CN109722533A - A method of vanadium trioxide is prepared using extracting vanadium from stone coal pickle liquor - Google Patents
A method of vanadium trioxide is prepared using extracting vanadium from stone coal pickle liquor Download PDFInfo
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Abstract
The invention discloses a kind of methods for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor, comprising the following steps: extracting vanadium from stone coal pickle liquor obtains extracting vanadium from stone coal richness vanadium scavenging solution through ion exchange resin absorption-desorption technique;Sodium hydroxide is added or sulfuric acid solution adjusts pH to 1~3, obtains liquid to be restored;Zinc powder reduction is added and is stirred, filter residue is filtered and discarded after reduction, obtains trivalent vanadium ion solution;Sodium hydroxide solution is added and reaches 5-6 to pH, is stirred, trivalent vanadium ion occurs precipitation reaction and is converted into vanadium hydroxide, and vanadium hydroxide filter cake is obtained by filtration;It will be placed in tube furnace after the drying of vanadium hydroxide filter cake, in N2Lower calcining and decomposing is protected to obtain vanadium trioxide.The present invention directly can prepare vanadium trioxide from extracting vanadium from stone coal richness vanadium scavenging solution, simplify technique, the generation of ammonia nitrogen waste water and ammonia is avoided, reduction reaction does not need to implement at high temperature under high pressure, has the advantages that simple process, easy to operate, production cost is low, environmental-friendly.
Description
Technical field
The present invention relates to non-ferrous metallurgy technology fields, more particularly to a kind of to utilize extracting vanadium from stone coal pickle liquor
The method for preparing vanadium trioxide.
Background technique
Vanadium trioxide is in grey black metallic luster at normal temperature, is a kind of important inorganic functional material, in metallurgy, electricity
The industries such as son, chemical industry have important application.Vanadium trioxide can be used for producing vanadium iron or metal vanadium powder, can also be by three oxidations
Vanadium carbide made of two vanadium or vanadium nitride are added molten steel and produce special steel material.Vanadium trioxide or a kind of important phase transition material
Material, optoelectronic switch, temperature sensor, holographic storage material, lithium ion battery material and in terms of have
There is important application value.
Currently, there are two types of the preparation methods of vanadium trioxide, the direct-reduction process of additional reducing agent and not additional reducing agent
Thermal decomposition method.The raw material of thermal decomposition method mainly has ammonium metavanadate and poly ammonium vanadate, and thermal decomposition method is to utilize ammonium vanadate heat point
The ammonia that solution generates decomposes the nascent hydron of generation further to restore vanadic anhydride, and advantage is not need additional reducing agent to drop
Lower part cost, the disadvantage is that ammonia cracking not exclusively causes reducing atmosphere inadequate, the exclusion for the ammonia not cracked will cause ring
Border pollution.The direct-reduction process of additional reducing agent is the method for preparing vanadium trioxide being widely used at present, using reducing agent
Usually C, CO, SO2、H2、NH3And CH4Deng, at high temperature heat-treat ammonium metavanadate, poly ammonium vanadate or vanadic anhydride it is contour
Valence vfanadium compound is to obtain vanadium trioxide, the disadvantages of this method are: thermal reduction temperature is high, energy consumption is high, and production technology is complicated.
Current vanadium trioxide preparation mostly uses ammonium metavanadate, poly ammonium vanadate or vanadic anhydride for raw material, preparation process compared with
For complexity, production cost is higher.Meanwhile ammonium metavanadate, poly ammonium vanadate preparation process in generate a large amount of ammonia nitrogen useless
Water, the process that thermal decomposition ammonium metavanadate, poly ammonium vanadate prepare vanadic anhydride can discharge a large amount of ammonia, these waste water and useless
Gas all causes serious pollution to environment.
Therefore, a kind of simple process how is provided, the vanadium trioxide preparation process that environmental-friendly, production cost is low is this
The problem of field technical staff's urgent need to resolve.
Summary of the invention
In view of this, the present invention provides a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor, this hair
It is bright by selecting suitable reducing agent, pentavalent vanadium is directly reduced to trivalent vanadium under normal pressure and temperature, simplifying processing step makes
Production cost reduces, while avoiding the generation of ammonia nitrogen waste water and ammonia, is conducive to the sustainable development of environment, has good
Prospects for commercial application.
