CN105236483B - A kind of preparation method of potassium metavanadate - Google Patents
A kind of preparation method of potassium metavanadate Download PDFInfo
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- CN105236483B CN105236483B CN201510626272.7A CN201510626272A CN105236483B CN 105236483 B CN105236483 B CN 105236483B CN 201510626272 A CN201510626272 A CN 201510626272A CN 105236483 B CN105236483 B CN 105236483B
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- C01G31/00—Compounds of vanadium
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Abstract
The invention belongs to field of hydrometallurgy, be specifically related to the preparation method of a kind of potassium metavanadate.The preparation method of potassium metavanadate of the present invention, comprises the following steps: a, be added to the water dissolvings by ammonium metavanadate and potassium carbonate, potassium bicarbonate or potassium hydroxide, and the while of microwave heating, evacuation carries out deamination reaction；B, by the solution stirring evaporative crystallization after a step deamination, when the crystal wherein crystallized accounts for the 1/3～1/2 of liquor capacity, add the ethanol of 1/2～1 volume of reaction solution volume, make solid separate out；C, solidliquid mixture b step obtained filter, and with ethanol rinse, obtain potassium metavanadate solid, vacuum drying, to obtain final product.The present invention has that technique is simple, the response time is short, easy to operate；Ethanol can recycle through rectification, and supplies consumption is few；Filtrate can be included into vanadium factory and be sunk ammonium metavanadate recycling, pollutes few；The features such as process energy consumption is low, advantage of lower cost.
Description
Technical field
The invention belongs to field of hydrometallurgy, be specifically related to the preparation method of a kind of potassium metavanadate.
Background technology
Potassium metavanadate is widely used in catalyst, drier, mordant, medical treatment photograph, plant inoculating and corrosion inhibitor etc..
Preparing potassium metavanadate at present and mainly have three kinds of methods, one is to add ammonium metavanadate and potassium hydroxide, ebuillition of heated in water
Remove ammonia so that final ph 8～10, evaporative crystallization obtains potassium metavanadate solid；A kind of method is to dissolve with potassium hydroxide
Ammonium poly-vanadate, after filtration, crystallization obtains potassium metavanadate solid；Another kind of method is toward containing adding appropriate calcium chloride in vanadium leachate
Obtain calcium vanadate precipitation, calcium vanadate is joined in certain density potassium bicarbonate solution and obtain calcium carbonate and potassium metavanadate, filter
After filtrate condensing crystallizing is obtained potassium metavanadate solid.
First method and second method are to prepare the common method of potassium metavanadate, and adding alkali in its technique, to add evanescence of heat ammonia the most time-consuming
5 hours, technique was the longest, consumed energy slightly higher.The third method technological process is relatively long, relatively costly, and potassium metavanadate
A small amount of calcium ion is left in middle meeting, affects the catalytic performance of potassium metavanadate.
Publication No. " CN103395838A ", invention entitled " a kind of high-purity potassium metavanadate and preparation method thereof ", disclose
A kind of to containing vanadium leachate adds desiliconizing agent, remove insoluble matter, obtain low-silicon and low-phosphorous containing vanadium scavenging solution, to low-silicon and low-phosphorous containing vanadium
Scavenging solution adds solubility ammonium salt and carries out precipitation, obtains ammonium vanadate；Vanadic acid is dissolved with potassium hydroxide, potassium carbonate or potassium bicarbonate
Ammonium, removes insoluble matter, obtains potassium vanadate solution, and evaporative crystallization obtains potassium metavanadate.This patent is after adding desiliconizing agent, containing vanadium
The pH of leachate, between 8～10, removes after insoluble matter, the pH containing vanadium scavenging solution between 1.3～3, pH value of solution front and back
Value changes greatly, and needs to consume more acid, and preparation method is complicated, although finally also can obtain potassium metavanadate, but is because
Containing foreign matter of phosphor, silicon, chromium, ferrum, calcium and sodium etc. in solution containing vanadium, the potassium metavanadate finally given still contains the impurity unit of trace
In element, and preparation process remaining ammonium salt cannot recycling, cause the waste of resource.
