonate are mixed, at normal temperature, the mixture is joined in the ball mill and ball milling carries out ammonization reaction, and the ball milling speed of control is 150r / min, the ball milling time is 60min, and the mass ratio of the feeding amount (calcium vanada...

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PUM

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Abstract

The invention relates to a method for preparing vanadic oxide from vanadium-containing raw materials through ball milling calcification and ammonification. The method comprises the following steps ofmixing quicklime, water and vanadium-containing raw materials; then, performing ball milling and calcification reaction; after the calcification is completed, performing solid-liquid separation to obtain calcium vanadate; at the normal temperature, mixing the obtained calcium vanadate with ammonium salt; then, performing ball milling; performing ammonification reaction; after the reaction is completed, performing solid-liquid separation; obtaining ammonium metavanadate-containing solution and calcium carbonate; performing impurity removal on the ammonium metavanadate-containing solution; performing cooling and crystallization on the solution subjected to impurity removal; performing solid-liquid separation to obtain ammonium metavanadate crystals; performing roasting; obtaining vanadic oxide. The low-liquid-solid-ratio quicklime and water are used; mixing, ball milling and activation are combined for performing calcification reaction; the calcification water consumption is reduced; thecalcification rate reaches 97 percent or higher; meanwhile, the ball milling ammonification reaction is performed at the normal temperature, so that the ammonia gas volatilization in the ammonification process is inhibited; the ammonification rate reaches 98 percent or higher. The technical flow process is shortened; the operation is convenient; the equipment is simple; good application prospectsare realized.

Description

technical field [0001] The invention relates to the technical field of vanadium chemical metallurgy, in particular to a method for preparing vanadium pentoxide by ball milling calcification-ammonization of vanadium-containing raw materials. Background technique [0002] With the advancement of science and technology, the application fields of vanadium continue to expand, and some high-tech fields have put forward higher requirements for the grade of vanadium raw materials, especially vanadium oxide. At present, high-end products in the vanadium application field include aerospace-grade vanadium-aluminum alloys, electrolytes for all-vanadium redox flow batteries, nano-scale vanadium functional materials, vanadium catalysts, vanadium luminescent materials, etc. For example, in the field of aerospace, vanadium-aluminum alloys are mainly used to produce jet engines, high-speed aircraft frames and rocket engine casings, and the requirements for specific elements of the raw materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2006/80
Inventor 王新东李兰杰白瑞国常金宝祁健赵备备赵亮
Owner HEBEI IRON AND STEEL
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