CN105821222A - Method for recovering sodium and/or potassium and separating vanadium from sodium orthovanadate and/or potassium orthovanadate - Google Patents
Method for recovering sodium and/or potassium and separating vanadium from sodium orthovanadate and/or potassium orthovanadate Download PDFInfo
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- CN105821222A CN105821222A CN201610182150.8A CN201610182150A CN105821222A CN 105821222 A CN105821222 A CN 105821222A CN 201610182150 A CN201610182150 A CN 201610182150A CN 105821222 A CN105821222 A CN 105821222A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention provides a method for recovering sodium and/or potassium and separating vanadium from sodium orthovanadate and/or potassium orthovanadate. The method includes the steps that a sodium orthovanadate solution and/or a potassium orthovanadate solution and CO2 react under the conditions that the temperature is 50-150 DEG C and the pressure is 1.0-3.0 MPa, then solid-liquid separation is carried out to obtain carbonate and/or bicarbonate and a vanadium-containing solution, and positive ions in the carbonate and the bicarbonate are sodium ions and/or potassium ions. By means of the method, the vanadium recovery rate is high (higher than 98%), and the technological process is short, easy to operate, simple and good in safety; in the separation process, sodium and/or potassium in the sodium orthovanadate and/or the potassium orthovanadate are/is converted into crystals or alkaline solutions so as to be recycled.
Description
Technical field
The invention belongs to vanadium field of chemical metallurgical technology, relate to one and return from sodium vanadate and/or positive potassium vanadate
Take in and/or the method for potassium separation vanadium, particularly relate to one and utilize sodium vanadate solution and/or positive potassium vanadate solution
With CO2Reaction reclaim sodium and/or the method for potassium separation vanadium in vanadate.
Background technology
In view of the successful application of sodium system sub-molten salt chromic salts cleaning procedure, Chinese Academy Of Sciences Process Engineering Research Institute
Successfully develop the NaOH vanadium slag cleaning new technology as reaction medium.For intermediate product vanadic acid sodium
High level transforms into a primary study direction.In sub-molten salt method vanadium extraction leachate, vanadium is mainly with positive vanadic acid root
Form exists, and the intermediate product crystallized out is sodium vanadate crystal;And tradition mainly the depositing of vanadium slag leachate vanadium
It is many vanadic acid root in mode, different according to the precipitant used, it is divided into calcium precipitation, molysite deposition, hydrolysis
Precipitation and ammonium salt precipitation.The main flow of sodium process for extracting vanadium is to add ammonium sulfate/ammonium chloride in vanadium solution,
Generating ammonium poly-vanadate, then high-temperature calcination becomes vanadic anhydride.The ammonium process of sinking can produce substantial amounts of high salinity,
Nitrogen-containing wastewater, unit vanadium product (in terms of vanadic anhydride) waste water generation amount is about 40 tons, severe contamination
Environment;Ton vanadium chrome waste water treatment cost, at about 3000 yuan, administers cost big.
CN101157478A discloses the preparation method of a kind of ammonium poly-vanadate, with traditional sodium roasting-water logging
What technique produced is raw material containing many sodium vanadate solutions, first makes vanadium generate vanadic acid with calcium chloride or the calcium nitrate of addition
Calcium, then turns molten with ammonium hydrogen carbonate, and vanadium enters solution, and calcium generates the calcium carbonate of more indissoluble, the vanadium after separation
Liquid sulfur acid for adjusting pH, precipitation obtains ammonium poly-vanadate.This technique compared with traditional handicraft, ammonia in vanadium wastewater
Content reduces, but there is the emission problem of ammonia nitrogen waste water.
CN101723455A discloses and prepares sodium metavanadate with many vanadic acid sodiums, is first adjusted by sodium vanadium extraction leachate
Joint pH value, then ebuillition of heated generates many vanadic acid sodiums solid, dissolves many vanadic acid sodiums with sodium hydroxide and produces
Sodium metavanadate.The shortcoming of the method is that precipitation process control difficulties is big and vanadium yield is low.
