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A system and method for preparing high-purity vanadium pentoxide powder by chlorination

A vanadium pentoxide and chlorination technology, applied in the chemical and metallurgical fields, can solve the problems of different names, inability to directly apply to the reactor, and reducing the recovery rate of vanadium precipitation.

Active Publication Date: 2019-03-29
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent has the following deficiencies: (1) Similar to the aforementioned research by Iowa State University in the United States, this patent actually only provides the principle process of chlorination and lacks specific operable solutions. For example, the chlorination method includes boiling Chlorination includes molten salt chlorination, and molten salt chlorination and boiling chlorination are completely different chlorination methods; for another example, it is proposed to use "rotary kiln, fluidized furnace, fluidized furnace, shaft furnace And multi-hearth furnace" and other reactors actually cover almost all the commonly used mainstream reactors in the field of metallurgical industry, but different reactors have very different requirements for raw materials. The shaft furnace can only handle "coarse" particles larger than 8mm. When using "fine particles", pelletizing and pre-sintering treatment are required, and boiling chlorination is generally suitable for processing fine particles, so for a specific vanadium raw material, it cannot be directly applied to rotary kilns, fluidized furnaces, fluidized fluidized furnaces, shaft furnaces and Reactors such as multi-hearth furnaces; besides, "fluidized furnace" and "fluidized fluidized furnace" are essentially the same, but they are called differently; it can be seen that because the operation methods and conditions of these reactors are very different, only the principle flow is given Can't implement in fact; (2) vanadium oxychloride is passed into ultrapure aqueous solution and hydrolyzed, because vanadium pentoxide is very easily dissolved in hydrochloric acid solution, the precipitation recovery rate of vanadium is too low; When HCl concentration is greater than 6.0mol / In the hydrochloric acid solution of L, when vanadium pentoxide is dissolved, reduction will occur to generate VOCl 2 , release chlorine gas simultaneously, and this will further reduce the precipitation recovery rate of vanadium; Precipitation and washing process will certainly produce a large amount of vanadium-containing hydrochloric acid solution, be difficult to realize comprehensive treatment effectively; (3) vanadium oxychloride is directly passed into ammoniacal solution Ammonium salt precipitation is carried out in the precipitation washing process, and there is also a large amount of ammonia nitrogen wastewater generated during the precipitation washing process, which is difficult to deal with and easily causes environmental pollution.

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  • A system and method for preparing high-purity vanadium pentoxide powder by chlorination

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Embodiment 1

[0076] combine figure 1 , the system for preparing high-purity vanadium pentoxide powder by the chlorination method used in this embodiment includes a feeding section 1, a chlorination section 2, a dedusting and rinsing section 3, a rectifying purification section 4, a catalytic oxidation section 5, a catalytic Oxidation product feeding section 6, calcination section 7, tail gas washing absorption tower 8, induced draft fan 9 and chimney 10;

[0077] Among them, the feeding section 1 includes an industrial-grade vanadium oxide silo 1-1, an industrial-grade vanadium oxide screw feeder 1-2, a carbon source silo 1-3, and a carbon source screw feeder 1-4;

[0078] The chlorination section 2 includes a chlorination bed feeder 2-1, a chlorination fluidized bed main body 2-2, a chlorination bed cyclone separator 2-3 and a chlorination residue discharger 2-4;

[0079] Dust removal and washing section 3 includes primary dust removal device 3-1, secondary dust removal device 3-2, prima...

Embodiment 2

[0093] This embodiment provides the method for preparing high-purity vanadium pentoxide powder using the system described in embodiment 1, comprising the following steps:

[0094] The industrial-grade vanadium oxide in the industrial-grade vanadium oxide silo 1-1 and the carbon source in the carbon source silo 1-3 pass through the industrial-grade vanadium oxide screw feeder 1-2 and the carbon source screw feeder 1-4 respectively. Enter the chlorination fluidized bed main body 2-2 after entering the chlorination bed feeder 2-1 mixing simultaneously; From the chlorine of the chlorine gas source main pipe and the nitrogen of the nitrogen gas source main pipe through the chlorination fluidized bed main body 2-2 bottom The air inlet enters the main body 2-2 of the chlorinated fluidized bed to maintain the fluidization of the vanadium oxide and the carbon source and react with it, and the chlorine gas and the carbon source work together to chlorinate the vanadium oxide and a small a...

Embodiment 3

[0101] In this example, powdered industrial-grade vanadium pentoxide (purity: 98.50%) is used as raw material, and the processing capacity is 80 kg / h. It is prepared by chlorination, dedusting and washing, rectification and purification of vanadium oxychloride, catalytic oxidation and calcination. Obtain high-purity vanadium pentoxide product.

[0102] In the main body 2-2 of the chlorination fluidized bed, the amount of petroleum coke added during the chlorination process is 30% of the mass of the industrial-grade vanadium pentoxide powder, the operating temperature of the chlorination is 600°C, and the operating gas velocity of the fluidization section is 3.00m / s, the mole fraction of chlorine in the chlorine-nitrogen mixed gas entering the air chamber is 20%; in the main body 5-4 of the catalytic oxidation fluidized bed, the water vapor fed into the catalytic oxidation process is 30% of the quality of vanadyl trichloride, and the catalytic oxidation operation The temperatu...

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Abstract

The invention belongs to the field of chemical industry and metallurgy, and provides a system and a method for preparing high-purity vanadium pentoxide powder through a chlorination method. Accordingto the method, an industrial grade vanadium oxide is converted into vanadium oxytrichloride by using fluidization chlorination; two-stage dust removing and four-stage leaching are performed to obtaincrude vanadium oxytrichloride; and the crude vanadium oxytrichloride is subjected to two-stage rectification, catalytic oxidation and calcination treatment to obtain the high-purity vanadium pentoxidepowder. According to the present invention, the too high furnace temperature can be prevented by spraying the vanadium oxytrichloride mud into the chlorination fluidized bed; by arranging the horizontal porous inner member in the catalytic oxidation fluidized bed, the generation of large gas bubbles can be inhibited, and the reaction efficiency can be improved; and the system and the method haveadvantages of strong raw material adaptability, no pollution wastewater emission, low production energy consumption, low operation cost, stable product quality and the like, are suitable for the large-scale industrial production of high-purity vanadium pentoxide powder with more than 4N, and have good economic and social benefits.

Description

technical field [0001] The invention belongs to the fields of chemical industry and metallurgy, and particularly relates to a system and method for preparing high-purity vanadium pentoxide powder by a chlorination method. Background technique [0002] Vanadium pentoxide is one of the important industrial vanadium products, widely used in the production of alloy additives such as ferrovanadium and vanadium nitride, as well as catalysts, colorants and cemented carbide additives. With the continuous development of new energy technologies, the demand for high-purity vanadium pentoxide (purity above 3N5) is increasingly strong in the battery industry, including all-vanadium redox flow batteries (VRB) with good large-scale energy storage performance and vanadium for electric vehicles Acid-based lithium-ion batteries, etc. However, the existing industrial technology can usually only prepare vanadium pentoxide with a purity of 2N5 (that is, the product specified in HGT3485-2003), w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02
CPCY02P20/129
Inventor 范川林朱庆山杨海涛
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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