CN105256137B - A kind of method of hydrolytic precipitation containing vanadium solution - Google Patents
A kind of method of hydrolytic precipitation containing vanadium solution Download PDFInfo
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- CN105256137B CN105256137B CN201510766044.XA CN201510766044A CN105256137B CN 105256137 B CN105256137 B CN 105256137B CN 201510766044 A CN201510766044 A CN 201510766044A CN 105256137 B CN105256137 B CN 105256137B
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- vanadium solution
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Abstract
The invention belongs to field of hydrometallurgy, and in particular to a kind of method of hydrolytic precipitation containing vanadium solution.A kind of method of the hydrolytic precipitation containing vanadium solution of the present invention, includes the following steps：A, reaction tube pre-processes：The pipe of an acid resistance material is taken, wherein filling vanadic anhydride；B, it is pre-processed containing vanadium solution：Pending containing vanadium solution is preheated, 95~100 DEG C is heated to, adjusts the pH containing vanadium solution；C, it filters and precipitates containing vanadium solution：Contain vanadium solution from bottom to up by pretreated, countercurrently by the reaction tube after a step process, and reaction tube lower half portion is heated, top half is cooled down, and obtains vanadic anhydride crystal.The method of the present invention by increasing filter pressure, pre-add crystal seed, the setting effective means such as differential temperature band, is carried out at the same time the filtering of precipitation process and ammonium poly-vanadate, and make obtained vanadium oxide particles size with unanimously.
Description
Technical field
The invention belongs to field of hydrometallurgy, and in particular to a kind of method of hydrolytic precipitation containing vanadium solution.
Background technology
Converter Vanadium-bearing Slag in metallurgical production enterprise is to produce the most basic raw material of vanadic anhydride product.Process Converter Vanadium-bearing Slag
Common method be that addition calcination object carries out oxidizing roasting, then the acidic leaching process that continues, in leachate containing 30~
The sodium vanadates of 40g/L vanadic anhydride meters, calcium vanadate, manganese vanadate and other impurity ionic salt compound.
It is well-known hydrolysis precipitation method be：Adjust solution ph 1.5~1.8, the heated solution under conditions of stirring
To 95~98 DEG C, precipitate 40~90 minutes.Tune is sour, during heated solution, the precipitation that vanadic anhydride hydrolytic process is formed
The stability of object can reduce, and impurity cationic can be entered under Coprecipitation in the structure of compound precipitates.
The shortcomings that above method is that the sedimentation time is longer, and residual vanadium amount is more in upper liquid, and sediment physical property is not up to standard,
Also there is the problems such as carefully scattered property is high, filterability is difficult, water content is higher, and impurity content is higher in sediment.
A kind of well-known plus seed Mtehod for hydrolytic precitpitation, five oxidations in the quality and solution of added precipitation seed
Two content of vanadium reach 1:1；During above-mentioned seeded precipitation, the impossible inherently shadow of solid phase crystal seed of introduced precipitation process
Ring sedimentation time, precipitation rate, precipitated products quality.The shortcomings that method, still has, and the sedimentation time is longer, residual vanadium rate in upper liquid
Higher, sediment physical property is not up to standard, and impurity content is higher in sediment.
Also a kind of well known Mtehod for hydrolytic precitpitation includes presetting acid, continuous steam heating, intermediate processing, still using upper
State invention prototype.Its inventive method refers to be, heats steam and heating liquid interacts, due to hot-spot, hole
Phenomenon forms a large amount of nucleus, by the specific surface area of thin scattered solid prosperity formed in crystallization process, so as to cause precipitation
Process occurs very rapid.Under these conditions, settling velocity shortens to 3~5 minutes, while residual vanadium amount is also subtracted in solution
It is few.But this method there is also it is inevitable the shortcomings that, sediment physical property it is completely not up to standard (carefully dissipate property：Particle size is 5
~10 microns or even smaller), very sad filter, solution moisture content is very high (generally reaching 100%), and impurity content is high.
Invention content
In view of the shortcomings of the prior art, the technical problems to be solved by the invention are to provide a kind of precipitation crystallinity height, particle
Uniformly, the few hydrolysis precipitation method of impurity content.