Summary of the invention
The deficiency existed for prior art, it is an object of the invention to provide a kind of from sodium vanadate and/or just
Reclaiming sodium and/or the method for potassium separation vanadium in potassium vanadate, the response rate of described method vanadium and sodium and/or potassium is high,
Technological process is short, it is easy to operation, simple and safety is good.
For reaching this purpose, the present invention by the following technical solutions:
A kind of recovery sodium and/or the method for potassium separation vanadium, described method from sodium vanadate and/or positive potassium vanadate
For: by sodium vanadate solution and/or positive potassium vanadate solution and CO2Being 50-150 DEG C in temperature, pressure is
React under 1.0-3.0MPa, solid-liquid separation afterwards, obtain carbonate and/or bicarbonate and containing vanadium solution,
Cation in described carbonate and bicarbonate is sodium ion and/or potassium ion.
The present invention uses sodium vanadate solution and/or positive potassium vanadate solution and CO2Reaction reclaim sodium and/or potassium,
Being separated by vanadium, the carbonate obtained and/or bicarbonate can be used as the additive of Leaching of Vanadium from Vanadium slag roasting simultaneously
Carrying out recycling, obtain can obtain containing the red cake of vanadium containing vanadium in vanadium solution after the conventional treatment of this area.
Described method technique is simple, and flow process is short, easy and simple to handle, and the response rate of vanadium is up to more than 98%.
Described solid-liquid separation is operation commonly used in the art, and described solid-liquid separation can reach in product
The purpose that separates with liquid of solid, typical but non-limiting solid-liquid separation method is as filtered or centrifugal
Separate.
Described vanadate solution is vanadium extraction leachate.Described method is particularly suited in Leaching of Vanadium from Vanadium slag technique processing
Vanadium slag leachate, it is possible to by vanadium high efficiente callback.
In described sodium vanadate solution, the concentration of vanadium is 20-50g/L, as 22g/L, 25g/L, 28g/L, 30g/L,
32g/L, 35g/L, 38g/L, 40g/L, 42g/L, 45g/L or 48g/L etc., preferably 22.71-45.56g/L;
The concentration of sodium is 27-68g/L, as 30g/L, 32g/L, 35g/L, 38g/L, 40g/L, 45g/L, 50g/L,
55g/L, 60g/L or 65g/L etc., preferably 30.73-61.64g/L.
In described positive potassium vanadate solution, the concentration of vanadium is 20-50g/L, as 22g/L, 25g/L, 28g/L, 30g/L,
32g/L, 35g/L, 38g/L, 40g/L, 42g/L, 45g/L or 48g/L etc., preferably 22.71-45.56g/L,
The concentration of potassium is 45-115g/L, as 50g/L, 55g/L, 60g/L, 70g/L, 80g/L, 90g/L, 100
G/L, 105g/L or 110g/L etc..
The temperature of described reaction is 50-150 DEG C, as 55 DEG C, 58 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C,
82℃、83、85℃、90℃、95℃、100℃、105℃、110℃、115℃、120℃、125℃、
130 DEG C, 135 DEG C, 140 DEG C or 145 DEG C etc., preferably 90-120 DEG C.
The pressure of described reaction is 1.0-3.0MPa, as 1.2MPa, 1.5MPa, 1.8MPa, 2.0MPa,
2.2MPa, 2.5MPa or 2.8MPa etc., preferably 1.2-2.5MPa.
Described sodium vanadate solution and/or just potassium vanadate solution and CO2Must could react raw with this understanding
Become carbonate and/or bicarbonate and containing vanadium solution.
The time of described reaction is 0.5-6h, as 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h,
5h or 5.5h etc., preferably 1-6h.
Described method also includes: will contain vanadium solution and regulate pH value in a heated condition, obtains containing the red cake of vanadium.
