Impurity removing method for vanadium contained leaching agent

A leachate and solid-liquid separation technology, applied in the direction of improving process efficiency, can solve the problems of large reagent consumption, long process flow, large reagent consumption, etc., achieve resource utilization of vanadium loss rate, good separation effect, reagent The effect of low consumption

Active Publication Date: 2016-12-21
WUHAN UNIV OF SCI & TECH
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Problems solved by technology

[0004] Lv Jixia et al. (Lv Jixia, Zhang Yimin, Liu Tao, Huang Jing. Experimental research on impurity removal of water leaching slag acid leaching solution for extracting vanadium from stone coal [J]. Metal Mine, 2008, (4): 149-151.) on water leaching slag acid The acid dipping solution obtained by leaching is under the condition that the ratio of the amount of vanadium in hydrogen peroxide to the acid dipping solution is 15, the volume ratio of the pickling solution and the copper-iron reagent (1g / L) is 8, and the impurity precipitation pH value is 6.5. Purification and removal of impurities, the removal of harmful impurities is relatively thorough, and the impurities aluminum, iron ions and vanadium are well separated, but the loss rate of vanadium in the process of removing impurities is as high as 15.52%. At the same time, the process is long and the consumption of reagents is large
[0005] "A method for extracting vanadium from stone coal acid leaching solution" (CN103789560A) patent technology, adopts two-step solvent extraction method to remove iron in sulfuric acid leaching solution, and first removes ferric iron in leaching solution with acidic phosphate extraction agent, and removes ferric iron in the leaching solution. After adjusting the pH of the iron solution, the vanadium is enriched with an acidic phosphate extractant; Yiqian Ma et al. 38-45.) For the leaching solution containing V(Ⅳ) 2.87g / L, Fe(Ⅱ) 2.71g / L, and Fe(Ⅲ) 8.45g / L, the same two-step solvent extraction method was used to remove iron, first using D2EHPA / TBP extractant removes the ferric iron in the vanadium-containing solution, and then uses D2EHPA / TBP extractant to enrich vanadium after iron removal, and the removal rate of Fe(Ⅲ) is about 90%; although the above method It can separate vanadium and iron in the acid immersion solution, but the process of separating vanadium and iron by two-step solvent extraction is complicated, and the consumption of reagents during the experiment is large
[0006] To sum up, the vanadium-containing leaching solution obtained from stone coal leaching has a high content of impurity aluminum ions and iron ions, which will affect the subsequent process of vanadium enrichment. Therefore, it is necessary to remove impurities from the vanadium-containing leaching solution. The existing vanadium-containing The impurity removal method of the leaching solution has the disadvantages of complex process, large reagent consumption and high vanadium loss rate

Method used

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Embodiment 1

[0022] A method for removing impurities in a vanadium-containing leaching solution. The concrete steps of the method described in this embodiment are:

[0023] Step 1. According to potassium sulfate: the mass ratio of aluminum in the vanadium-containing leach solution is (2.5-3.0): 1, the potassium sulfate is added to the vanadium-containing leach solution, crystallized at 5-8° C. for 3-6 hours, and a period of solid-liquid Separation to obtain liquid and potassium alum after crystallization.

[0024] The chemical composition of the vanadium-containing leaching solution is: the vanadium concentration is 0.8-1.8g / L, the aluminum concentration is 12-25g / L, and the iron concentration is 1-10g / L; the pH value of the vanadium-containing leaching solution is 0.5-1.5 .

[0025] Step 2, according to the amount of total substance in the reducing agent: the ratio of the amount of substance of Fe(III) in the liquid after the crystallization is (1.5~2.5): 1; Add the reducing agent in th...

Embodiment 2

[0031] A method for removing impurities in a vanadium-containing leaching solution. Except following, all the other are with embodiment 1:

[0032] The reducing agent is a mixture of iron powder and sodium sulfite; the precipitating agent is soluble hydrogen oxalate; the cations contained in the precipitating agent are potassium ions and sodium ions.

[0033] The vanadium-containing leaching solution of this embodiment after impurity removal is measured: the vanadium concentration is 0.8-1.8g / L, and the loss rate of vanadium is less than 1%; the aluminum concentration is 3.2-5.0g / L, and the removal rate of aluminum is 70-85%. ; The iron concentration is 0.15~1.6g / L, and the removal rate of iron is 80~95%.

Embodiment 3

[0035] A method for removing impurities in a vanadium-containing leaching solution. Except following, all the other are with embodiment 1:

[0036] The reducing agent is sodium thiosulfate; the precipitating agent is a mixture of soluble oxalates and soluble hydrogen oxalates; the cations contained in the precipitating agent are potassium ions, sodium ions and ammonium ions.

[0037] The vanadium-containing leaching solution of this embodiment after impurity removal is measured: the vanadium concentration is 0.8-1.8g / L, and the loss rate of vanadium is less than 1%; the aluminum concentration is 3.5-6.0g / L, and the removal rate of aluminum is 70-85%. ; The iron concentration is 0.08~1.45g / L, and the removal rate of iron is 80~95%.

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Abstract

The invention relates to an impurity removing method for a vanadium contained leaching agent. According to the technical scheme, potassium sulphate is added into the vanadium contained leaching agent according to the mass ratio of the potassium sulphate to aluminum in the vanadium contained leaching agent being (2.5-4.0):1, crystallization is carried out, primary solid-liquid separation is carried out, and liquid obtained after crystallization and potassium alum are obtained. A reducing agent is added into the liquid obtained after crystallization according to the ratio of the amount of total matter in the reducing agent to the amount of the Fe(III) matter in the liquid obtained after crystallization being (1.5-3.5):1, stirring is carried out, and liquid obtained after reducing is obtained. A precipitator is added into the liquid obtained after reducing according to the ratio of C2O4<2-> matter in the precipitator to the amount of iron matter in the liquid obtained after reducing being (2-15):1, stirring is carried out, secondary solid-liquid separation is carried out, and the vanadium contained leaching agent obtained after impurity removing and filter residues are obtained; the vanadium contained leaching agent obtained after impurity removing is used for the follow-up vanadium enrichment process; and the filter residues are dried, and therefore the oxalates compound by-products of iron are obtained. The impurity removing method has the beneficial effects of being good in vanadium and impurity ion separating effect, simple in process, small in reagent consumption, low in vanadium loss rate and capable of achieving resource utilization.

Description

technical field [0001] The invention belongs to the technical field of vanadium-containing leaching solution. Specifically, it relates to a method for removing impurities in a vanadium-containing leaching solution. Background technique [0002] During the leaching process of vanadium-containing stone coal, a large amount of impurities such as aluminum and iron will be leached together with the vanadium. Excessive concentration of impurities in the vanadium-containing leaching solution will not only lead to emulsification or ion exchange resin poisoning in subsequent extractions, but also reduce Vanadium product purity. Therefore, before the vanadium enrichment process, the impurity ions in the vanadium-containing leaching solution must be removed. Usually, vanadium and impurity ions can be separated by methods such as extraction, ion exchange, and chemical precipitation. [0003] Fu Chaoyang (Fu Chaoyang. One-step method of stone coal vanadium extraction stripping liquid a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/22C22B3/44
CPCC22B3/44C22B34/22Y02P10/20
Inventor 张一敏胡鹏程刘涛黄晶陈铁军
Owner WUHAN UNIV OF SCI & TECH
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