To achieve the goals above, the invention adopts the following technical scheme:
A method of vanadium trioxide is prepared using extracting vanadium from stone coal pickle liquor, comprising the following steps:
(1) extracting vanadium from stone coal pickle liquor obtains extracting vanadium from stone coal richness vanadium scavenging solution through ion exchange resin absorption-desorption technique;
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 1~3 is adjusted using sodium hydroxide or sulfuric acid solution, obtains liquid to be restored;
(3) zinc powder reduction is added in the liquid to be restored that step (2) obtains and is stirred, is filtered after reduction and discards filter
Slag obtains trivalent vanadium ion solution;
(4) sodium hydroxide solution is added in the trivalent vanadium ion solution that step (3) obtains until pH reaches 5-6, into
Row stirring, trivalent vanadium ion occur precipitation reaction and are converted into vanadium hydroxide, and vanadium hydroxide filter cake is obtained by filtration;
(5) it is placed in tube furnace after the vanadium hydroxide filter cake drying obtained step (4), in N2Lower calcining and decomposing is protected to obtain
To vanadium trioxide product.
By adopting the above technical scheme the utility model has the advantages that
1, since the present invention directly can prepare vanadium trioxide from extracting vanadium from stone coal richness vanadium scavenging solution, with prior art phase
Than eliminating the process by preparing intermediate products ammonium vanadate or poly ammonium vanadate etc. through ammonium salt precipitating containing vanadium solution, simplifying work
Skill avoids the generation of ammonia nitrogen waste water and ammonia, and reduction reaction does not need to implement under high-temperature and high-pressure conditions, has technique letter
Advantage single, easy to operate, production cost is low, environmental-friendly.
2, the present invention using zinc powder as reducing agent, zinc powder can rapidly and efficiently by pentavalent vanadium in extracting vanadium from stone coal pickle liquor also
Originally it is trivalent vanadium, and with the increase of zinc powder dosage, can significantly improves the conversion ratio of product, but when zinc powder dosage reaches
When certain value, the conversion ratio of product tends towards stability, and no longer significantly improves.The present invention is restored than the prior art with hydrogen
Advantage: 1) can operate under normal temperature and pressure conditions, not high to equipment requirement, reduce energy consumption, reduce production cost;2) hydrogen is
A kind of flammable explosive gas has certain security risk.
Preferably, the vanadium in the extracting vanadium from stone coal richness vanadium scavenging solution exists in the form of five valence states, vanadium concentration be 30~
100g/L。
Preferably, the adsorbent that the ion exchange resin absorption-desorption technique uses is polystyrene macroporous type highly basic
Any one in anion exchange resin or polystyrene macroporous type weak basic anion exchange resin;The ion exchange resin
The strippant that absorption-desorption technique uses is mixed in a certain ratio gained for any one or two kinds in NaOH or NaCl solution
Mixed solution.
By adopting the above technical scheme the utility model has the advantages that the adsorbent that the present invention uses can effectively be enriched with extracting vanadium from stone coal acidleach
Vanadium in liquid, greatly improves the concentration of vanadium, while removing the foreign ions such as removing heavy metals, is purified solution containing vanadium.
Preferably, the concentration control of strippant NaOH and NaCl in 0.5-2mol/L, the mixing strippant
Mol ratio is controlled in 1:0.5-1.5.
Preferably, the additional amount of zinc powder is 1.2~1.5 times of theoretical amount in the step (3), and reduction temperature is room
Temperature, recovery time are 20~60min, and mixing speed is 100~500r/min.
By adopting the above technical scheme the utility model has the advantages that pentavalent vanadium rapidly and efficiently can be reduced to trivalent vanadium by zinc powder, with
Zinc powder dosage, the increase of recovery time and mixing speed can significantly improve the conversion ratio of product, but when zinc powder dosage reaches
When to certain value, the conversion ratio of product tends towards stability, and no longer significantly improves.
Preferably, which is characterized in that the reaction time of precipitation reaction is 30~90min, reaction temperature in the step (4)
It is 20~60 DEG C, mixing speed is 100~500r/min.
Preferably, N in the step (5)2Flow is 1L/min, and heating rate is 5 DEG C/min, and calcination time is 1~5h.
