Method for recovering vanadium and iron from acid liquor containing tetravalent vanadium and ferrous iron

A technology of divalent iron and tetravalent vanadium, applied in the field of wet vanadium extraction, which can solve the problems of iron resources not being recycled, large amount of washing water, and reduction of resin adsorption, and achieve simple, efficient, deep purification, and simple operation cost Low, high resource recovery rate effect

Active Publication Date: 2021-04-09
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
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AI Technical Summary

Problems solved by technology

The methods for enriching vanadium mainly include extraction method and ion exchange method, such as CN101289703A, CN106282538A and CN101580902A public extraction methods enrich vanadium usually use P204 extractant, P204 is easier to extract ferric and tetravalent vanadium, so it is necessary to extract Pentavalent vanadium is reduced to tetravalent, and ferric iron is reduced to bivalent. The problem is that the stripping liquid needs to consume oxidant to oxidize tetravalent vanadium to pentavalent vanadium. The extraction agent is easy to emulsify, and the raffinate is difficult to treat organic wastewater.
[0004] CN109706329A, CN104841682A, CN108559843A and CN108754191A disclose that the ion exchange method usually adopts a weakly basic anion exchange resin to absorb pentavalent vanadium anions under the condition of pH=2-3, and long-term operation will produce aluminum and iron hydroxide precipitation to block the resin , to reduce the adsorption capacity of the resin, and at the same time, the ion exchange method also has problems such as a large amount of washing water
[0005] Regardless of whether extraction or ion exchange is used to enrich vanadium in the acid leach solution, the iron in the raffinate and effluent is usually neutralized by adding calcium and enters the slag phase, resulting in no recycling of iron resources in stone coal.
Moreover, there are cationic impurities such as iron, aluminum, magnesium, potassium, and calcium in the extraction and stripping vanadium enrichment solution, and anion impurities such as silicon, phosphorus, arsenic, molybdenum, chromium, and uranium in the ion exchange desorption vanadium enrichment solution, and the types of impurities increase. Reduce the difficulty of impurity removal and reduce the purity of vanadium products

Method used

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  • Method for recovering vanadium and iron from acid liquor containing tetravalent vanadium and ferrous iron
  • Method for recovering vanadium and iron from acid liquor containing tetravalent vanadium and ferrous iron
  • Method for recovering vanadium and iron from acid liquor containing tetravalent vanadium and ferrous iron

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Embodiment 1

[0075] Present embodiment provides a kind of method that reclaims vanadium and iron from pickling solution, as figure 1 Shown, main element concentration is V1.68g / L in described stone coal pickling solution, Fe 8.96g / L, Al 12.39g / L, described method comprises the steps:

[0076] (1) Control the temperature of the stone coal acid leaching solution to 90°C, add sodium hydroxide to adjust the pH of the acid leaching solution to 2.5, then add iron oxyhydroxide crystal seeds, and the solid-liquid ratio of iron oxyhydroxide crystal seeds to the acid leaching solution kg / m 3 It is 2:1, stirring (stirring speed is 60r / min, and stirring time is 30min) to obtain pretreatment liquid after seed crystal is evenly distributed, and main element concentration is V1.65g / L in the pretreatment liquid, Fe 8.97g / L, Al 12.43g / L;

[0077] (2) add oxygenant sodium perchlorate to step (1) pretreatment liquid and carry out oxidation treatment, the oxygenant consumption is ferrous iron and tetravalent...

Embodiment 2

[0085] This embodiment provides a method for reclaiming vanadium and iron from the acid leaching solution. The concentration of main elements in the acid leaching solution for stone coal is V 1.68g / L, Fe 8.96g / L, and Al 12.39g / L. Said method comprises the steps:

[0086] (1) Control the temperature of the stone coal acid leaching solution at 95°C, add sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonium carbonate, ammonium bicarbonate, magnesium carbonate, aluminum carbonate, ferrous carbonate, iron carbonate and carbonic acid Calcium adjusts the pH of the acid leaching solution to be 2. After solid-liquid separation, the filtrate is added with iron oxyhydroxide crystal seeds, and the solid-liquid ratio of iron oxyhydroxide crystal seeds to the acid leaching solution is kg / m 3 1.8:1, stirring (stirring speed is 50r / min, and stirring time is 60min) to obtain pretreatment liquid after seed crystal even distribution, main element concentratio...

Embodiment 3

[0095] This embodiment provides a method for reclaiming vanadium and iron from the acid leaching solution. The concentration of main elements in the acid leaching solution for stone coal is V 1.68g / L, Fe 8.96g / L, and Al 12.39g / L. Said method comprises the steps:

[0096] (1) Control the temperature of the stone coal acid leaching solution at 35°C, add sodium hydroxide, potassium hydroxide, ammonia water, magnesium hydroxide, calcium hydroxide, ferrous hydroxide, ferric hydroxide and aluminum hydroxide to adjust the temperature of the acid leaching solution The pH is 1.7, after solid-liquid separation, the filtrate is added with ferric oxyhydroxide seeds, and the liquid-solid ratio of ferric oxyhydroxide seeds to the pickling solution is kg / m 3 is 0.08:1, stirring (stirring speed is 300r / min, and stirring time is 10min) to obtain pretreatment liquid after seed crystal is evenly distributed, and main element concentration is V1.63g / L in the pretreatment liquid, Fe 24.82g / L, Al ...

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Abstract

The invention relates to a method for recovering vanadium and iron from acid liquor containing tetravalent vanadium and ferrous iron, which comprises the following steps: (1) adding an iron oxyhydroxide seed crystal into the acid liquor containing tetravalent vanadium and ferrous iron, and stirring to obtain a pretreatment solution; (2) carrying out oxidation treatment on the obtained pretreatment solution, and carrying out solid-liquid separation to obtain a ferrovanadium enriched material and a filtrate; (3) mixing the obtained ferrovanadium enriched material with alkali liquor, carrying out conversion treatment, then carrying out water leaching, and carrying out solid-liquid separation to obtain iron oxyhydroxide and a vanadium-containing solution; and (4) sequentially carrying out purification treatment and vanadium precipitation on the obtained vanadium-containing solution, and carrying out solid-liquid separation to obtain ammonium metavanadate. The method realizes enrichment, dissociation and productization of ferrovanadium in the acid liquor, simply and efficiently realizes deep purification of the vanadium-containing solution, synchronously recovers aluminum resources, has the advantages of high resource recovery rate, high product purity, simple operation, low cost and no emission of three wastes, and has a wide application prospect.

Description

technical field [0001] The invention relates to the field of vanadium extraction by wet method, in particular to a method for recovering vanadium and iron from an acid solution containing tetravalent vanadium and ferrous iron. Background technique [0002] Stone coal is a vanadium-containing polymetallic mineral resource and one of the main raw materials for extracting vanadium. In addition to vanadium, stone coal often contains aluminum, potassium, iron, calcium, magnesium, molybdenum, nickel, cobalt, copper, and titanium. , chromium, uranium, silver selenium and other associated elements. At present, the methods for extracting vanadium from stone coal mainly include two categories: roasting method and acid leaching method. Due to the instability of the roasting process, the process of vanadium extraction by roasting is seriously polluted and the recovery rate of vanadium is low. At present, the acid leaching process is mostly used in production, including direct acid lea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/44C22B34/22C01G49/02
CPCC22B3/44C22B34/22C01G49/02Y02P10/20
Inventor 董玉明刘宏辉米界非杨建旺张笛裴丽丽徐红彬
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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