CN107475518B - A kind of method that vanadium classification is leached - Google Patents
A kind of method that vanadium classification is leached Download PDFInfo
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- CN107475518B CN107475518B CN201710942560.2A CN201710942560A CN107475518B CN 107475518 B CN107475518 B CN 107475518B CN 201710942560 A CN201710942560 A CN 201710942560A CN 107475518 B CN107475518 B CN 107475518B
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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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- 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
Abstract
The invention discloses the methods that a kind of classification of vanadium is leached, and belong to field of metallurgy.A kind of method that vanadium classification is leached: slurry pH is leached containing vanadium by successively adjusting, successively carry out classification leaching, level-one including 10≤pH < 13 leaches, the second level of 7≤pH < 10 leaches, the three-level of 6≤pH < 7 leaches, the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；Six grades of leachings of 1.5≤pH < 2.5, seven grades of leachings of 1.0≤pH < 1.5.The method of the present invention is according to V5+Existence form and color in different pH leachates, creative provides a kind of vanadium classification disengaging method, generates different leaching products, significantly improves V leaching rate, being classified accumulative leaching rate can be to 96% or more；It can be according to V in calcification baking clinker5+Existence form, flexible choice leach rank, reduce classification number, reduce cost, field conduct is strong, have wide promotional value.
Description
Technical field
The invention belongs to field of metallurgy, are related to a kind of method that vanadium classification is leached.
Background technique
Conventional vanadium leaching method is Rapid Leaching+leach at a slow speed.The mixing speed within 15min occurs for Rapid Leaching
It is exceedingly fast, phosphoric acid, temperature increased dramatically with the sharply addition and the sharply decline of pH of dilute sulfuric acid, while generating big quantitative response
Heat, reaction heat is excessively high, causes extraction temperature higher, leaches and precipitation phenomenon occurs, vanadium is caused to lose.It leaches at a slow speed and occurs
After 15min, mixing speed is moderate, phosphoric acid, temperature with dilute sulfuric acid be slowly added to become with the stabilization of pH it is slow and
Stablize.
The method of the quick reduction pH Rapid Leaching used in the prior art, in the preferable fast reaction of current heat insulation effect
Outstanding problem in tank, with the sharply raising for leaching phosphoric acid, temperature, reaction heat be increased dramatically, and cause to leach generation precipitation
Phenomenon, vanadium loss are more serious；Increase liquid-solid ratio, the method for dilute sulphuric acid concentration is taken to be only capable of alleviating Rapid Leaching slightly
The great quantities of spare that (in 15min) is generated reacts heat problem, can not equally solve the problems, such as to leach incomplete and precipitation.
Summary of the invention
For above-mentioned vanadium leaching method in the prior art, the present invention provides a kind of classifications of vanadium to leach
Method, method includes the following steps:
Water phase and calcification baking clinker are mixed to get and leach slurry A containing vanadium, classification leaching is successively carried out according to slurry pH；
The classification is leached the level-one including 10≤pH < 13 and is leached, and the second level of 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and 4
The level Four of≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；The operation that the classification is leached are as follows:
When the slurry A containing vanadium leaching is 10≤pH < 13, level-one leaching is carried out, then pass sequentially through and adjust slurry pH, successively
The second level for carrying out 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, and the five of 2.5≤pH < 3
Grade leaches, and filters to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 7≤pH < 10, directly progress second level leaching, then pass sequentially through adjusting slurry
PH, the three-level for successively carrying out 6≤pH < 7 leach, and the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches, and filter
Leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 6≤pH < 7, directly progress three-level leaching, then pass sequentially through adjusting slurry
PH, the level Four for successively carrying out 4≤pH < 5 leach, and the Pyatyi of 2.5≤pH < 3 leaches, and filter to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 4≤pH < 5, directly progress level Four leaching, then pass sequentially through adjusting slurry
PH, the Pyatyi for carrying out 2.5≤pH < 3 leach, and filter to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 2.5≤pH < 3, directly progress Pyatyi leaching filters to obtain and leaches vanadium liquid A.