A kind of method of the hydrolytic precipitation containing vanadium solution of the present invention, includes the following steps：
A, reaction tube pre-processes：The pipe of acid resistance material is taken, wherein filling vanadic anhydride；
B, it is pre-processed containing vanadium solution：Pending containing vanadium solution is preheated, is heated to 95~100 DEG C, adjusting contains
The pH of vanadium solution to 1.5~2；Wherein, according to solid-to-liquid ratio, the vanadic anhydride filled in reaction tube:It is pending containing vanadium solution=
0.5~2g:1L；
C, it filters and precipitates containing vanadium solution：By b step it is pretreated containing vanadium solution from bottom to up, countercurrently by a steps at
Reaction tube after reason, and being heated to reaction tube lower half portion, make by the temperature containing vanadium solution of reaction tube for 101~
110 DEG C, reaction tube top half is cooled down, be cooled to 30~40 DEG C；Flow velocity containing vanadium solution is 0.1~1L/ (h
cm2), contain vanadium solution after obtaining containing the vanadic anhydride crystal and hydrolytic precipitation in vanadium solution.
Method of a kind of hydrolytic precipitation containing vanadium solution described above, reaction tube is acid resistance stainless steel wherein in a steps
Matter.
Method of a kind of hydrolytic precipitation containing vanadium solution described above, the grain size of vanadic anhydride wherein filled in a steps
For 15~30um.
Further, technical solution more preferably, method of a kind of hydrolytic precipitation containing vanadium solution described above, wherein
According to solid-to-liquid ratio in b step, the vanadic anhydride preferably filled in reaction tube:It is pending to contain vanadium solution=0.5~0.9g:
1L。
Method of a kind of hydrolytic precipitation containing vanadium solution described above adjusts pH value and uses volume ratio as 1 wherein in b step:1
Sulfuric acid.
Further, in order to enable preferably to filter precipitation containing vanadium solution, using pumping at the top of reaction tube wherein in step c
Filter pump is filtered to containing vanadium solution.
Further, in order to enable preferably to crystallize precipitation, while cooling agent is environmentally safe containing vanadium solution, wherein
Reaction tube top half is cooled down using the air of atomization in step c.
Further, technical solution more preferably, method of a kind of hydrolytic precipitation containing vanadium solution described above, c steps
The filtering rate containing vanadium solution is preferably 0.2L/ (hcm in rapid2)。
Method of a kind of hydrolytic precipitation containing vanadium solution described above, wherein the vanadic anhydride crystal obtained after precipitation filtering
Grain size is 180~500um, pentoxide content >=97% in crystal, rate >=99% of precipitation containing vanadium solution.
A kind of method of the hydrolytic precipitation containing vanadium solution of the present invention, by increasing filter pressure, pre-add crystal seed, setting difference temperature
The effective means such as degree band, are carried out at the same time the filtering of precipitation process and ammonium poly-vanadate, and make obtained vanadic anhydride
Grain size with unanimously.
Specific embodiment
A kind of method of the hydrolytic precipitation containing vanadium solution of the present invention, includes the following steps：
A, reaction tube pre-processes：The pipe of acid resistance material is taken, wherein filling vanadic anhydride；
B, it is pre-processed containing vanadium solution：Pending containing vanadium solution is preheated, is heated to 95~100 DEG C, adjusting contains
The pH of vanadium solution to 1.5~2；Wherein, according to solid-to-liquid ratio, the vanadic anhydride filled in reaction tube:It is pending containing vanadium solution=
0.5~2g:1L；
C, it filters and precipitates containing vanadium solution：By b step it is pretreated containing vanadium solution from bottom to up, countercurrently by a steps at
Reaction tube after reason, and being heated to reaction tube lower half portion, make by the temperature containing vanadium solution of reaction tube for 101~
110 DEG C, reaction tube top half is cooled down, be cooled to 30~40 DEG C；Flow velocity containing vanadium solution is 0.1~1L/ (h
cm2), contain vanadium solution after obtaining containing the vanadic anhydride crystal and hydrolytic precipitation in vanadium solution.