Publication No. " CN102531055A ", invention entitled " preparation method of sodium metavanadate/potassium metavanadate ", disclose one
Kind sodium vanadium extraction leachate is heated to 80～90 DEG C, according to the mass ratio of Ca:V=1.5:1～2:1 in sodium vanadium extraction leachate
Add calcium chloride saturated solution, stir while keeping under 80～90 DEG C of temperature conditionss, mistake after reaction 30～40min
Filter obtains calcium vanadate solid, and the calcium vanadate solid obtained is washed and filtered, and the calcium vanadate solid after washing is placed in container
In, be subsequently adding a certain amount of sodium bicarbonate or potassium bicarbonate solution, be sufficiently stirred under the conditions of 60～70 DEG C, reaction 30～
Filter after 40min, evaporate, crystallize the sodium metavanadate obtained or potassium metavanadate solution, finally crystal is separated and dried must
To sodium metavanadate or potassium metavanadate.This patent can prepare potassium metavanadate or sodium metavanadate, but, inclined vanadium prepared by the method
In acid sodium or potassium metavanadate, impurity is higher, additionally, while preparation calcium vanadate, phosphorus and silicon also in calcium vanadate, it addition,
When using potassium bicarbonate to carry out anti-molten calcium vanadate, also have substantial amounts of calcium and enter in potassium vanadate solution, cause in potassium metavanadate
Calcium content exceeds standard, and calcium is a kind of important element affecting potassium metavanadate as catalyst activity, and it can cause potassium metavanadate making
Harden during catalyst.
Summary of the invention
For above not enough, the present invention provides one, and technique is simple, supplies consumption is few, low cost, high efficiency, and can realize money
The preparation method of the potassium metavanadate of source recycling.
The preparation method of potassium metavanadate of the present invention, comprises the following steps:
A, according to mol ratio VO3 -:K+=1:1.01～1.05, adds ammonium metavanadate with potassium carbonate, potassium bicarbonate or potassium hydroxide
In water, obtaining the solution that potassium concentration is 1.75～2.53mol/L, microwave heating to 25～70 DEG C, evacuation takes off simultaneously
Ammonia reaction 15～30min；
B, by the solution stirring evaporative crystallization after a step deamination, when the crystal wherein crystallized accounts for the 1/3～1/2 of liquor capacity,
Add the ethanol of 1/2～1 volume of reaction solution volume, make solid separate out；
C, solidliquid mixture b step obtained filter, and with ethanol rinse 2～3 times, obtain potassium metavanadate solid, 50～
It is vacuum dried 4～8h at 70 DEG C, to obtain final product.
The preparation method of potassium metavanadate described above, wherein in b step, evaporative crystallization is more than 80 DEG C.
The preparation method of potassium metavanadate described above, wherein in b step, the volume fraction of ethanol is 95%.
The preparation method of potassium metavanadate described above, wherein in step c, volume fraction of ethanol is 50～70%.
The preparation method of potassium metavanadate described above, wherein filters in step c and can select simple and efficient sucking filtration.
The present invention directly uses ammonium metavanadate, potassium bicarbonate or potassium carbonate or potassium hydroxide to be raw material, in prior art usually
Use potassium hydroxide.Directly using high-purity ammonium metavanadate and potassium bicarbonate or potassium carbonate or potassium hydroxide is raw material, permissible
Reduce the impurity in final potassium metavanadate, improve the purity of potassium metavanadate, and present invention process is simple, low cost, preparation
Potassium metavanadate has the highest value, and raw material can be with recycling, and environmental pollution is little.
Employing microwave heating has the features such as firing rate is fast, thermal loss is little, degassing is the most thorough, easy to operate, the most permissible
Shorten the process time, improve productivity ratio, reduction cost, product quality can be improved again.
The present invention uses microwave heating to make ammonium metavanadate and potassium bicarbonate or potassium carbonate or potassium hydroxide carry out deamination reaction, no
Reaction only can be made comparatively fast to carry out, compared with general technology deamination reaction more than 5 hours, the present invention need only to 15min with
On, substantially reduce generation technique, indirectly save production cost；It addition, utilize microwave energy high, react free of contamination
Feature, can make deamination reaction carry out more thoroughly, and the potassium metavanadate purity of generation is higher, indirectly improves finished product ammonium metavanadate
Yield and purity.
The present invention is to accelerate the reaction of ammonium metavanadate and potassium bicarbonate with microwave and quickly slough ammonia, then by solution evaporation after reaction
Crystallization potassium metavanadate solid is promoted with ethanol after part water.The ammonia wherein generated can decrease resource with recycling
Waste.