Wherein, in the above method, the classification leaching further includes six grades of leachings of 1.5≤pH < 2.5,1.0≤pH < 1.5
Seven grades leaching, it is described classification leach operation are as follows:
When the slurry A containing vanadium leaching is 10≤pH < 13, level-one leaching is carried out, then pass sequentially through and adjust slurry pH, successively
The second level for carrying out 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, and the five of 2.5≤pH < 3
Grade leaches；The slurry separation that Pyatyi is leached obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches to soak containing vanadium
Slurry B out, then pass sequentially through and adjust slurry pH, successively the six of 1.5≤pH < 2.5 grade leach, seven grades of leachings of 1.0≤pH < 1.5
Out, it filters to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 7≤pH < 10, directly progress second level leaching, then pass sequentially through adjusting slurry
PH, the three-level for successively carrying out 6≤pH < 7 leach, and the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；By Pyatyi
The slurry of leaching separates, and obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches containing vanadium leaching slurry B, then according to
Secondary by adjusting slurry pH, successively the six of 1.5≤pH < 2.5 grade are leached, and seven grades of leachings of 1.0≤pH < 1.5 filter to leach
Vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 6≤pH < 7, directly progress three-level leaching, then pass sequentially through adjusting slurry
PH, the level Four for successively carrying out 4≤pH < 5 leach, and the Pyatyi of 2.5≤pH < 3 leaches；The slurry separation that Pyatyi is leached, obtains
Vanadium liquid A and residue are leached, it is residue obtained mixed with water, match to leach slurry B containing vanadium, then pass sequentially through and adjust slurry pH, according to
Six grades of leachings of secondary 1.5≤pH < 2.5, seven grades of leachings of 1.0≤pH < 1.5, filter to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 4≤pH < 5, directly progress level Four leaching, then pass sequentially through adjusting slurry
PH, the Pyatyi for carrying out 2.5≤pH < 3 leach；The slurry separation that Pyatyi is leached obtains leaching vanadium liquid A and residue, residue obtained
It is mixed with water, match to leach slurry B containing vanadium, then pass sequentially through and adjust slurry pH, successively the six of 1.5≤pH < 2.5 grade leach,
Seven grades of leachings of 1.0≤pH < 1.5, filter to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 2.5≤pH < 3, directly progress Pyatyi leaching；The slurry that Pyatyi is leached
Separation obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches to leach slurry B containing vanadium, then pass sequentially through adjusting
Slurry pH, successively the six of 1.5≤pH < 2.5 grade leach, and seven grades of leachings of 1.0≤pH < 1.5 filter to leach vanadium liquid B；
Or: adjusting the pH for leaching slurry A containing vanadium is 1.5≤pH < 2.5, directly carries out six grades of leachings, then pass through adjusting
Slurry pH carries out seven grades of leachings of 1.0≤pH < 1.5, filters to leach vanadium liquid A；
Or: adjusting the pH for leaching slurry A containing vanadium is 1.0≤pH < 1.5, directly carries out seven grades of leachings, filters to leach
Vanadium liquid A.
Wherein, in the above method, the water phase is at least one of water or low concentration vanadium liquid；The low concentration vanadium liquid
PH is 2.5~4.0, and vanadium concentration is 3~8g/L, in terms of V.
Wherein, described when classification, which is leached, leaches since level-one, second level, three-level, level Four or Pyatyi in the above method
To leach slurry A containing vanadium be to be not less than 2.5 by liquid-solid ratio by water phase and calcification baking clinker, preparation obtains；The liquid-solid ratio is
By volume, solid is by mass for water phase.
Wherein, in the above method, when classification, which is leached, leaches since six grades or seven grades, the slurry A containing vanadium leaching is
It is not less than 2.0 by liquid-solid ratio by water phase and calcification baking clinker, preparation obtains；It is described containing vanadium leach slurry B be by water phase with it is residual
Slag is not less than 2.0 by liquid-solid ratio, and preparation obtains；By volume for water phase, solid is by mass for the liquid-solid ratio.
Wherein, in the above method, when calcification baking clinker is (Ca, Mn) V2O7Or Ca2V2O7At least one of when, by water
It is mutually mixed with calcification baking clinker by liquid-solid ratio 2.67~3, obtains leaching slurry A containing vanadium, directly be leached since leaching second level.
Wherein, in the above method, when calcification baking clinker is Ca (VO3)2When, water phase is consolidated with calcification baking clinker by liquid
It than 2.1~2.5 mixing, obtains leaching slurry A containing vanadium, adjusting and leaching the pH of slurry A containing vanadium is 1.5≤pH < 2.5, directly from six
Grade, which leaches, to be started to leach.
Wherein, in the above method, use mass concentration for 30~65% sulphur acid for adjusting pH.
Wherein, in the above method, the extraction time of every grade of leaching is 5~10min.
The beneficial effects of the present invention are:
The method of the present invention is according to V5+Existence form and color in different pH leachates, creative provides a kind of vanadium
Method of classified leaching can be controlled accurately and leach pH and suitable extraction temperature, generate different leaching products, be shown
Work reduces precipitation caused by scene is sharply reacted or leaches incomplete problem, further increases leaching rate, is classified accumulative leach
Rate can be to 96% or more, remarkable in economical benefits；It can be according to V in calcification baking clinker5+Existence form, flexible choice leach grade
Not, classification number is reduced, cost is reduced, field conduct is strong, has wide promotional value.