Specific grain surface that the initial concentration of solution, pH value, precipitation process are formed product, the hydrolysising condition of system, filtering
The thickness of diffusion layer on surface, speed, density all to hydrolytic precipitation oxide have an impact.Wherein, the initial concentration of solution it is bigger,
PH numerical value is lower, and nucleation speed is fast, but Growing Process of Crystal Particles is especially short, and crystal grain is caused to fail to grow up, it is impossible to which it is qualified to be formed
Product, cause product density low, a problem that filtration difficulty.Therefore, such as want to be settled out qualified product, need quickly
Nucleation rate, crystal grain-growth process at a slow speed, in this way, can just obtain up-to-standard product.
Method of a kind of hydrolytic precipitation containing vanadium solution described above, reaction tube is acid resistance stainless steel wherein in a steps
Matter.
Wherein, the reaction tube is thinner, and the pressure of filtering is right in this way to the power provided containing vanadium solution with regard to big with regard to big
Precipitated products are just advantageous, and the vanadium oxide precipitated, crystal grain is more uniform, tiny, but meticulous pipe, and the rate of filtration is too
Slowly, thus be typically chosen in practical applications pipe diameter for 1~10cm with regard to proper.
Method of a kind of hydrolytic precipitation containing vanadium solution described above, the grain size of vanadic anhydride crystal seed filled in a steps
For 15~30um.
Further, technical solution more preferably, method of a kind of hydrolytic precipitation containing vanadium solution described above, wherein
According to solid-to-liquid ratio, preferably vanadic anhydride in b step:It is pending to contain vanadium solution=0.5~1g:1L.If vanadic anhydride
Amount it is excessive, can influence the rate travel of solution containing vanadium, reduce production efficiency；If the amount of vanadic anhydride is very few in pipe, contain
Vanadium in vanadium solution cannot be fully crystallized precipitation, and the effect of experiment is not achieved.
Method of a kind of hydrolytic precipitation containing vanadium solution described above adjusts pH value and uses volume ratio as 1 wherein in b step:1
Sulfuric acid, i.e., by 98% concentrated sulfuric acid, using clear water according to 1:1 ratio is diluted to obtain to it.
Further, in order to enable preferably to filter precipitation containing vanadium solution, using pumping at the top of reaction tube wherein in step c
Filter pump is filtered to containing vanadium solution.
Further, in order to enable preferably to crystallize precipitation, while cooling agent is environmentally safe containing vanadium solution, wherein
Reaction tube top half is cooled down using the air of atomization in step c.
Further, technical solution more preferably, method of a kind of hydrolytic precipitation containing vanadium solution described above, c steps
The filtering rate containing vanadium solution is preferably 0.2L/ (hcm in rapid2).Filter effect and vanadic anhydride crystallization effect be by
Containing pressure caused by vanadium solution and the residence time co-determination in pipe containing vanadium solution, the rate of filtration is smaller, and pressure is got over
It is low, but the residence time is long；It is on the contrary.Therefore, it is needed within the rate of filtration in practical application, according to the specific feelings containing vanadium solution
Condition selects a suitable rate of filtration.
Method of a kind of hydrolytic precipitation containing vanadium solution described above, wherein the vanadic anhydride crystal obtained after precipitation filtering
Grain size is 180~500um, pentoxide content >=97% in crystal, rate >=99% of precipitation containing vanadium solution.
The invention of the present invention is intended to increase specific surface area between its solid-liquid, thus reduces the sedimentation time and increases product density,
But by 180~500um of obtained sediment diameter, its very sad filter, very low to proportion is determined, moisture content is very high.
Moreover in the above method, ultra-fine precipitates contact for a long time with leachate, directly result in impurity element since ion exchange, ion are inhaled
Attached process is entered in precipitation solid phase.
Under the conditions of solid ion remains static, in the ductile layer with maximum hydrodynamic resistance, therefore in stratiform
In grown；Precipitating ion belongs to the discrete state of crystal grain in quiescent layer, with density, the increase to proportion, structure
More securely.
Solid ion (APV foreign ions) relies on high concentration range, actually from start to finish all in quick growth
State, so as to limit the precipitation of foreign ion.Upper partly precipitated ion in stationary state layer, in the contact process with mother liquor
In and in follow-up downward moving process its mass unit increases to 100 times or more, therefore, precipitation process impurity element has
The absorption for being exchanged with each other process that may occur will not destroy the density of product.