Potassium metavanadate prepared by the present invention, according to the potassium metavanadate price about 7.2 ten thousand/ton of 99% purity current on market, 99% is pure
Degree vanadic anhydride 7.5 ten thousand/ton rough calculation, sale potassium metavanadate is relatively sold the vanadic anhydride profit growth of equal vanadium metering and is existed
More than 35%.And the most not producing garbage during potassium metavanadate prepared by the intermediate product ammonium metavanadate of vanadium, environmental pollution is very
Little；Produce potassium metavanadate and can expand the sale kind of vanadium product, expand the range of application of vanadium, increase the total sales volume of vanadium.
There is advantages that
1, technique is simple, the response time is short, easy to operate；
2, ethanol can recycle through rectification, and supplies consumption is few；
3, filtrate can be included into vanadium factory and sunk ammonium metavanadate recycling, pollutes few；
4, process energy consumption is low, advantage of lower cost.
Detailed description of the invention
The preparation method of potassium metavanadate of the present invention, comprises the following steps:
A, according to mol ratio VO3 -:K+=1:1.01～1.05, adds ammonium metavanadate with potassium carbonate, potassium bicarbonate or potassium hydroxide
In water, obtaining the solution that potassium concentration is 1.75～2.53mol/L, microwave heating to 25～70 DEG C, evacuation takes off simultaneously
Ammonia reaction 15～30min；
B, by the solution stirring evaporative crystallization after a step deamination, when the crystal wherein crystallized accounts for the 1/3～1/2 of liquor capacity,
Add the ethanol of 1/2～1 volume of reaction solution volume, make solid separate out；
C, solidliquid mixture b step obtained filter, and with ethanol rinse 2～3 times, obtain potassium metavanadate solid, 50～
It is vacuum dried 4～8h at 70 DEG C, to obtain final product.
The preparation method of potassium metavanadate described above, wherein in b step, evaporative crystallization is more than 80 DEG C.
The preparation method of potassium metavanadate described above, wherein in b step, the volume fraction of ethanol is 95%.
The preparation method of potassium metavanadate described above, wherein in step c, volume fraction of ethanol is 50～70%.
The preparation method of potassium metavanadate described above, wherein filters in step c and can select simple and efficient sucking filtration.
The present invention directly uses ammonium metavanadate, potassium bicarbonate or potassium carbonate or potassium hydroxide to be raw material, in prior art usually
Use potassium hydroxide.Directly using high-purity ammonium metavanadate and potassium bicarbonate or potassium carbonate or potassium hydroxide is raw material, permissible
Reduce the impurity in final potassium metavanadate, improve the purity of potassium metavanadate, and present invention process is simple, low cost, preparation
Potassium metavanadate has the highest value, and raw material can be with recycling, and environmental pollution is little.
Employing microwave heating has the features such as firing rate is fast, thermal loss is little, degassing is the most thorough, easy to operate, the most permissible
Shorten the process time, improve productivity ratio, reduction cost, product quality can be improved again.
The present invention uses microwave heating to make ammonium metavanadate and potassium bicarbonate or potassium carbonate or potassium hydroxide carry out deamination reaction, no
Reaction only can be made comparatively fast to carry out, compared with general technology deamination reaction more than 5 hours, the present invention need only to 15min with
On, substantially reduce generation technique, indirectly save production cost；It addition, utilize microwave energy high, react free of contamination
Feature, can make deamination reaction carry out more thoroughly, and the potassium metavanadate purity of generation is higher, indirectly improves finished product ammonium metavanadate
Yield and purity.
The present invention is to accelerate the reaction of ammonium metavanadate and potassium bicarbonate with microwave and quickly slough ammonia, then by solution evaporation after reaction
Crystallization potassium metavanadate solid is promoted with ethanol after part water.The ammonia wherein generated can decrease resource with recycling
Waste.
Potassium metavanadate prepared by the present invention, according to the potassium metavanadate price about 7.2 ten thousand/ton of 99% purity current on market, 99% is pure
Degree vanadic anhydride 7.5 ten thousand/ton rough calculation, sale potassium metavanadate is relatively sold the vanadic anhydride profit growth of equal vanadium metering and is existed
More than 35%.And the most not producing garbage during potassium metavanadate prepared by the intermediate product ammonium metavanadate of vanadium, environmental pollution is very
Little；Produce potassium metavanadate and can expand the sale kind of vanadium product, expand the range of application of vanadium, increase the total sales volume of vanadium.
Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described, the most therefore limits the present invention to institute
Among the scope of embodiments stated.
