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Deironing method for vanadium-bearing stone coal lixivium

A technology of leachate and vanadium stone, which is applied in the field of vanadium-containing stone coal extraction, can solve the problems of high iron content in leachate, waste of resources, waste of iron resources, etc., and achieve the effects of low iron content, reduced impact, and low vanadium loss rate

Active Publication Date: 2016-06-22
WUHAN UNIV OF SCI & TECH
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AI Technical Summary

Problems solved by technology

[0002] At present, vanadium-containing stone coal is usually leached with sulfuric acid and leaching aids to obtain a vanadium-containing leach solution. During the leaching process, a large amount of iron enters the leach solution with vanadium, which reduces the ability of subsequent extraction or ion exchange processes to enrich vanadium, and at the same time increases the consumption of subsequent reagents. amount; the waste liquid after the leaching liquid is enriched with vanadium by extraction or ion exchange process is usually used to prepare the acid solution required for leaching, and the valuable iron element in the waste liquid is not recycled, resulting in a waste of iron resources
[0003] Zhao Jie et al. (Zhao Jie, Zhang Yimin, Huang Jing, Liu Tao, Wang Fei, Liu Juan. Thermodynamic analysis of acid leaching process for roasted stone coal samples[J]. Nonferrous Metals (Smelting Section), 2013, (10): 27- 31.) The stone coal raw ore is crushed to less than 3mm, roasted at 700°C for 1 hour, and then ground to a particle size of less than 0.074mm, accounting for 80wt% of the roasted cooked sample. The roasted cooked sample has a sulfuric acid concentration of 4mol / L and a liquid-solid ratio 1.5︰1, 5wt% fluorine-containing leaching agent, and 98°C for 4 hours of stirring and leaching, the vanadium concentration in the obtained acid leaching solution is 1.01g / L and the iron concentration is 2.05g / L, and the iron concentration is the vanadium concentration 2.03 times of that, too high iron concentration will not only increase the consumption of chemicals in the subsequent process, but also affect the subsequent vanadium-enriched liquid and product purity
[0004] Li Changlin (Li Changlin. Refractory stone coal vanadium extraction process and related theoretical research [D]. Changsha: Central South University, 2010.) used two-stage countercurrent leaching, the total acid consumption during leaching was 55wt%, and the amount of calcium fluoride additive 1.9wt%, the temperature is 95°C, the liquid-solid ratio is 1:1, the leaching time of each stage is 4h, the leaching rate of vanadium can reach 83.27%, the concentration of vanadium in the leaching solution is 4~5g / L and the concentration of iron is 30g / L About L, the iron concentration is 6~7.5 times of the vanadium concentration, and the iron content in the leaching solution is too high, which increases the difficulty of subsequent processing
[0005] Huang Yunsheng et al. (Huang Yunsheng, Wu Haiying, Dai Zilin, Wei Qing, Li Guiying. Study on the separation of vanadium and iron in the acid leaching solution of a stone coal vanadium mine in Shaanxi [J]. Mining and Metallurgy Engineering, 2013, 33(4): 104-107.) The supernatant of the No. 1 dense pool that was leached by sulfuric acid in a certain place in Shaanxi and washed by 6-stage countercurrent thickening was separated from vanadium and iron by extraction, wherein the concentration of vanadium in the supernatant was 1.34g / L and the concentration of iron was 4.12g / L, the iron concentration is 3.1 times of the vanadium concentration, and the iron concentration in the supernatant is high, which affects the subsequent enrichment process of vanadium. At the same time, the test did not recover and utilize the iron element in the raffinate with an iron concentration of 2.19g / L , resulting in a waste of iron resources
[0006] "A Method for Recycling the Raffinate of Vanadium Extraction from Stone Coal" (CN102787238A) patent technology provides a method for recycling the raffinate. The iron concentration in the raffinate is greater than 2g / L and the iron element has not been recycled, resulting in waste of resources
[0007] To sum up, the leach solution obtained by sulfuric acid leaching for extracting vanadium from stone coal has the disadvantage of high content of iron ions, which increases the consumption of reagents in the subsequent process. Iron element has not been recycled, resulting in waste of iron resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for removing iron from vanadium-bearing coal leachate. The specific steps of the iron removal method are:

[0031] Step 1. First crush the vanadium-containing stone coal to a particle size of less than 3mm, roast it at 750~800℃ for 1~1.3h, cool to room temperature, and then grind to a particle size of less than 0.074mm accounting for 65~80wt% to obtain Vanadium stone coal calcine.

[0032] Step 2: Mix the vanadium-containing coal calcine with water according to a liquid-solid ratio of 0.8 to 1.3 L / kg to obtain a vanadium-containing coal slurry.

[0033] Step 3: Adding the leaching agent to the vanadium-containing coal slurry, stirring at 80-88°C for 2 to 4 hours, and separating the solid and liquid to obtain the vanadium-containing coal leaching solution and the leaching residue.