By adopting the above technical scheme the utility model has the advantages that making the vanadium hydroxide of trivalent sufficiently be decomposed into vanadium trioxide, simultaneously
It prevents vanadium trioxide to be oxidized to high price barium oxide, guarantees product purity.
Compared with prior art, the present invention makes using extracting vanadium from stone coal pickle liquor as raw material by purification, reduction, precipitating, calcining
99% vanadium trioxide is up to for purity, and the conversion ratio of vanadium trioxide is greater than 90%, present invention eliminates by containing
The process that vanadium solution prepares intermediate products ammonium vanadate or poly ammonium vanadate etc. through ammonium salt precipitating, simplifies technique, avoids ammonia nitrogen
The generation of waste water and ammonia, reduction reaction do not need to implement under high-temperature and high-pressure conditions, have simple process, easy to operate, raw
Produce at low cost, environmental-friendly advantage.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
(1) extracting vanadium from stone coal pickle liquor obtains the bone coal that vanadium concentration is 50g/L through ion exchange resin absorption-desorption technique
Vanadium extraction richness vanadium scavenging solution, ion exchange resin therein are D301 macroporous type weak basic anion exchange resin, and strippant is
The mixed solution of the NaOH and NaCl of the 1.0mol/L ratio mixing of 1:1 in molar ratio, the vanadium in pickle liquor is with the shape of five valence states
Formula exists.
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 2.5 is adjusted with sodium hydroxide or sulfuric acid solution;
(3) zinc powder reduction is added, zinc powder additional amount is 1.2 times of theoretical amount, and reduction temperature is room temperature, and the recovery time is
30min, mixing speed 150r/min, filtering, discard filter residue, obtain three valence state vanadium ion solution;
(3) sodium hydroxide solution is added in three valence state vanadium ion solution and stops to pH value for 5.8, reaction time 45min, instead
30 DEG C of temperature are answered, mixing speed 150r/min.After three valence state vanadium ions are converted into vanadium hydroxide precipitating, hydrogen-oxygen is obtained by filtration
Change vanadium filter cake, is dried for standby.
(4) the vanadium hydroxide filter cake after drying is placed in tube furnace, in N2The lower calcining of protection, nitrogen flow 1L/
Min, heating rate are 5 DEG C/min, and calcination temperature is 650 DEG C, calcination time 2h, obtain vanadium trioxide through calcining and decomposing and produce
Product.
The conversion ratio of vanadium trioxide is 90.2% in the present embodiment, and the purity of vanadium trioxide is 99.0%.
Embodiment 2
(1) extracting vanadium from stone coal pickle liquor obtains the bone coal that vanadium concentration is 80g/L through ion exchange resin absorption-desorption technique
Vanadium extraction richness vanadium scavenging solution, ion exchange resin therein are D202 macroporous type strong basic anion-exchange resin, and strippant is
The NaOH solution of 2.0mol/L, the vanadium in pickle liquor exist in the form of five valence states.
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 2 is adjusted with sodium hydroxide or sulfuric acid solution;
(3) zinc powder reduction is added, zinc powder additional amount is 1.4 times of theoretical amount, and reduction temperature is room temperature, and the recovery time is
50min, mixing speed 450r/min, filtering, discard filter residue, obtain three valence state vanadium ion solution;
(4) sodium hydroxide solution is added in three valence state vanadium ion solution and stops to pH value for 5.2, reaction time 75min, instead
Answer temperature 50 C, mixing speed 450r/min.After three valence state vanadium ions are converted into vanadium hydroxide precipitating, hydrogen-oxygen is obtained by filtration
Change vanadium filter cake, is dried for standby.
(5) the vanadium hydroxide filter cake after drying is placed in tube furnace, in N2The lower calcining of protection, nitrogen flow 1L/
Min, heating rate are 5 DEG C/min, and calcination temperature is 800 DEG C, calcination time 4h, obtain vanadium trioxide through calcining and decomposing and produce
Product.
The conversion ratio of vanadium trioxide is 92.0% in the present embodiment, and the purity of vanadium trioxide is 99.2%.
Embodiment 3
(1) extracting vanadium from stone coal pickle liquor obtains the bone coal that vanadium concentration is 30g/L through ion exchange resin absorption-desorption technique
Vanadium extraction richness vanadium scavenging solution, ion exchange resin therein are D202 macroporous type strong basic anion-exchange resin, and strippant is
The NaCl solution of 2.0mol/L, the vanadium in pickle liquor exist in the form of five valence states.