The described Crack cause containing the red cake of vanadium is: along with the increase of solution acidity, and vanadic acid root separates out with the form of vanadic acid,
Form the red cake Han vanadium.The described further roasting of red cake containing vanadium can obtain vanadic anhydride.Utilize containing vanadium solution system
The technology that the standby red cake containing vanadium is known to the skilled person.Those skilled in the art add described in can will readily appreciate that
The temperature of heat and concrete pH value.
Described method also includes: described sodium carbonate and/or sodium bicarbonate crystal are reacted with aqua calcis,
Obtain sodium hydroxide solution and/or potassium hydroxide solution.Sodium hydroxide solution and/or potassium hydroxide solution can be used for
The alkaline media of Leaching of Vanadium from Vanadium slag technique, has recycled the sodium in sodium vanadate and/or positive potassium vanadate and/or potassium.
As preferred technical scheme, described method comprises the steps:
(1) in sodium vanadate solution and/or positive potassium vanadate solution, it is passed through CO2, it is 50-150 DEG C in temperature,
Pressure is reaction 0.5-6h under the conditions of 1.0-3.0MPa, obtains product, wherein, in sodium vanadate solution
The concentration of vanadium is 20-50g/L, and the concentration of sodium is 27-68g/L, and in positive potassium vanadate solution, the concentration of vanadium is
20-50g/L, the concentration of potassium is 45-115g/L;
(2) product is carried out solid-liquid separation and obtains carbonate and/or bicarbonate crystal and containing vanadium solution,
Cation in described carbonate and bicarbonate is sodium ion and/or potassium ion;
(3) sodium carbonate and/or sodium bicarbonate crystal are reacted with aqua calcis, obtain sodium hydroxide molten
Liquid and/or potassium hydroxide solution;Vanadium solution will be contained regulate pH value in a heated condition and obtain containing the red cake of vanadium.
Compared with prior art, the invention have the benefit that
What the present invention provided reclaims sodium and/or the method for potassium separation vanadium, vanadium from sodium vanadate and/or positive potassium vanadate
The response rate high (response rate of vanadium is more than 98%), technological process is short, easily operated, simple and safety is good;
It addition, in separation process, the metal cation in positive vanadate can be transformed into carbonate and/or bicarbonate
Salt crystal or strong base solution, and then it is applied to the additive of Leaching of Vanadium from Vanadium slag roasting, it is recycled utilization, it is possible to
Reduce the cost containing vanadium raw materials vanadium extraction.
Detailed description of the invention
Technical scheme is further illustrated below by detailed description of the invention.
Embodiment 1:
A kind of method reclaiming sodium separation vanadium from positive sodium vanadate solution, described method comprises the steps:
(1) dispensing: mixed with water by sodium vanadate, stirs, and being made into vanadium concentration is 28.56g/L, sodium
The sodium vanadate solution that concentration is 38.13g/L;
(2) reaction: be passed through CO in sodium vanadate solution2, it is 90 DEG C in temperature, pressure is 1.2MPa
Lower reaction 3h, obtains product;
(3) filter: product is filtered, obtain sodium carbonate and/or sodium bicarbonate crystal and containing vanadium solution;
(4) causticization: sodium carbonate/bicarbonate crystal is reacted with aqua calcis, after reaction terminates,
It is filtrated to get calcium carbonate and sodium hydroxide solution, recycles the sodium in sodium vanadate;
(5) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, be filtrated to get
Containing solution after the red cake of vanadium and vanadium extraction, containing V=0.34g/L, Na=7.40g/L in solution after vanadium extraction.
Step (4) and step (5) are without sequencing.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 99.04%;The response rate of sodium is 84.47%.
