Method for preparing M-phase VO2 by using inactivated vanadium battery positive electrolyte

A positive electrolyte and vanadium battery technology, applied in the field of vanadium dioxide, can solve the problems of vanadium ion concentration and sulfuric acid concentration exceeding the standard, vanadium ion valence mismatch, unusable and other problems, achieve high added value, easy promotion and application, and low cost low effect

Inactive Publication Date: 2019-12-27
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the vanadium battery electrolyte has been recycled for a long time, the concentration of vanadium ions and sulfuric acid seriously exceeds the standard, the valence state of vanadium ions does not match, and the energy attenuation is serious, which makes it invalid and unusable

Method used

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  • Method for preparing M-phase VO2 by using inactivated vanadium battery positive electrolyte
  • Method for preparing M-phase VO2 by using inactivated vanadium battery positive electrolyte

Examples

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Effect test

Embodiment 1

[0027] Measure 500ml of 1# electrolyte and heat it to 70°C in the reaction vessel, and continuously feed high-purity SO into the electrolyte during slow stirring 2 Gas for 6h, after aeration, continue to insulate and stir for 30min to obtain a blue-black solution, and dropwise add NaOH solution to adjust the pH of the electrolyte to 4, filter to obtain a black precipitate, wash twice with deionized water, dry and grind to obtain a black powder, and Evenly spread on the bottom of the porcelain boat, place in a vacuum furnace, bake at 600°C for 5 hours, cool down to room temperature to obtain VO 2 48.4g, the total vanadium yield is 70.7%.

Embodiment 2

[0029] Measure 500ml of 1# electrolyte and heat it to 30°C in the reaction vessel, add 260g of vanadium sulfate V decahydrate to the electrolyte 2 (SO 4 ) 3 10H 2O, keep stirring for 3 hours to obtain a blue-black solution, and dropwise add ammonia water with a mass fraction of 25-28% to adjust the pH of the electrolyte to 3, filter to obtain a black precipitate, wash twice with deionized water, dry and grind to obtain a black powder , spread it evenly on the bottom of the porcelain boat, place it in an atmosphere furnace, and bake it at 650 ° C for 4 hours under the protection of argon gas, and continue to cool down to room temperature with argon gas to obtain VO 2 44.7g, the total vanadium yield is 65.3%.

Embodiment 3

[0031] Measure 500ml of 1# electrolyte and heat it to 100°C in the reaction vessel, add 87g of dihydrate oxalic acid H to the electrolyte 2 C 2 o 4 2H 2 O, keep stirring for 9h to obtain a blue-black solution, and add Na to it 2 CO 3 Adjust the pH of the electrolyte to 5, filter to obtain a black precipitate, wash it twice with deionized water, dry and grind to obtain a black powder, spread it evenly on the bottom of the porcelain boat, place it in a vacuum furnace, and bake it at 700°C for 3 hours. Cool down to room temperature to get VO 2 53.1g, the total vanadium yield is 77.6%.

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Abstract

The invention discloses a method for preparing M-phase VO2 by using an inactivated vanadium battery positive electrolyte. The method belongs to the technical field of vanadium dioxide, and comprises the following steps: (1) adding a reducing agent into the anode electrolyte of the failed vanadium battery to carry out reduction reaction, adding a precipitant into the electrolyte after the reductionreaction is finished to adjust the pH value to 3-6, carrying out solid-liquid separation, and washing the solid product to obtain a black precipitate; and (2) calcining the black precipitate to obtain VO2 powder. According to the method, the inactivated vanadium battery electrolyte is used as a raw material, so that resource recycling is realized, and the preparation cost of VO2 is reduced; meanwhile, the method is simple in process and suitable for industrial application; and the prepared VO2 is high in purity, high in additional value and high in crystallinity, and can be widely applied tothe fields of intelligent windows, photoelectric switches, thermistors and the like.

Description

technical field [0001] The invention belongs to the technical field of vanadium dioxide, and in particular relates to a method for preparing M-phase VO by utilizing the anode electrolyte of an invalid vanadium battery. 2 Methods. Background technique [0002] Vanadium dioxide has a variety of crystal phases such as A phase, M phase, B phase, and R phase. Among them, the M phase VO 2 It has phase transition characteristics at around 68°C, from the monoclinic structure M phase to the tetragonal rutile structure R phase, and this process is reversible as the temperature increases and decreases. At the same time, as the phase transition occurs, its transmittance , reflectivity, resistivity, magnetic susceptibility, etc. all have sudden changes, therefore, VO 2 It is widely used in smart windows, photoelectric switches, thermistors and other fields. [0003] Currently, VO 2 Powder preparation methods mainly include hydrothermal method, thermal decomposition method, sol-gel me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2004/03
Inventor 刘波彭穗李道玉
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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