The intermediate processing that the present invention is taken, the formation of solid phase is formed in continuous precipitation process, the pH value of solution
The residual vanadium amount in leachate is influenced, the present invention relies on H+The increase of concentration, it is miscellaneous in sediment acquired in reduction in precipitation process
The content of matter.
In the complete precipitation process of v element, the height of counterfeit vaporization layer be it is necessary, the precipitation quantity of statistics wherein and
Kinetic parameter all makes it under atmospheric conditions, the boiling point increased can be obtained under heated solution adjusting, without reaching
The danger of boiling.Therefore, in atmospheric conditions, the filter layer in leachate adds by the reaction temperature for improving solution
The speed of fast precipitation process.
Special, academic expertise in precipitation process limit the content of wherein impurity, vanadic anhydride prepared by the present invention
Content reaches 97~98%；The particle size of sediment reaches 180~500 microns, and present invention process setting reduces product and contains
Water rate makes product be more easy to filter and wash；There is the upward wiring being perfectly clear, therefore point of mother liquor, sediment in mixed liquor
From the filter plant for not needing to profession.
According to theory, the reaction tube filled with vanadic anhydride is longer, to the filtering containing vanadium solution and precipitated crystal effect
Better, inventor has found by many experiments, for every 1L it is pending containing vanadium solution, need acid resistance reaction tube
Length for 100cm or so, as long as can achieve the purpose that be kept completely separate precipitation, but in the premise for reaching ideal effect
Under, length substantially 200cm or so of experiment reaction tube of the invention.
The present invention fills the vanadium oxide particles of full small particle in reaction tube, can both make containing the vanadium in vanadium solution according to
Precipitation is further crystallized by the vanadic anhydride of small particle, forms more large-sized vanadic anhydride crystal；It can make to reach again
To the purpose of impurity screening, make to be partitioned from containing impurity such as calcium oxide, the manganese oxide in vanadium solution, so as to reach what is detached with vanadium
Purpose.
The present invention is cooled down in the top half of reaction tube, and lower half portion heating, is in order to increase temperature difference band, after precipitation
Crystal grain cause to shrink, so as to control the uniformity of crystallite dimension.
The specific embodiment of the present invention is further described with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
The industrial extracted liquid of 2L is taken, wherein containing vanadic anhydride 0.1655mol/L, calcium oxide 0.01786mol/L,
Manganese oxide 0.2114mol/L, pH value containing vanadium solution 1.6 by it by reaction tube vertical 200cm, heat the bottom of reaction tube,
Cool down the top of reaction tube, the cross section 2.4cm of reaction tube2, liquid movement speed 0.2L/ (h.cm2).It is filled out in reaction vessel
The vanadic anhydride precipitate particle sizes filled are 15~30 microns, and weight is 1.5 kilograms, and vanadic anhydride is molten with containing vanadium in reaction tube
The solid-to-liquid ratio of liquid is：0.5g:1L, containing vanadium solution, reaction temperature is 101 DEG C in reaction tube.
Finally obtain 73.6g, the sediment that 180~200 microns of particle diameter, moisture content 15%, after melting
Pentoxide content reaches 98.5% in product, calcium oxide 0.7%, manganese oxide 0.7%, and the rate of deposition in solution reaches
99.1%.
Embodiment 2
The industrial extracted liquid of 2L is taken, wherein containing vanadic anhydride 0.1375mol/L, calcium oxide 0.02679mol/L,
Manganese oxide 0.1692mol/L, pH value containing vanadium solution 1.8 by it by reaction tube vertical 200cm, heat the bottom of reaction tube,
Cool down the top of reaction tube, the cross section 2.4cm of reaction tube2, liquid movement speed 1L/ (h.cm2).It is filled in reaction vessel
Vanadic anhydride precipitate particle sizes for 15~30 microns, weight is 1.5 kilograms, in reaction tube vanadic anhydride with containing vanadium solution
Solid-to-liquid ratio be：0.9g:1L, containing vanadium solution, reaction temperature is 105 DEG C in reaction tube.