Specific embodiment
Specifically, a kind of method that vanadium classification is leached, comprising the following steps:
Water phase and calcification baking clinker are mixed to get and leach slurry A containing vanadium, classification leaching is successively carried out according to slurry pH；
The classification is leached the level-one including 10≤pH < 13 and is leached, and the second level of 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and 4
The level Four of≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；The operation that the classification is leached are as follows:
When the slurry A containing vanadium leaching is 10≤pH < 13, level-one leaching is carried out, then pass sequentially through and adjust slurry pH, successively
The second level for carrying out 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, and the five of 2.5≤pH < 3
Grade leaches, and filters to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 7≤pH < 10, directly progress second level leaching, then pass sequentially through adjusting slurry
PH, the three-level for successively carrying out 6≤pH < 7 leach, and the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches, and filter
Leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 6≤pH < 7, directly progress three-level leaching, then pass sequentially through adjusting slurry
PH, the level Four for successively carrying out 4≤pH < 5 leach, and the Pyatyi of 2.5≤pH < 3 leaches, and filter to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 4≤pH < 5, directly progress level Four leaching, then pass sequentially through adjusting slurry
PH, the Pyatyi for carrying out 2.5≤pH < 3 leach, and filter to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 2.5≤pH < 3, directly progress Pyatyi leaching filters to obtain and leaches vanadium liquid A.
Inventor leaches in practice in vanadium and finds, V5+Existence form is different in different pH liquid, pH variation, V5+In the presence of
Form converts rapidly, and V5+Color also changes correspondingly, and slurry color, extraction time, leaching rate can be passed through by leaching terminal
Deng judgement.The present invention is according to V5+Existence form and color in different leaching pH, provide a kind of vanadium method of classified leaching, with
Under vanadium method of classified leaching of the present invention is specifically explained:
1, the slurry A containing vanadium leaching is 10≤pH < 13, carries out level-one leaching, and leaching product is colourless containing V2O7 4-It leaches
Slurry；
10≤pH < 13:2VO4 3-(colourless)+2H+→V2O7 4-(colourless)+H2O
2, the slurry A containing vanadium leaching is 7≤pH < 10, carries out second level leaching, and leaching product is colourless containing V4O12 4-Leached material
Slurry；
7≤pH < 10:2V2O7 4-(colourless)+4H+→V4O12 4-(colourless)+2H2O
3, the slurry A containing vanadium leaching is 6≤pH < 7, carries out three-level leaching, and leaching product is orange containing V10O28 6-Leached material
Slurry；
6≤pH < 7:2.5V4O12 4-(colourless)+4H+→V10O28 6-(orange)+2H2O
4, the slurry A containing vanadium leaching is 4≤pH < 5, carries out level Four leaching, and leaching product is orange containing HV10O28 5-It leaches
Slurry；
4≤pH < 5:V10O28 6-(orange)+H+→HV10O28 5-(orange)
5, the slurry A containing vanadium leaching is 2.5≤pH < 3, carries out Pyatyi leaching, and leaching product is darkorange containing H2V10O28 4-
Leach slurry；
2.5≤pH < 3:HV10O28 5-(orange)+H+→H2V10O28 4-(darkorange)
It is the H of darkorange by the product that Pyatyi leaches2V10O28 4-Slurry is leached, pH can not be controlled at this time too high
(3≤pH < 4) otherwise can occur to hydrolyze precipitation:
3≤pH < 4:H2V10O28 4-(darkorange)+4H++2H2O→5V2O5·H2O (brick-red solid)
Also can not be too low by pH control, it otherwise can occur to hydrolyze precipitation:
1.5≤pH < 2.5:H2V10O28 4-(darkorange)+14H+→10VO2 +(light yellow)+8H2O
PH≤1:2VO2 +(light yellow)+2H2O→V2O5·H2O (brick-red solid)+2H+
In addition, the leaching rank of the method for the present invention can also be including six grades of leachings of 1.5≤pH < 2.5,1.0≤pH <
1.5 seven grades of leachings, the operation that the classification is leached are as follows:
When the slurry A containing vanadium leaching is 10≤pH < 13, level-one leaching is carried out, then pass sequentially through and adjust slurry pH, successively
The second level for carrying out 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, and the five of 2.5≤pH < 3
Grade leaches；The slurry separation that Pyatyi is leached obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches to soak containing vanadium
Slurry B out, then pass sequentially through and adjust slurry pH, successively the six of 1.5≤pH < 2.5 grade leach, seven grades of leachings of 1.0≤pH < 1.5
Out, it filters to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 7≤pH < 10, directly progress second level leaching, then pass sequentially through adjusting slurry
PH, the three-level for successively carrying out 6≤pH < 7 leach, and the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；By Pyatyi