Embodiment 2:
A kind of method reclaiming sodium separation vanadium from positive sodium vanadate solution, described method comprises the steps:
(1) dispensing: mixed with water by sodium vanadate, stirs, and being made into vanadium concentration is 45.56g/L, sodium
The sodium vanadate solution that concentration is 61.64g/L;
(2) reaction: be passed through CO in sodium vanadate solution2, it is 120 DEG C in temperature, pressure is 2.5MPa
Lower reaction 1.5h, obtains product;
(3) filter: product is filtered, obtain sodium carbonate and/or sodium bicarbonate crystal and containing vanadium solution,
Recycle the sodium in sodium vanadate;
(4) precipitation: regulate pH value containing vanadium solution in a heated condition, afterwards, filter, obtain containing vanadium red
Solution after cake and vanadium extraction, containing V=0.41g/L, Na=11.53g/L in solution after vanadium extraction.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 99.3%;The response rate of sodium is 85.97%.
Embodiment 3:
A kind of method reclaiming sodium separation vanadium from positive sodium vanadate solution, described method comprises the steps:
(1) dispensing: mixed with water by sodium vanadate, stirs, and being made into vanadium concentration is 35.08g/L, sodium
The sodium vanadate solution that concentration is 47.46g/L;
(2) reaction: be passed through CO in sodium vanadate solution2, it is 110 DEG C in temperature, pressure is 2.0MPa
Under carry out react 1h, obtain product;
(3) filter: product is filtered, obtain sodium carbonate and/or sodium bicarbonate crystal and containing vanadium solution,
Recycle the sodium in sodium vanadate;
(4) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, be filtrated to get
Containing solution after vanadium red cake product and vanadium extraction, containing V=0.53g/L, Na=9.11g/L in solution after vanadium extraction.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 98.8%;The response rate of sodium is 85.03%.
Embodiment 4:
A kind of method reclaiming sodium separation vanadium from positive sodium vanadate solution, described method comprises the steps:
(1) dispensing: mixed with water by sodium vanadate, stirs, and being made into vanadium concentration is 22.71g/L, sodium
The sodium vanadate solution that concentration is 30.73g/L;
(2) reaction: be passed through CO in sodium vanadate solution2, it is 105 DEG C in temperature, pressure is 1.5MPa
Lower reaction 6h, obtains product;
(3) filter: product is filtered, obtain sodium carbonate and/or sodium bicarbonate crystal and containing vanadium solution;
(4) causticization: sodium carbonate/bicarbonate crystal is reacted with aqua calcis, after reaction terminates,
Filtering, obtain calcium carbonate and sodium hydroxide solution, sodium hydroxide solution returns the alkali for Leaching of Vanadium from Vanadium slag technique
Medium, has recycled the sodium in sodium vanadate;
(5) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, filters,
To containing solution after the red cake of vanadium and vanadium extraction, containing V=0.48g/L, Na=5.50g/L in solution after vanadium extraction.
Step (4) and step (5) are without sequencing.
After testing, calculate, vanadium conversion ratio 98.56% in the present embodiment;The response rate of sodium is 87.82%.
Embodiment 5
A kind of method reclaiming sodium separation vanadium from positive sodium vanadate solution, described method comprises the steps:
(1) dispensing: mixed with water by sodium vanadate, stirs, and being made into vanadium concentration is 20g/L, sodium
Concentration is the sodium vanadate solution of 27g/L;
(2) reaction: be passed through CO in sodium vanadate solution2, it is 50 DEG C in temperature, pressure is 3.0MPa
Lower reaction 5.5h, obtains product;
(3) filter: product is filtered, obtain sodium carbonate and/or sodium bicarbonate crystal and containing vanadium solution;
(4) causticization: sodium carbonate/bicarbonate crystal is reacted with aqua calcis, after reaction terminates,
Filtering, obtain calcium carbonate and sodium hydroxide solution, sodium hydroxide solution returns the alkali for Leaching of Vanadium from Vanadium slag technique
Medium, has recycled the sodium in sodium vanadate;
(5) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, filters,
To containing solution after the red cake of vanadium and vanadium extraction, containing V=0.50g/L, Na=4.97g/L in solution after vanadium extraction.
Step (4) and step (5) are without sequencing.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 98.1%;The response rate of sodium is 82.6%.