Finally obtain 63.3g, the sediment that 180~200 microns of particle diameter, moisture content 15%, after melting
Pentoxide content reaches 98.3% in product, calcium oxide 0.7%, manganese oxide 0.9%, and the rate of deposition in solution reaches
99%.
Embodiment 3
The industrial extracted liquid of 2L is taken, wherein containing vanadic anhydride 0.1100mol/L, calcium oxide 0.02679mol/L,
Manganese oxide 0.1128mol/L, pH value containing vanadium solution 2 by it by reaction tube vertical 200cm, heat the bottom of reaction tube, cold
But the top of reaction tube, the cross section 2.4cm of reaction tube2, liquid movement speed 0.5L/ (h.cm2).It is filled in reaction vessel
Vanadic anhydride precipitate particle sizes for 15~30 microns, weight is 1.5 kilograms, in reaction tube vanadic anhydride with containing vanadium solution
Solid-to-liquid ratio be：1.5g:1L, containing vanadium solution, reaction temperature is 110 DEG C in reaction tube.
Finally obtain 53.6g, the sediment that 180~200 microns of particle diameter, moisture content 15%, after melting
Pentoxide content reaches 98.2% in product, calcium oxide 0.8%, manganese oxide 0.9%, and the rate of deposition in solution reaches
99%.
Claims (7)
1. a kind of method of hydrolytic precipitation containing vanadium solution, it is characterised in that：Include the following steps：
A, reaction tube pre-processes：The pipe of acid resistance material is taken, wherein filling vanadic anhydride；Wherein, the grain of vanadic anhydride
Diameter is 15~30 μm；
B, it is pre-processed containing vanadium solution：Pending containing vanadium solution is preheated, is heated to 95~100 DEG C, is adjusted molten containing vanadium
The pH of liquid to 1.5~2；Wherein, according to solid-to-liquid ratio, the vanadic anhydride filled in reaction tube:It is pending containing vanadium solution=0.5~
2g:1L；
C, it filters and precipitates containing vanadium solution：By b step it is pretreated containing vanadium solution from bottom to up, countercurrently by a step process after
Reaction tube, and reaction tube lower half portion is heated, it is 101~110 to make the temperature containing vanadium solution by reaction tube
DEG C, reaction tube top half is cooled down, is cooled to 30~40 DEG C；Flow velocity containing vanadium solution is 0.1~1L/ (hcm2),
It obtains containing vanadium solution after hydrolytic precipitation；
Obtained vanadic anhydride crystal particle diameter is 180~500 μm after precipitation filtering, pentoxide content in crystal >=
97%, rate >=99% of precipitation containing vanadium solution.
2. a kind of method of hydrolytic precipitation containing vanadium solution according to claim 1, it is characterised in that：Reaction tube is in a steps
Acid resistance stainless steel.
3. a kind of method of hydrolytic precipitation containing vanadium solution according to claim 1, it is characterised in that：According to solid-liquid in b step
Than the vanadic anhydride filled in reaction tube:It is pending to contain vanadium solution=0.5~0.9g:1L.
4. a kind of method of hydrolytic precipitation containing vanadium solution according to claim 1, it is characterised in that：PH value is adjusted in b step
Volume ratio is used as 1:1 sulfuric acid.
5. a kind of method of hydrolytic precipitation containing vanadium solution according to claim 1, it is characterised in that：Tube top is reacted in step c
Portion is filtered using suction filter pump to containing vanadium solution.
6. a kind of method of hydrolytic precipitation containing vanadium solution according to claim 1, it is characterised in that：In step c on reaction tube
Half part is cooled down using the air of atomization.
7. a kind of method of hydrolytic precipitation containing vanadium solution according to claim 1, it is characterised in that：Contain vanadium solution in step c
Filtering rate be 0.2L/ (hcm2)。
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| CN110666703B (en) * | 2019-09-12 | 2021-04-16 | 武汉大学 | Closed autogenous abrasive material jet device and experimental method using same |
| CN111020231A (en) * | 2019-12-04 | 2020-04-17 | 杨秋良 | Method for precipitating vanadium from sodium vanadium-rich liquid without ammonia |
| CN113957262B (en) * | 2021-10-29 | 2022-09-23 | 东北大学 | Method for precipitating vanadium from vanadium-chromium leaching solution without ammonium |
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