Embodiment 1
117g ammonium metavanadate and 101.1g potassium bicarbonate are dissolved in the water of 400ml, microwave heating evacuation deamination gas simultaneously
Reacting 15 minutes, temperature controls between room temperature to 70 DEG C；By reacted solution stirring evaporative crystallization；Solution crystallizes institute
When accounting for liquor capacity about 1/3, the ethanol adding reaction solution volume equal volume makes potassium metavanadate solid separate out；Sucking filtration, and use
A small amount of volume fraction is the ethanol solution drip washing 2 times of 50%, and the potassium metavanadate solid obtained is taken out very in 50 DEG C of vacuum drying ovens
Empty dry, obtain potassium metavanadate product, potassium metavanadate yield 82.7%；Filtrate and drip washing filtrate with rectifying column rectification obtain ethanol and
Rectification mother solution, ethanol can Reusability, in rectification mother solution add ammonium salt sink ammonium metavanadate recycle, the overall recovery of vanadium exists
98.4%.
Embodiment 2
117g ammonium metavanadate and 103g potassium bicarbonate being dissolved in the water of 500ml, microwave heating evacuation deamination gas simultaneously is anti-
Answering 20 minutes, temperature controls between room temperature to 70 DEG C；By reacted solution stirring evaporative crystallization；In solution, crystallization is shared
During liquor capacity about 2/5, the ethanol adding reaction solution volume 2/3 volume makes potassium metavanadate solid separate out；Sucking filtration, and with a small amount of
The ethanol solution drip washing that volume fraction is 60% 2 times, the potassium metavanadate solid obtained evacuation in 60 DEG C of vacuum drying ovens is done
Dry, obtain potassium metavanadate product, potassium metavanadate yield 85.1%；Filtrate and drip washing filtrate obtain ethanol and rectification with rectifying column rectification
Mother solution, ethanol can Reusability, in rectification mother solution add ammonium salt sink ammonium metavanadate recycle, the overall recovery of vanadium is 98.8%.
Embodiment 3
117g ammonium metavanadate and 105g potassium bicarbonate being dissolved in the water of 600ml, microwave heating evacuation deamination gas simultaneously is anti-
Answering 25 minutes, temperature controls between room temperature to 70 DEG C；By reacted solution stirring evaporative crystallization；In solution, crystallization is shared
During liquor capacity about 1/2, the ethanol adding reaction solution volume 1/2 volume makes potassium metavanadate solid separate out；Sucking filtration, and with a small amount of
The ethanol solution drip washing that volume fraction is 70% 2 times, the potassium metavanadate solid obtained evacuation in 70 DEG C of vacuum drying ovens is done
Dry, obtain potassium metavanadate product, potassium metavanadate yield 85.2%；Filtrate and drip washing filtrate obtain ethanol and rectification with rectifying column rectification
Mother solution, ethanol can Reusability, in rectification mother solution add ammonium salt sink ammonium metavanadate recycle, the overall recovery of vanadium is 99.0%.
Claims (5)
1. the preparation method of potassium metavanadate, it is characterised in that: comprise the following steps:
A, according to mol ratio VO3 -:K+=1:1.01～1.05, adds ammonium metavanadate with potassium carbonate, potassium bicarbonate or potassium hydroxide
In water, obtaining the solution that potassium concentration is 1.75～2.53mol/L, microwave heating to 25～70 DEG C, evacuation takes off simultaneously
Ammonia reaction 15～30min；
B, by the solution stirring evaporative crystallization after a step deamination, when the crystal wherein crystallized accounts for the 1/3～1/2 of liquor capacity,
Add the ethanol of 1/2～1 volume of reaction solution volume, make solid separate out；
C, solidliquid mixture b step obtained filter, and with ethanol rinse 2～3 times, obtain potassium metavanadate solid, 50～
It is vacuum dried 4～8h at 70 DEG C, to obtain final product.
The preparation method of potassium metavanadate the most according to claim 1, it is characterised in that: in b step, evaporative crystallization is 80
More than DEG C.
The preparation method of potassium metavanadate the most according to claim 1, it is characterised in that: in b step, the volume fraction of ethanol is
95%.
The preparation method of potassium metavanadate the most according to claim 1, it is characterised in that: in step c volume fraction of ethanol be 50～
70%.
The preparation method of potassium metavanadate the most according to claim 1, it is characterised in that: step c is filtered into sucking filtration.
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| "KVO3的制备和性质研究";关鲁雄等;《矿冶工程》;19970930;第17卷(第3期);第51页第1.1和1.2部分，第52页表2 * |
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