[0034] The leaching agent is a mixture of soluble acids, soluble oxalate-containing substances and fluoride salts, and the ratio of the amount of hydrogen ion substances in the leaching age...

Embodiment 2

[0040] A method for removing iron from vanadium-bearing coal leachate. The specific steps of the iron removal method are:

[0041] Step 1. The vanadium-containing stone coal is crushed to a particle size of less than 3mm, roasted at 780~860℃ for 1.2~1.6h, cooled to room temperature, and then ground to a particle size of less than 0.074mm accounting for 65~80wt% to obtain Vanadium stone coal calcine.

[0042] Step 2: Mix the vanadium-containing coal calcine with water according to a liquid-solid ratio of 1.1 to 1.6 L / kg to obtain vanadium-containing coal slurry.

[0043] Step 3: Adding the leaching agent to the vanadium-containing coal slurry, stirring at 85-95°C for 3 to 5 hours, and separating the solid and liquid to obtain the vanadium-containing coal leaching solution and the leaching residue.

[0044] The leaching agent is a mixture of soluble acids, soluble oxalate-containing substances and fluoride salts, and the ratio of the amount of hydrogen ion substances in the leaching ag...

Embodiment 3

[0053] A method for removing iron from vanadium-bearing coal leachate. The specific steps of the iron removal method are:

[0054] Step 1. First crush the vanadium-containing stone coal to a particle size of less than 3mm, roast it at 850~900℃ for 1.5~2h, cool to room temperature, and then grind to a particle size of less than 0.074mm accounting for 65~80wt% to obtain vanadium Stone coal calcine.

[0055] Step 2: Mix the vanadium-containing coal calcine with water according to the liquid-solid ratio of 1.5-2L / kg to obtain vanadium-containing coal slurry.

[0056] Step 3: Adding the leaching agent to the vanadium-containing coal slurry, stirring at 90-100°C for 4.5-6 hours, and separating the solid and liquid to obtain the vanadium-containing coal leaching solution and the leaching residue.

[0057] The leaching agent is a mixture of soluble acids, soluble oxalate-containing substances and fluoride salts, and the ratio of the amount of hydrogen ion substances in the leaching agent to ...

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Abstract

The invention relates to a deironing method for vanadium-bearing stone coal lixivium. According to the technical scheme, the deironing method comprises the steps that vanadium-bearing stone coal is firstly subjected to crushing, roasting and ore grinding to obtain vanadium-bearing stone coal roasted ore, the vanadium-bearing stone coal roasted ore and water are stirred to obtain vanadium-bearing stone coal ore pulp, then a leaching agent is added, heating and stirring are carried out, and solid-liquid separation is carried out to obtain the vanadium-bearing stone coal lixivium and leaching residues; reduced iron powder is added into the vanadium-bearing stone coal lixivium, and the adding amount of the reduced iron power is 2-4 times the stoichiometric number of the chemical reaction for reducing Fe3+ in the vanadium-bearing stone coal lixivium into Fe2+; heating and stirring are carried out, the pH value is adjusted to range from 1.5 to 5, heating and stirring are carried out, solid-liquid separation is carried out, and deironed lixivium and a filter cake are obtained; and the deironed lixivium is used for the vanadium enrichment technology, and a ferrous oxalate dehydrate byproduct is obtained after the filter cake is dried. Vanadium and iron in the vanadium-bearing stone coal lixivium can be effectively separated, the iron in the vanadium-bearing stone coal lixivium can be recycled, the vanadium loss rate in the deironing process is low, the iron content of the deironed lixivium is low, and the influence of the iron on the subsequent vanadium enrichment technology is reduced.

Description

technical field [0001] The invention belongs to the technical field of vanadium extraction from vanadium-containing stone coal. In particular, the invention relates to a method for removing iron from a vanadium-containing stone coal leaching solution. Background technique [0002] At present, vanadium-containing stone coal is usually leached with sulfuric acid and leaching aids to obtain a vanadium-containing leach solution. During the leaching process, a large amount of iron enters the leach solution with vanadium, which reduces the ability of subsequent extraction or ion exchange processes to enrich vanadium, and at the same time increases the consumption of subsequent reagents. amount; the waste liquid after the leach liquid is enriched with vanadium by extraction or ion exchange process is usually used to prepare the acid solution required for leaching, and the valuable iron element in the waste liquid is not recycled, resulting in a waste of iron resources. [0003] Zh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/04C22B34/22C22B3/16C22B3/08C22B3/10C22B3/44C07C51/41C07C55/07
CPCC07C51/412C07C55/07C22B3/04C22B3/08C22B3/10C22B3/165C22B3/44C22B34/22Y02P10/20
Inventor 张一敏胡鹏程刘涛黄晶陈铁军
Owner WUHAN UNIV OF SCI & TECH
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