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A method for removing impurities in vanadyl sulfate crystals

A technology of vanadyl sulfate crystal and vanadyl sulfate, which is applied in chemical instruments and methods, vanadium compounds, climate sustainability, etc., can solve the problems of long process flow, expensive reagents, and high cost, so as to simplify the process flow and reduce production. Cost, good economic effect

Active Publication Date: 2018-04-24
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main reason restricting the development of vanadium battery at present is that its cost remains high, and the root cause is that the preparation cost of electrolyte is too high. The Chinese patent of CN103482702A " method for preparing high-purity vanadium oxide and high-concentration electrolyte for vanadium battery") prepares battery-grade vanadyl sulfate based on high-purity vanadium pentoxide, and the process of preparing high-purity vanadium pentoxide is often It involves multiple steps such as remelting, separation and purification, precipitation, and calcination. The process is complicated, the process is long, and the effect of impurity removal is not ideal. The main impurities such as chromium and iron are high. The presence of iron and chromium will seriously reduce the efficiency of vanadium batteries. Energy efficiency and corrosion of electrode materials seriously affect the operation of the vanadium battery system
[0003] At present, the impurity removal of vanadyl sulfate is mainly divided into two types, one is to remove impurities in raw materials (including qualified liquid of vanadium pentoxide and vanadium), and the main step is to return vanadium pentoxide to the qualified liquid or directly to the qualified liquid Add precipitant, such as magnesium salt, aluminum salt and calcium salt, etc. to remove anionic impurities such as silicate, chromate, phosphate in the solution, and then remove most of cationic impurities, such as sodium, potassium, calcium, Magnesium, etc. (Refer to the Chinese patent "Preparation method of high-concentration and high-purity vanadium battery electrolyte" with publication number CN103515642A; Hou Haijun. Research on the preparation technology of high-purity ammonium metavanadate [J]. Steel Vanadium Titanium, 2013, 34(3)), this method has a long process flow, complex operation process, unsatisfactory impurity removal effect and the introduction of new impurity ions
Another method of impurity removal is mainly through the method of extraction-back extraction. Although this method saves the processes such as leachate removal of impurities, ammonium salt precipitation of vanadium, and redissolution, the production process is simplified, production time is saved, and the preparation process is unnecessary. Introduce other impurities, but the extraction and ion exchange have problems such as small processing capacity, expensive reagents, high cost, deteriorating operating environment and low purity of the product (reference publication number is CN103151549A Chinese patent "a preparation based on extraction-back extraction system Method for high-purity vanadium battery electrolyte"); In addition, there is a method for removing impurities directly in vanadyl sulfate solution
[0004] The above impurity removal methods all have their own shortcomings, which limit their industrial application and hinder the development of vanadium batteries to a certain extent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] Evaporate the vanadyl sulfate solution containing impurity elements (Cr 0.223%, K 1.22%, Na 1.35%) to a supersaturated state, take 10L of 1mol vanadium ions in the supersaturated solution, add 100g of seed crystals, h cooling rate to carry out cooling crystallization to obtain the first vanadyl sulfate crystal. Wherein, the first vanadyl sulfate crystal contains 0.017% Cr, 0.015% K and 0.022% Na.

[0032] Take by weighing the first vanadyl sulfate crystal of 100g, join in 50ml absolute ethanol solution, stir and wash 3min, after filtering, the second vanadyl sulfate crystal of gained is added to 100ml concentration and is the pure vanadyl sulfate saturated solution of 3.0mol / L, Stir and wash for 3 minutes, filter, and dry at 60°C for 30 minutes to obtain vanadyl crystals of the third acid, in which Cr 85%; compared with the first vanadyl sulfate crystal, the reduction rate of Cr in the third vanadyl sulfate crystal is 52.9%, the reduction rate of Na is 53.3%, and the re...

example 2

[0034] Evaporate the vanadyl sulfate solution containing impurity elements (Cr 0.072%, K 0.121%, Na 0.257%) to a supersaturated state, take 10L of 1mol vanadium ions in the supersaturated solution, add 80g of seed crystals, and heat at 1.2°C / h cooling rate to carry out cooling crystallization to obtain the first vanadyl sulfate crystal. Wherein, the first vanadyl sulfate crystal contains 0.006% Cr, 0.009% K and 0.006% Na.

[0035] Take by weighing the first vanadyl sulfate crystal of 100g, join in 80ml absolute ethanol solution, stir and wash 4min, after filtering, the gained second vanadyl sulfate crystal is added to 80ml concentration and is the pure vanadyl sulfate saturated solution of 3.5mol / L, Stir and wash for 4 minutes, filter, and dry at 55°C for 46 minutes to obtain the third vanadyl sulfate crystal, in which Cr 87%; compared with the first vanadyl sulfate crystal, the reduction rate of Cr in the third vanadyl sulfate crystal is 66.7%, the reduction rate of Na is 66...

example 3

[0037] Evaporate the vanadyl sulfate solution containing impurity elements (Cr 0.457%, K 0.647%, Na 0.813%) to a supersaturated state, take 10L of 1mol vanadium ions in the supersaturated solution, add 120g of seed crystals, and heat at 2°C / h cooling rate to carry out cooling crystallization to obtain the first vanadyl sulfate crystal. Wherein, the first vanadyl sulfate crystal contains 0.033% Cr, 0.054% K and 0.042% Na.

[0038] Weigh 100g of the first vanadyl sulfate crystals, add it to 100ml of absolute ethanol solution, stir and wash for 4.8min, filter and add the second vanadyl sulfate crystals to 120ml of pure vanadyl sulfate saturated solution with a concentration of 4.0mol / L , stirred and washed for 5 minutes, filtered, and dried at 50°C for 60 minutes to obtain the third vanadyl sulfate crystal, Cr92%; compared with the first vanadyl sulfate crystal, the reduction rate of Cr in the third vanadyl sulfate crystal is 51.5%, the reduction rate of Na is 51.9%, and the red...

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Abstract

The invention provides a method for removing impurities in vanadyl sulfate crystal, comprising: washing to remove crystal water and crystal surface impurities for first vanadyl sulfate crystal, and filtering to obtain second vanadyl sulfate crystal. The method for removing impurities in vanadyl sulfate crystal enables impurity elements to be removed directly from vanadyl sulfate crystal, vanadium content of vanadyl sulfate crystal is increased, the technical process is simplified, production cost is reduced, and the method is economical.

Description

technical field [0001] The invention relates to the field of hydrometallurgy, in particular to a method for removing impurities in vanadyl sulfate crystals. Background technique [0002] As an emerging energy storage system, batteries have many advantages such as long service life, large capacity, high power, and high safety. The main reason restricting the development of vanadium battery at present is that its cost remains high, and the root cause is that the preparation cost of electrolyte is too high. The Chinese patent of CN103482702A " method for preparing high-purity vanadium oxide and high-concentration electrolyte for vanadium battery") prepares battery-grade vanadyl sulfate based on high-purity vanadium pentoxide, and the process of preparing high-purity vanadium pentoxide is often It involves multiple steps such as remelting, separation and purification, precipitation, and calcination. The process is complicated, the process is long, and the effect of impurity rem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00H01M8/18
CPCC01G31/00C01P2006/80H01M8/18Y02E60/50Y02P70/50
Inventor 刘波彭穗汪南方李道玉陈婷曹敏龙秀丽陈勇韩慧果
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD