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Method for preparing vanadium electrolyte

A technology of electrolyte and solution, which is applied in the field of preparation of vanadium electrolyte, can solve the problems of complicated steps, high preparation cost, and poor controllability, and achieve the effect of low cost, few steps, and strong controllability of composition

Active Publication Date: 2018-01-09
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the problems of high preparation cost, complicated steps and poor controllability of the existing vanadium electrolyte, the present invention provides a method for preparing vanadium electrolyte from alkaline vanadium-containing solution by solvent extraction. Alkaline vanadium-containing solution can still obtain high-purity vanadium electrolyte through one-step extraction-reextraction, and the obtained vanadium electrolyte can be used in all-vanadium redox flow batteries

Method used

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  • Method for preparing vanadium electrolyte
  • Method for preparing vanadium electrolyte

Examples

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Embodiment 1

[0041] Dissolve the vanadium raw material in sodium hydroxide alkali solution to obtain an alkaline solution containing vanadium ~ 20g / L. The alkaline vanadium-containing solution contains impurities (g / L): Si 0.74; Al 0.36; Ca 0.039; Mn 0.017; Cu 0.012; Na 39.7, Fe and other impurities are less than 10mg / L.

[0042] Add sulfuric acid to the basic vanadium-containing solution to adjust the pH to 3.0, and then add sodium sulfite heptahydrate as a reducing agent. The amount of sodium sulfite is 1.1 times the theoretical content, and the vanadium is completely reduced to tetravalent. The solution after reduction was added with 0.1% hexamethylphosphoramide as a stabilizer, and then extracted with 30% (v / v) P507 / kerosene, compared to (organic phase / water phase volume ratio) 1:1, the three levels of vanadium at room temperature Stage countercurrent stage extraction, control the equilibrium pH to 1.8, and the extraction rate is 99%. The organic phase after extraction was mixed with ...

Embodiment 2

[0044] The basic vanadium-containing solution in Example 1 is adjusted to a pH value of 0.2 with hydrochloric acid, and then added H 2 o 2 reduction, H 2 o 2 The consumption is 2 times of theoretical consumption, and the feed liquid after reduction, adds 1% phenylphosphoric acid, adopts 40% (v / v) P204 / heptane extraction again, adopts five-stage countercurrent extraction, compares (organic phase / water Phase volume ratio) 5: 1, the five-stage extraction of vanadium, the control equilibrium pH is 1.5, and the extraction rate is 99.8%. The extracted organic phase was washed with 0.02M H2O containing 5g / L V(IV). 2 SO 4 The solution was subjected to five-stage countercurrent washing at room temperature, and the washing ratio (volume ratio of organic phase / water phase) was 5:1. After washing with 4.5mol / L H 2 SO 4 Carry out five-stage countercurrent stripping of vanadium under the condition of 20:1 with the ratio (organic phase / water phase volume ratio) at room temperature, t...

Embodiment 3

[0046] The basic vanadium-containing solution in Example 1 was adjusted to pH 1.5 with sulfuric acid, then added oxalic acid for reduction, then added 0.5% methylphosphoric acid as a silicon stabilizer, extracted with 5% (v / v) Cyannex272 / tridecane, The extraction ratio (volume ratio of organic phase / water phase) is 1:5, at room temperature, the equilibrium pH is controlled to be 1.5, and the single-stage extraction rate of vanadium is 85%. The organic phase after extraction was mixed with 0.05mol / L H containing 2g / L V 2 SO 4 The solution was washed at room temperature with a wash ratio (volume of organic phase:volume of aqueous phase) of 10:1. After washing with 5.0mol / L H 2 SO 4 Carry out single-stage stripping vanadium under the condition of being 1: 1 at room temperature, the stripping rate of vanadium is 95.7%, and the content of stripping liquid contains 1.59mol / L V and 2.9mol / L H 2 SO 4 , the total content of impurities (including Si, Al, Fe, Mg, Ca) is less than ...

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Abstract

A method for preparing a vanadium electrolyte comprises the following steps that (1) a vanadium-containing acidic solution is prepared; (2) vanadium in the vanadium-containing acidic solution is reduced to be tetravalence, and a stabilizer is added to obtain a vanadium-containing water phase, wherein the stabilizer is alkyl phosphamide, aryl phosphate, alkyl phosphate or amine alkyl phosphate; (3)the vanadium-containing water phase is extracted through an organic phase, and the extracted organic phase is washed through washing liquid; (4) the washed organic phase is subjected to reverse extraction to obtain reverse extraction liquid; and (5) organic matter carried in the reverse extraction liquid is removed, and thus the vanadium electrolyte is obtained. According to the method, the middle step for preparing a high-purity vanadium oxide is omitted, the one-step solvent extraction method is adopted, the vanadium electrolyte is prepared from the alkaline vanadium-containing solution, inthe preparing process, the steps are few, simple and easy to control, the cost is low, and the prepared vanadium electrolyte is high in composition controllability.

Description

technical field [0001] The invention relates to the field of preparation of vanadium electrolyte, in particular to a method for preparing vanadium electrolyte by using alkaline vanadium-containing solution as raw material. Background technique [0002] With the rapid development of clean energy, energy storage technology is particularly important. The all-vanadium redox flow battery (vanadium battery) uses vanadium ions of different valence states in the electrolyte to store and convert electrical energy. It has the advantages of high energy storage power, high charge and discharge efficiency, many cycles, simple equipment, safety and environmental protection. Vanadium electrolyte is also one of the core materials of the whole battery, and its production technology and production cost largely determine the cost of vanadium batteries. The vanadium concentration, ionic strength, acidity and impurity content in the vanadium electrolyte have a great influence on the performance...

Claims

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Application Information

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IPC IPC(8): C22B34/22C22B3/38
CPCY02P10/20
Inventor 齐涛陈德胜朱兆武王丽娜王伟菁张健刘亚辉赵宏欣贾志军
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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