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 1 is adjusted with sodium hydroxide or sulfuric acid solution;
(3) zinc powder reduction is added, zinc powder additional amount is 1.3 times of theoretical amount, and reduction temperature is room temperature, and the recovery time is
20min, mixing speed 500r/min, filtering, discard filter residue, obtain three valence state vanadium ion solution;
(4) sodium hydroxide solution is added in three valence state vanadium ion solution and stops to pH value for 5.0, reaction time 90min, instead
20 DEG C of temperature are answered, mixing speed 500r/min.After three valence state vanadium ions are converted into vanadium hydroxide precipitating, hydrogen-oxygen is obtained by filtration
Change vanadium filter cake, is dried for standby.
(5) the vanadium hydroxide filter cake after drying is placed in tube furnace, in N2The lower calcining of protection, nitrogen flow 1L/
Min, heating rate are 5 DEG C/min, and calcination temperature is 900 DEG C, calcination time 1h, obtain vanadium trioxide through calcining and decomposing and produce
Product.
The conversion ratio of vanadium trioxide is 93% in the present embodiment, and the purity of vanadium trioxide is 99.1%.
Embodiment 4
(1) extracting vanadium from stone coal pickle liquor obtains the bone coal that vanadium concentration is 100g/L through ion exchange resin absorption-desorption technique
Vanadium extraction richness vanadium scavenging solution, ion exchange resin therein are D301 macroporous type weak basic anion exchange resin, and strippant is
The NaCl solution of 0.5mol/L, the vanadium in pickle liquor exist in the form of five valence states.
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 3 is adjusted with sodium hydroxide or sulfuric acid solution;
(3) zinc powder reduction is added, zinc powder additional amount is 1.5 times of theoretical amount, and reduction temperature is room temperature, and the recovery time is
50min, mixing speed 300r/min, filtering, discard filter residue, obtain three valence state vanadium ion solution;
(4) sodium hydroxide solution is added in three valence state vanadium ion solution and stops to pH value for 6.0, reaction time 30min, instead
Answer temperature 60 C, mixing speed 350r/min.After three valence state vanadium ions are converted into vanadium hydroxide precipitating, hydrogen-oxygen is obtained by filtration
Change vanadium filter cake, is dried for standby.
(5) the vanadium hydroxide filter cake after drying is placed in tube furnace, in N2The lower calcining of protection, nitrogen flow 1L/
Min, heating rate are 5 DEG C/min, and calcination temperature is 700 DEG C, calcination time 3h, obtain vanadium trioxide through calcining and decomposing and produce
Product.
The conversion ratio of vanadium trioxide is 92% in the present embodiment, and the purity of vanadium trioxide is 99.4%.
Embodiment 5
(1) extracting vanadium from stone coal pickle liquor obtains the bone coal that vanadium concentration is 65g/L through ion exchange resin absorption-desorption technique
Vanadium extraction richness vanadium scavenging solution, ion exchange resin therein are D202 macroporous type strong basic anion-exchange resin, and strippant is
The mixed solution of the NaOH and NaCl of the 1.5mol/L ratio mixing of 1:0.5 in molar ratio, the vanadium in pickle liquor is with five valence states
Form exists.
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 1.5 is adjusted with sodium hydroxide or sulfuric acid solution;
(3) zinc powder reduction is added, zinc powder additional amount is 1.5 times of theoretical amount, and reduction temperature is room temperature, and the recovery time is
60min, mixing speed 300r/min, filtering, discard filter residue, obtain three valence state vanadium ion solution;
(4) sodium hydroxide solution is added in three valence state vanadium ion solution and stops to pH value for 5.5, reaction time 30min, instead
Answer temperature 60 C, mixing speed 100r/min.After three valence state vanadium ions are converted into vanadium hydroxide precipitating, hydrogen-oxygen is obtained by filtration
Change vanadium filter cake, is dried for standby.
(5) the vanadium hydroxide filter cake after drying is placed in tube furnace, in N2The lower calcining of protection, nitrogen flow 1L/
Min, heating rate are 5 DEG C/min, and calcination temperature is 600 DEG C, calcination time 5h, obtain vanadium trioxide through calcining and decomposing and produce
Product.
The conversion ratio of vanadium trioxide is 93% in the present embodiment, and the purity of vanadium trioxide is 99.2%.
