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Method for crystallizing and separating large-particle ammonium metavanadate from vanadium-containing solution

A technology for ammonium metavanadate and crystallization separation, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of non-scaling ammonium metavanadate, affecting the heat transfer effect of heat exchangers, and slow cooling rate , achieve the effects of shortening the crystallization time, good application prospects, and increasing the cooling rate

Active Publication Date: 2019-09-27
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] For this leaching system, CN104294047A proposes a kind of crystallization method of ammonium metavanadate in the ammonium leaching solution, and this method utilizes the mode of cooling crystallization to obtain ammonium metavanadate from the solution containing ammonium metavanadate, but its cooling process and The cooling method is not specified
In the industrial production process, if the method of natural cooling is adopted, the cooling rate is very slow, the cooling time is very long, and the crystallization efficiency is low
If a heat exchanger is used for cooling, due to the supersaturation at the heat exchange interface, the ammonium metavanadate fine crystals are easy to accumulate on the heat exchange surface, resulting in fouling of the heat exchanger, which seriously affects the heat exchange effect of the heat exchanger , if not treated in time, it is easy to completely block the heat exchanger, resulting in interruption of operation
Moreover, this method does not control the morphology of ammonium metavanadate crystals, and cannot obtain ammonium metavanadate crystals with large particles and complete crystal morphology.
However, an efficient, non-fouling, crystal morphology-controllable crystallization method for ammonium metavanadate has not been found yet.

Method used

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  • Method for crystallizing and separating large-particle ammonium metavanadate from vanadium-containing solution

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Experimental program
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Effect test

Embodiment 1

[0029] Such as figure 1 Shown, the technical process that the present invention crystallizes and separates large particle ammonium metavanadate from vanadium-containing solution can be:

[0030] (1) The vanadium-containing raw material roasting clinker is mixed with ammonium bicarbonate solution for ammonization reaction, the liquid-solid ratio is 0.2:1 (mass ratio), the concentration of ammonium bicarbonate is 50wt%, and the ammonization reaction temperature is 40°C. After melting, crystal slag mixed slurry is obtained;

[0031] (2) Mix the hot liquid with the crystalline slag mixture obtained in step (1), the liquid-solid ratio of the hot liquid and the crystalline slag mixture is 3:1 (mass ratio), heat it to 70°C for 30 minutes under stirring conditions, and make it react with All the ammonium metavanadate mixed with the slag phase was dissolved in water, and filtered at 70°C to obtain tailings and pre-crystallization liquid. The concentration of ammonium metavanadate in t...

Embodiment 2

[0035] Transfer the 85°C vanadium-containing solution (the concentration of ammonium metavanadate is 30g / L) obtained after ammonium leaching of vanadium-containing clinker into a vacuum crystallizer for cooling and crystallization, and adjust the vacuum to 0.066MPa; when the temperature reaches 60 When the temperature reaches 58°C, add 0.75% ammonium metavanadate mass seed crystals, and a small amount of crystals are precipitated instantly; when the temperature reaches 50°C, adjust the vacuum degree to 0.11MPa; when the temperature reaches 39°C When the crystallization is completed, the ammonium metavanadate crystal and the crystallization mother liquor are obtained by filtering after the crystallization is completed.

[0036] The total time for cooling from 85°C to 39°C is 30 minutes, the average particle size of the crystals is 300 μm, and no scaling phenomenon was found on the inner wall of the crystallizer during the crystallization process.

Embodiment 3

[0038] Transfer the 90°C vanadium-containing purification solution with a concentration of 40g / L of ammonium metavanadate into a vacuum crystallizer for cooling and crystallization, and adjust the vacuum degree to 0.06MPa; when the temperature reaches 60°C, add 1% ammonium metavanadate by mass When the temperature reaches 50°C, the vacuum degree is adjusted to 0.15MPa; when the temperature is 35°C, the crystallization is completed, and after the crystallization is completed, filter to obtain ammonium metavanadate crystals and crystallization mother liquor.

[0039] The total time for cooling from 90°C to 35°C is 33 minutes, the average particle size of the crystals is 400 μm, and no scaling phenomenon was found on the inner wall of the crystallizer during the crystallization process.

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Abstract

The invention relates to a method for crystallizing and separating large-particle ammonium metavanadate from a vanadium-containing solution. The method is characterized in that vacuum-cooling crystallization of the vanadium-containing solution is carried out in three stages to obtain metavanadic acid crystals; in the first stage, the vacuum crystallization temperature is 60-95 DEG C, and the vacuum degree is 0.06-0.07 MPa; in the second stage, the vacuum crystallization temperature is 50-60 DEG C, and the vacuum degree is 0.07-0.08 MPa; and in the third stage, the vacuum crystallization temperature is 30-50 DEG C, and the vacuum degree is 0.08-0.15 MPa. The staged vacuum cooling crystallization method is adopted to obtain large-particle ammonium metavanadate crystals having a uniform particle size and a size of 200 [mu]m or more, and has the advantages of significant increase of the cooling rate, shortening of the crystallization time, no fouling phenomenon in the crystallization process, and good application prospect.

Description

technical field [0001] The invention belongs to the technical field of vanadium chemical industry and metallurgy, and relates to a method for crystallizing ammonium metavanadate, in particular to a method for crystallizing and separating large-grain ammonium metavanadate from a vanadium-containing solution. . Background technique [0002] Vanadium slag is a general term for the vanadium-containing slag obtained by oxidative blowing of vanadium-containing molten iron or vanadium-containing iron concentrate by wet vanadium extraction, and is an important raw material for vanadium extraction. The traditional method for extracting vanadium from vanadium slag is sodium roasting of vanadium slag-water leaching to extract vanadium. This method is to add sodium salt (such as salt, Glauber’s salt, soda ash, etc.) Oxidized to soluble sodium vanadate, sodium vanadate into the solution after water immersion. The recovery rate of vanadium in the sodium roasting process is low, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/006C01P2004/60
Inventor 王少娜杜浩刘彪王欣然李昊男
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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