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Method for preparing NaV2O5 from vanadium-enriched liquid obtained by extracting vanadium from shale

A technology of vanadium-enriched liquid and vanadium liquid, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of ammonia nitrogen wastewater and waste gas environmental pollution, increase process energy consumption, low conversion efficiency, etc., to avoid ammonia nitrogen Effects of waste water, shortened preparation time, and reduced energy consumption

Active Publication Date: 2018-11-02
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method takes a long time to synthesize, has low conversion efficiency and poor reproducibility
Chinese patent 201610662118.X discloses a NaV 2 o 5 The preparation method of the method is to dissolve vanadium pentoxide in sodium hydroxide solution, then reduce it with hydrogen, and obtain NaV by hydrothermal reaction. 2 o 5 , this patent uses hydrogen as the reducing agent, although it is clean and non-polluting, but using gas as the reducing agent, the instrument needs excellent airtightness, and there is a risk of explosion
On the one hand, from vanadium-rich liquid to process vanadium products, and then to NaV 2 o 5 , which increases the process flow and corresponding energy consumption; on the other hand, when preparing ammonium vanadate salt and ammonium polyvanadate, excessive ammonium is added to produce a large amount of ammonia nitrogen wastewater, which is prepared by pyrolysis of ammonium vanadate salt and ammonium polyvanadate When vanadium pentoxide is used, a large amount of nitrogen-containing waste gas is produced, and ammonia nitrogen waste water and waste gas cause serious environmental pollution

Method used

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  • Method for preparing NaV2O5 from vanadium-enriched liquid obtained by extracting vanadium from shale
  • Method for preparing NaV2O5 from vanadium-enriched liquid obtained by extracting vanadium from shale

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Preparation of NaV from a vanadium-rich liquid for extracting vanadium from shale 2 o 5 method, including the following steps:

[0031] 1) According to the molar ratio of oxalate and vanadium in the vanadium-rich solution is 0.25, oxalic acid is dissolved in the shale vanadium-rich solution with a vanadium concentration of 17.52g / L, and the pH of the solution is adjusted to 3.0 with sulfuric acid to obtain the to-be-reacted liquid;

[0032] 2) Transfer the liquid to be reacted to a high-temperature and high-pressure reactor, react for 7 hours at a temperature of 180° C., and obtain a slurry after natural cooling;

[0033]3) The slurry is separated into solid and liquid to obtain solid and liquid, and the solid is vacuum-dried at 60°C to obtain NaV 2 o 5 ;

[0034] NaV in this example 2 o 5 The conversion rate is 98.64%, and the purity is 99.07%.

[0035] The NaV obtained by the preparation method of this embodiment 2 o 5 Refer to the attached X-ray diffraction...

Embodiment 2

[0038] Preparation of NaV from a vanadium-rich liquid for extracting vanadium from shale 2 o 5 method, including the following steps:

[0039] 1) According to the molar ratio of oxalate and vanadium in the vanadium-rich solution being 1.0, potassium oxalate is dissolved in the shale vanadium-rich solution with a vanadium concentration of 19.68g / L, and the pH of the solution is adjusted to 5.0 with sulfuric acid to obtain The reaction solution;

[0040] 2) Transfer the liquid to be reacted to a high-temperature and high-pressure reactor, react for 6 hours at a temperature of 220° C., and obtain a slurry after natural cooling;

[0041] 3) The slurry is separated into solid and liquid to obtain solid and liquid, and the solid is vacuum dried at 80°C to obtain NaV 2 o 5 ;

[0042] NaV in this example 2 o 5 The conversion rate is 99.11%, and the purity is 99.10%.

Embodiment 3

[0044] A vanadium-rich liquid NaV for extracting vanadium from shale 2 o 5 method, including the following steps:

[0045] 1) According to the molar ratio of oxalate root and vanadium in the vanadium-rich solution being 2.0, sodium oxalate is dissolved in the shale vanadium-rich solution with a vanadium concentration of 22.73g / L, and the pH of the solution is adjusted to 7.0 with sulfuric acid to obtain The reaction solution;

[0046] 2) Transfer the liquid to be reacted to a high-temperature and high-pressure reactor, react at a temperature of 230°C for 8 hours, and obtain a slurry after natural cooling;

[0047] 3) The slurry is separated into solid and liquid to obtain solid and liquid, and the solid is vacuum-dried at 60°C to obtain NaV 2 o 5 ;

[0048] NaV in this example 2 o 5 The conversion rate is 99.54%, and the purity is 99.32%.

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Abstract

The invention discloses a method for preparing NaV2O5 from vanadium-enriched liquid obtained by extracting vanadium from shale. The method comprises the steps that 1, vanadium shale pickle liquor is reacted through an extraction-back extraction technology to obtain the vanadium-enriched liquid; 2, a reducing agent is dissolved in the vanadium-enriched liquid according to the molar ratio of the reducing agent to vanadium in the vanadium-enriched liquid of 0.25-3.0, acid liquor or alkaline liquor is used for adjusting the solution pH value to be 2.0-7.0, and a to-be-reacted solution is obtained;3, the to-be-reacted solution obtained in step 2 is reacted at 180-230 DEG C for 5-8 hours, and after natural cooling, slurry is obtained; 4, the slurry obtained in step 3 is subjected to solid-liquid separation to obtain solid and liquid, and the solid is subjected to vacuum drying at 60-100 DEG C to obtain the NaV2O5. The method has the advantages of being environmentally friendly, pollution-free, safe, simple in technology, short in preparation time, low in energy consumption and the like.

Description

technical field [0001] The invention relates to the technical field of preparing non-ferrous metal smelting, in particular to a vanadium-rich liquid for extracting vanadium from shale to prepare NaV 2 o 5 Methods. Background technique [0002] NaV 2 o 5 It is a layered structure vanadate, Na ion is located in V 2 o 5 Between the layers, it has good charge-discharge cycle stability, and can be used as the positive electrode material of lithium batteries, and can also be used as the positive electrode material of sodium batteries. Therefore, NaV 2 o 5 It is a very promising electrochemical material. As a successor to GeCuO 3 The second inorganic spin Pels material after that. NaV 2 o 5 The bandgap from the spin-single-crystal ground state to the first excited state is very small, which makes it also of great significance in quantum switches. [0003] Now reported NaV 2 o 5 There are two kinds of preparation methods: solid phase sintering method and hydrothermal s...

Claims

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Application Information

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IPC IPC(8): C01G31/00
CPCC01G31/00C01P2002/72C01P2004/03C01P2006/80
Inventor 张一敏康倩包申旭张国斌刘涛
Owner WUHAN UNIV OF TECH
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