Embodiment 6
(3) extracting vanadium from stone coal pickle liquor obtains the bone coal that vanadium concentration is 65g/L through ion exchange resin absorption-desorption technique
Vanadium extraction richness vanadium scavenging solution, ion exchange resin therein are D301 macroporous type weak basic anion exchange resin, strippant 2mol/
The mixed solution of the NaOH and NaCl of the L ratio mixing of 1:1.5 in molar ratio, the vanadium in pickle liquor are deposited in the form of five valence states
?.
(4) extracting vanadium from stone coal richness vanadium scavenging solution pH to 2 is adjusted with sodium hydroxide or sulfuric acid solution;
(3) zinc powder reduction is added, zinc powder additional amount is 1.5 times of theoretical amount, and reduction temperature is room temperature, and the recovery time is
50min, mixing speed 400r/min, filtering, discard filter residue, obtain three valence state vanadium ion solution;
(4) sodium hydroxide solution is added in three valence state vanadium ion solution and stops to pH value for 5.5, reaction time 30min, instead
Answer temperature 60 C, mixing speed 200r/min.After three valence state vanadium ions are converted into vanadium hydroxide precipitating, hydrogen-oxygen is obtained by filtration
Change vanadium filter cake, is dried for standby.
(5) the vanadium hydroxide filter cake after drying is placed in tube furnace, in N2The lower calcining of protection, nitrogen flow 1L/
Min, heating rate are 5 DEG C/min, and calcination temperature is 650 DEG C, calcination time 4h, obtain vanadium trioxide through calcining and decomposing and produce
Product.
The conversion ratio of vanadium trioxide is 93.4% in the present embodiment, and the purity of vanadium trioxide is 99.3%.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (7)
1. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor, which comprises the following steps:
(1) extracting vanadium from stone coal pickle liquor obtains extracting vanadium from stone coal richness vanadium scavenging solution through ion exchange resin absorption-desorption technique;
(2) extracting vanadium from stone coal richness vanadium scavenging solution pH to 1~3 is adjusted using sodium hydroxide or sulfuric acid solution, obtains liquid to be restored;
(3) zinc powder reduction is added in the liquid to be restored that step (2) obtains and is stirred, filter residue is filtered and discarded after reduction,
Obtain trivalent vanadium ion solution;
(4) sodium hydroxide solution is added in the trivalent vanadium ion solution that step (3) obtains until pH reaches 5-6, is stirred
It mixes, trivalent vanadium ion occurs precipitation reaction and is converted into vanadium hydroxide, and vanadium hydroxide filter cake is obtained by filtration;
(5) it is placed in tube furnace after the vanadium hydroxide filter cake drying obtained step (4), in N2Lower calcining and decomposing is protected to obtain three
V 2 O product.
2. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor according to claim 1, feature exist
In the vanadium in the extracting vanadium from stone coal richness vanadium scavenging solution exists in the form of five valence states, and vanadium concentration is 30~100g/L.
3. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor according to claim 2, feature exist
In, the adsorbent that step (1) the ion exchange resin absorption-desorption technique uses for polystyrene macroporous type highly basic yin from
Any one in sub-exchange resin or polystyrene macroporous type weak basic anion exchange resin;And the strippant used for
Any one or two kinds in NaOH or NaCl solution are mixed in a certain ratio resulting mixed solution.
4. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor according to claim 3, feature exist
In the concentration control of strippant molar ratio of NaOH and NaCl in 0.5-2mol/L, the mixing strippant matches control
System is in 1:0.5-1.5.
5. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor according to claim 1-4,
It is characterized in that, the additional amount of zinc powder is 1.2~1.5 times of theoretical amount in the step (2), reduction temperature is room temperature, also
The former time is 20~60min, and mixing speed is 100~500r/min.
6. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor according to claim 5, feature exist
In the reaction time of precipitation reaction is 30~90min in the step (3), and reaction temperature is 20~60 DEG C, and mixing speed is
100~500r/min.
7. a kind of method for preparing vanadium trioxide using extracting vanadium from stone coal pickle liquor according to claim 6, feature exist
In N in the step (4)2Flow is 1L/min, and the heating rate of calcining is 5 DEG C/min, 600~900 DEG C of calcination temperature, is forged
The burning time is 1~5h.
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