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A method for hydrothermal oxalic acid complex leaching of vanadium in vanadium-iron-spinel vanadium-containing minerals

A spinel, ferrous oxalate technology, applied in the direction of improving the process efficiency, can solve the problems of difficult leaching tailings treatment, fluoride pollution to the environment, inability to discharge at will, etc., to speed up the leaching reaction rate, simplify the process steps, Leachate cleaning effect

Active Publication Date: 2020-05-19
UNIV OF SCI & TECH BEIJING
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Problems solved by technology

Chinese patent CN105624435A uses fluoride and oxalic acid as leaching agents to selectively leach vanadium in stone coal, but the leaching rate is low, and fluoride pollutes the environment and is harmful to humans
Xu Mengchun and others conducted experimental research on the leaching behavior of vanadium extraction tailings (Xu Mengchun. Experimental research on the leaching behavior of vanadium extraction tailings [D]. Northeastern University, 2012.), under pressure conditions, to control the amount of oxalic acid added To avoid excessive dissolution of iron, the vanadium-containing phase in the vanadium extraction tailings is mainly vanadium-iron spinel, which inhibits the dissolution of iron and will inevitably prevent the leaching of vanadium, so the leaching rate is low, up to about 66%.
Moreover, there are still a large amount of unleached vanadium and chromium elements in the leaching residue, which cannot be discharged at will, and the leaching tailings are difficult to treat

Method used

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  • A method for hydrothermal oxalic acid complex leaching of vanadium in vanadium-iron-spinel vanadium-containing minerals
  • A method for hydrothermal oxalic acid complex leaching of vanadium in vanadium-iron-spinel vanadium-containing minerals
  • A method for hydrothermal oxalic acid complex leaching of vanadium in vanadium-iron-spinel vanadium-containing minerals

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Experimental program
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Effect test

Embodiment 1

[0026] Using vanadium trioxide and ferric oxide as initial raw materials, they were calcined at 1200°C for 48 hours in a reducing atmosphere to obtain pure Fe 2 VO 4 . will obtain pure Fe 2 VO 4 Grind the particle size to less than 0.074mm, weigh 0.2g of ball-milled vanadium iron spinel and 0.6g of reduced iron powder, mix them together and put them into the reactor, add 20ml of 30% oxalic acid solution in the reactor Inside, a mixed slurry is formed, and the leaching reaction is carried out under the conditions of a reaction temperature of 135° C., a time of 120 minutes, and a stirring speed of 500 rpm. After the reaction is completed, solid-liquid separation is carried out to obtain a vanadium-containing leachate and a filter cake, and the filter cake is washed. Obtain ferrous oxalate by-product and leaching residue according to elutriation method. Finally, the concentration of vanadium in the leaching solution was measured by ICP-AES to be 2.2g / L, and the concentration ...

Embodiment 2

[0028] According to the methods of Chinese patents CN106011456A and CN107641723A, stone coal is used as the initial raw material, ferric oxide is used as an additive, and the temperature is 1200 ° C under a reducing atmosphere. Roasting, after magnetic separation, a vanadium-iron-spinel-type vanadium-containing concentrate is obtained . Ball mill the obtained vanadium-iron-spinel-type vanadium-containing concentrate to a particle size below 0.074mm, weigh 0.2g of ball-milled vanadium concentrate, and 0.6g of reduced iron powder, mix them together, put them into the reaction kettle, add Put 20ml of oxalic acid solution with a mass fraction of 30% in a reaction kettle to form a mixed slurry. Under the conditions of a reaction temperature of 135°C, a time of 120min, and a stirring speed of 500rpm, a leaching reaction is carried out. After the reaction is completed, solid-liquid separation is carried out to obtain vanadium-containing Leachate and filter cake, the filter cake is wa...

Embodiment 3

[0030]Using vanadium slag as the initial raw material, the vanadium slag is ball-milled to a particle size below 0.074mm. Weigh 0.2g of ball-milled vanadium slag and 0.6g of reduced iron powder, mix them together and put them into the reactor, add 20ml of oxalic acid solution with a mass fraction of 30% in the reactor to form a mixed slurry. Under the conditions of 135°C, 120min, and stirring speed of 500rpm, the leaching reaction was carried out. After the reaction, the solid-liquid separation was carried out to obtain the vanadium-containing leachate and filter cake. The filter cake was washed, and the by-products of ferrous oxalate and Leach residue. Finally, the concentration of vanadium in the leach solution was measured to be 497mg / L by ICP-AES, and the leaching rate was 89%, and the concentration of iron in the leach solution was measured to be 75mg / L.

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Abstract

The invention provides a method for leaching vanadium in ferrovanadium spinel vanadium-containing minerals through complexing of hydrothermal oxalic acid, and belongs to the field of leaching of vanadium in ferrovanadium spinel vanadium-containing minerals through a hydrothermal method. According to the method, the ferrovanadium spinel vanadium-containing minerals are used as raw materials, ferrumpowder is used as a reducing agent, an oxalic acid solution is used as a leaching agent, and the ferrovanadium spinel vanadium-containing minerals, the ferrum powder and the oxalic acid are mixed into slurry to react under a hydrothermal condition; and solid-liquid separation is conducted on the slurry obtained after the reaction, so that clean vanadium-containing leachate and a ferrous oxalate by-product are obtained. According to the method, oxalate ions with a the strong complexing effect react with vanadium and ferrum in ferrovanadium spinel to form [V(C2O4)3]<3-> and [Fe(C2O3]<3-> to enter the solution; and the formed [Fe(C2O3]<3-> reacts with the Fe powder to form ferrous oxalate sediment, so that proceeding of the reaction is facilitated, and the leaching reaction rate is increased. By adoption of the method, vanadium in the ferrovanadium spinel vanadium-containing minerals can be effectively extracted, vanadium and ferrum are separated in the leaching process, the process steps are simplified, and the by-product, namely the ferrous oxalate, with high added value is obtained.

Description

technical field [0001] The invention belongs to the field of leaching vanadium in vanadium-iron-spinel type vanadium-containing minerals by hydrothermal method. It specifically relates to a method for obtaining vanadium-containing leaching solution and ferrous oxalate by-products by using strong complexation of oxalate ions and high-pressure reduction conditions to accelerate the leaching reaction rate. Background technique [0002] Vanadium is an important metal element, which is widely used in machinery, aviation, electronic technology, defense industry and other industries, so it is called the metal "vitamin". my country's vanadium resources are mainly vanadium-titanium magnetite and vanadium-containing stone coal, and these two different vanadium-containing resources can be transformed into vanadium-containing minerals with vanadium-iron spinel phase through metallurgical means. [0003] At present, the pressurized hydrometallurgical process has the characteristics of s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/16C22B34/22
CPCC22B3/165C22B34/22Y02P10/20
Inventor 闫柏军陈学鑫董自慧
Owner UNIV OF SCI & TECH BEIJING
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