Embodiment 6
A kind of method reclaiming sodium separation vanadium from positive sodium vanadate solution, described method comprises the steps:
(1) dispensing: mixed with water by sodium vanadate, stirs, and being made into vanadium concentration is 50g/L, sodium
Concentration is the sodium vanadate solution of 68g/L;
(2) reaction: be passed through CO in sodium vanadate solution2, it is 150 DEG C in temperature, pressure is 1.0MPa
Lower reaction 0.5h, obtains product;
(3) filter: product is filtered, obtain sodium carbonate and/or sodium bicarbonate crystal and containing vanadium solution,
Recycle the sodium in sodium vanadate;
(4) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, be filtrated to get
Containing solution after vanadium red cake product and vanadium extraction, containing V=0.6g/L, Na=12.78g/L in solution after vanadium extraction.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 98.8%;The response rate of sodium is 83.2%.
Embodiment 7
A kind of method reclaiming potassium separation vanadium from positive vitriol acid potassium solution, described method comprises the steps:
(1) dispensing: mixed with water by positive potassium vanadate, stir, being made into vanadium concentration is 25g/L, potassium
Concentration is the positive potassium vanadate solution of 45g/L;
(2) reaction: be passed through CO in positive potassium vanadate solution2, it is 105 DEG C in temperature, pressure is 2.5MPa
Under carry out react 3h, obtain product;
(3) filter: product is filtered, obtain potassium carbonate and/or potassium bicarbonate crystal and containing vanadium solution,
Recycle the potassium in positive potassium vanadate;
(4) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, be filtrated to get
Containing solution after vanadium red cake product and vanadium extraction, containing V=0.55g/L, K=8.73g/L in solution after vanadium extraction.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 98.3%;The response rate of potassium is 82.6%.
Embodiment 8
A kind of method reclaiming potassium separation vanadium from positive vitriol acid potassium solution, described method comprises the steps:
(1) dispensing: mixed with water by positive vitriol acid potassium, stir, being made into vanadium concentration is 50g/L, potassium
Concentration is the positive vitriol acid potassium solution of 115g/L;
(2) reaction: be passed through CO in positive vitriol acid potassium solution2, it is 85 DEG C in temperature, pressure is 1.8MPa
Lower reaction 2.5h, obtains product;
(3) filter: product is filtered, obtain potassium carbonate and/or potassium bicarbonate crystal and containing vanadium solution;
(4) causticization: potassium carbonate/potassium bicarbonate crystal is reacted with aqua calcis, after reaction terminates,
It is filtrated to get calcium carbonate and potassium hydroxide solution, recycles the potassium in positive potassium vanadate;
(5) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, be filtrated to get
Containing solution after vanadium red cake product and vanadium extraction, containing V=0.625g/L, K=21.26g/L in solution after vanadium extraction.
Step (4) and step (5) are without sequencing.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 98.55%;The response rate of sodium is 81.91%.
Embodiment 9
A kind of method reclaiming potassium separation vanadium from positive vitriol acid potassium solution, described method comprises the steps:
(1) dispensing: mixed with water by positive vitriol acid potassium, stir, being made into vanadium concentration is 20g/L, and potassium is dense
Degree is the positive vitriol acid potassium solution of 45g/L;
(2) reaction: be passed through CO in positive vitriol acid potassium solution2, it is 85 DEG C in temperature, pressure is 1.8MPa
Lower reaction 4h, obtains product;
(3) filter: product is filtered, obtain potassium carbonate and/or potassium bicarbonate crystal and containing vanadium solution;
(4) precipitation: carry out pH regulator containing vanadium solution in a heated condition, after reaction terminates, be filtrated to get
Containing solution after vanadium red cake product and vanadium extraction, containing V=0.44g/L, K=8.31g/L in solution after vanadium extraction.
After testing, calculating, in the present embodiment, vanadium conversion ratio is 98.2%;The response rate of potassium is 81.53%.
Comparative example 1
A kind of sodium process for extracting vanadium reclaims the method that sodium salt cleaning produces vanadium product, and described method removes reaction temperature
Being 55 DEG C, reaction pressure is that outside 3.2MPa, remaining is same as in Example 1.
