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Method for preparing vanadium dioxide from vanadium slag by short process

A technology of vanadium dioxide and short process, applied in the direction of vanadium oxide, etc., can solve the problems of large environmental pollution, complicated process, high cost, etc., and achieve the effect of short process, high purity and strong applicability

Active Publication Date: 2019-10-22
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

[0004] As mentioned above, most of the raw materials used in the production of vanadium dioxide powder are vanadium pentoxide, or various complex precursors prepared with vanadium pentoxide as raw materials, resulting in higher raw material costs for the preparation of vanadium dioxide. The use of acid and alkali also produces corresponding environmental costs, and the process becomes complicated
In addition V 2 o 5 It is produced by heating and oxidatively decomposing ammonium metavanadate or poly(poly)ammonium vanadate, which itself has a relatively high cost, and the current industrial production process of vanadium pentoxide is relatively polluting to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The vanadium slag is crushed to 0.074mm and accounts for 70%, 100g of vanadium slag is mixed with 10g of calcium carbonate, and then the resulting mixture is added into a muffle furnace and air is introduced to carry out high-temperature roasting, the roasting temperature is controlled at 1100°C, and the roasting time is 60min; Add 200ml of pure water to the clinker obtained from roasting, add 40g of oxalic acid to control the pH of the system to 3.7, control the leaching temperature at 90°C and stir and leaching for 60 minutes, filter to obtain the vanadium-containing leaching solution and residue; concentrate and crystallize the vanadium-containing solution, and separate the solid and liquid Afterwards, vanadyl oxalate solid was obtained. The obtained vanadyl oxalate solid was placed in an atmosphere furnace, fed with nitrogen, calcined at 380° C. for 1 hour, and cooled to obtain vanadium dioxide powder.

[0035] The vanadium dioxide powder obtained in this embodiment...

Embodiment 2

[0037] The vanadium slag comprising the ingredients listed in Table 1 is crushed to 0.074mm and accounts for 80%, 100g of vanadium slag is mixed with 8g of calcium oxide, and then the resulting mixture is added to a muffle furnace and fed with air for high-temperature roasting, and the roasting temperature is controlled to be 950 ℃, the roasting time is 100min; add 300ml pure water to the clinker obtained by roasting, add 30g oxalic acid to control the pH of the system to 4.6, control the leaching temperature at 90℃, stir and leaching for 45min, filter to obtain the vanadium-containing leaching solution and residue; the vanadium-containing solution Carry out concentrated crystallization, and obtain vanadyl oxalate solid after solid-liquid separation. The obtained vanadyl oxalate solid was placed in an atmosphere furnace, fed with argon, calcined at 350°C for 2 hours, and cooled to obtain vanadium dioxide powder.

[0038] The vanadium dioxide powder obtained in this embodiment ...

Embodiment 3

[0040]The vanadium slag containing the ingredients listed in Table 1 is crushed to 0.074mm, accounting for 85%. Take 100g of vanadium slag and put air into the muffle furnace for high-temperature roasting. The roasting temperature is controlled to be 900°C, and the roasting time is 120min; Add 400ml of pure water to the material, add 40g of oxalic acid to control the pH of the system to 3.1, control the leaching temperature at 60°C and stir for 30 minutes, filter to obtain the vanadium-containing leachate and residue; concentrate and crystallize the vanadium-containing solution, and obtain oxalic acid oxygen after solid-liquid separation. Vanadium solid. Place the obtained vanadyl oxalate solid in an atmosphere furnace, vacuumize the furnace to a relative vacuum of -0.15MPa, calcinate at 400°C for 1.5h, and obtain vanadium dioxide powder after cooling.

[0041] The vanadium dioxide powder obtained in this embodiment is detected by ICP, and its purity is 99.91wt%.

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Abstract

The invention discloses a method for preparing vanadium dioxide from vanadium slag by a short process, and belongs to the technical field of preparation of vanadium dioxide. The method comprises the following steps: calcining the vanadium slag to obtain a calcinated clinker; adding water and oxalic acid into the calcined clinker, leaching, filtering, concentrating and crystallizing a filtrate, andthen performing solid-liquid separation to obtain a vanadyl oxalate solid; calcining the vanadyl oxalate solid to obtain the vanadium dioxide. According to the method, the vanadium slag is used as araw material, the oxalic acid is used for selectively leaching vanadium so as to separate the vanadium from other impurity elements, then a vanadium-containing solution is concentrated, crystallized and dried to obtain the vanadyl oxalate solid, and finally the vanadyl oxalate solid is calcined to obtain vanadium dioxide powder; the method is short in process and strong in applicability; in addition, an obtained vanadium dioxide product is high in purity.

Description

technical field [0001] The invention belongs to the technical field of vanadium dioxide preparation, and in particular relates to a method for preparing vanadium dioxide in a short process from vanadium slag. Background technique [0002] Vanadium dioxide is a phase change material, which has the characteristics of transition from a monoclinic semiconductor phase to a tetragonal metal phase at a temperature around 68°C, and the optical and electrical properties of the material will change abruptly. This material can be widely used in fields such as intelligent windows, anti-laser radiation, photoelectric switches and antistatic coatings. [0003] At present, vanadium dioxide mainly uses hydrothermal synthesis method and high temperature thermal reduction method. ammonium acid etc. Such as CN104071843A, using dihydrate oxalic acid to reduce vanadium pentoxide to obtain M phase vanadium dioxide. CN101041464 A, heat and melt vanadium pentoxide at 810°C for 10-30 minutes, pou...

Claims

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Application Information

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IPC IPC(8): C01G31/02
CPCC01G31/02C01P2006/80
Inventor 杨晓陈婷韩慧果
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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