After testing, calculating, in the present embodiment, vanadium comprehensive yield is 77.08%;The response rate of sodium is 62.39%.
Comparative example 2
A kind of sodium process for extracting vanadium reclaims the method that sodium salt cleaning produces vanadium product, and described method removes reaction temperature
Being 155 DEG C, reaction pressure is that outside 0.8MPa, remaining is same as in Example 1.
After testing, calculating, in the present embodiment, vanadium comprehensive yield is 75.69%;The response rate of sodium is 61.75%.
Applicant states, the foregoing is only the detailed description of the invention of the present invention, but protection scope of the present invention
Being not limited thereto, person of ordinary skill in the field is it will be clearly understood that any skill belonging to the art
Art personnel in the technical scope that the invention discloses, the change that can readily occur in or replacement, all fall within the present invention
Protection domain and open within the scope of.
Claims (10)
1. from sodium vanadate and/or positive potassium vanadate, reclaim sodium and/or a method for potassium separation vanadium, its feature
Being, described method is: by sodium vanadate solution and/or positive potassium vanadate solution and CO2In temperature it is
50-150 DEG C, pressure is to react under 1.0-3.0MPa, and solid-liquid separation afterwards obtains carbonate and/or bicarbonate
Salt and containing vanadium solution, the cation in described carbonate and bicarbonate is sodium ion and/or potassium ion.
Method the most according to claim 1, it is characterised in that described sodium vanadate solution and/or just
Potassium vanadate solution is vanadium extraction leachate.
Method the most according to claim 1 and 2, it is characterised in that vanadium in described sodium vanadate solution
Concentration be 20-50g/L, preferably 22.71-45.56g/L, the concentration of sodium is 27-68g/L, be preferably
30.73-61.64g/L。
4. according to the method one of claim 1-3 Suo Shu, it is characterised in that in described positive potassium vanadate solution,
The concentration of vanadium is 20-50g/L, preferably 22.71-45.56g/L, and the concentration of potassium is 45-115g/L.
5. according to the method one of claim 1-4 Suo Shu, it is characterised in that the temperature of described reaction is
90-120℃。
6. according to the method one of claim 1-5 Suo Shu, it is characterised in that the pressure of described reaction is
1.2-2.5MPa。
7. according to the method one of claim 1-6 Suo Shu, it is characterised in that the time of described reaction is
0.5-6h, preferably 1-6h.
8. according to the method one of claim 1-7 Suo Shu, it is characterised in that described method also includes: will
Regulate pH value containing vanadium solution in a heated condition, obtain containing the red cake of vanadium.
9. according to the method one of claim 1-8 Suo Shu, it is characterised in that described method also includes: will
Described carbonate and/or bicarbonate crystal react with aqua calcis, obtain sodium hydroxide solution and/or hydrogen
Potassium oxide solution.
10. according to the method one of claim 1-9 Suo Shu, it is characterised in that described method includes as follows
Step:
(1) in sodium vanadate solution and/or positive potassium vanadate solution, it is passed through CO2, it is 50-150 DEG C in temperature,
Pressure is reaction 0.5-6h under the conditions of 1.0-3.0MPa, obtains product, wherein, in sodium vanadate solution
The concentration of vanadium is 20-50g/L, and the concentration of sodium is 27-68g/L, and in positive potassium vanadate solution, the concentration of vanadium is
20-50g/L, the concentration of potassium is 45-115g/L;
(2) product is carried out solid-liquid separation and obtains carbonate and/or bicarbonate crystal and containing vanadium solution,
Cation in described carbonate and bicarbonate is sodium ion and/or potassium ion;
(3) sodium carbonate and/or sodium bicarbonate crystal are reacted with aqua calcis, obtain sodium hydroxide molten
Liquid and/or potassium hydroxide solution;Vanadium solution will be contained regulate pH value in a heated condition and obtain containing the red cake of vanadium.
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