The slurry of leaching separates, and obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches containing vanadium leaching slurry B, then according to
Secondary by adjusting slurry pH, successively the six of 1.5≤pH < 2.5 grade are leached, and seven grades of leachings of 1.0≤pH < 1.5 filter to leach
Vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 6≤pH < 7, directly progress three-level leaching, then pass sequentially through adjusting slurry
PH, the level Four for successively carrying out 4≤pH < 5 leach, and the Pyatyi of 2.5≤pH < 3 leaches；The slurry separation that Pyatyi is leached, obtains
Vanadium liquid A and residue are leached, it is residue obtained mixed with water, match to leach slurry B containing vanadium, then pass sequentially through and adjust slurry pH, according to
Six grades of leachings of secondary 1.5≤pH < 2.5, seven grades of leachings of 1.0≤pH < 1.5, filter to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 4≤pH < 5, directly progress level Four leaching, then pass sequentially through adjusting slurry
PH, the Pyatyi for carrying out 2.5≤pH < 3 leach；The slurry separation that Pyatyi is leached obtains leaching vanadium liquid A and residue, residue obtained
It is mixed with water, match to leach slurry B containing vanadium, then pass sequentially through and adjust slurry pH, successively the six of 1.5≤pH < 2.5 grade leach,
Seven grades of leachings of 1.0≤pH < 1.5, filter to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 2.5≤pH < 3, directly progress Pyatyi leaching；The slurry that Pyatyi is leached
Separation obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches to leach slurry B containing vanadium, then pass sequentially through adjusting
Slurry pH, successively the six of 1.5≤pH < 2.5 grade leach, and seven grades of leachings of 1.0≤pH < 1.5 filter to leach vanadium liquid B；
Or: adjusting the pH for leaching slurry A containing vanadium is 1.5≤pH < 2.5, directly carries out six grades of leachings, then pass through adjusting
Slurry pH carries out seven grades of leachings of 1.0≤pH < 1.5, filters to leach vanadium liquid A；
Or: adjusting the pH for leaching slurry A containing vanadium is 1.0≤pH < 1.5, directly carries out seven grades of leachings, filters to leach
Vanadium liquid A.
In conjunction with the explanation that the present invention leaches level-one to Pyatyi, six grades are leached below and seven grades of leachings are specifically solved
It releases:
6, adjusting the pH for leaching slurry A containing vanadium is 1.5≤pH < 2.5, carries out six grades of leachings, and it is lurid for leaching product
Containing VO2 +Leach slurry；
1.5≤pH < 2.5:VO3 -(colourless)+2H+→VO2 +(light yellow)+H2O
7, adjusting the pH for leaching slurry A containing vanadium is 1.0≤pH < 1.5, carries out seven grades of leachings, and leaching product is orange contain
HV10O28 5-Leach slurry；
1.0≤pH < 1.5:10VO2 +(light yellow)+8H2O→HV10O28 5-(orange)+15H+
At this time if pH controls too low (pH≤1), it can occur to hydrolyze precipitation, produce brick-red solid:
PH≤1:2VO2 +(light yellow)+2H2O→V2O5·H2O (brick-red solid)+2H+
Level-one to Pyatyi is leached mainly for high vanadium clinker in the method for the present invention, and full content of vanadium (TV meter) is 6~10%；Six
For grade to seven grades of leachings mainly for low vanadium clinker, full content of vanadium (TV meter) is 1~5%；And for middle vanadium clinker, full content of vanadium
When (TV meter) is 5~6%, then it can be leached, can also be leached by low vanadium clinker by high vanadium clinker, it can in actual production
According to the final accumulative V leaching rate of clinker, optimal Leaching way is selected.
In the method for the present invention, one to Pyatyi leaching is true with the practical pH of clinker gained mixed with water slurry A containing vanadium leaching
Fixed initial leaching rank；Depended on containing the practical pH that vanadium leaches slurry the soluble acidic substance in clinker number, clinker and water
Phase mass volume ratio, water phase pH etc.；After determining initial leaching rank, then passes sequentially through and adjust slurry pH progress subsequent level leaching
Out, it such as when determining since leaching level-one, is leached through level-one, then passes sequentially through and adjust slurry pH, successively carry out two to five
Grade leaches, the slurry filtration that Pyatyi is leached, and can obtain leaching vanadium liquid A；In another example when determining since leaching second level, warp
Second level leaches, then passes sequentially through and adjust slurry pH, successively carries out three and leaches to Pyatyi, the slurry filtration that Pyatyi is leached can
It obtains leaching vanadium liquid A.
When clinker is after one to Pyatyi leaches, it is also necessary to when carrying out six grades and seven grades leachings again, due to being leached by Pyatyi
Vanadium concentration is higher (vanadium concentration is not less than 25g/L, in terms of V) in obtained slurry, adds up V leaching rate up to 90% or more, at this time
If directly carrying out six grades of leachings, pH is controlled into too low (1.5≤pH < 2.5 or pH≤1), hydrolysis precipitation easily occurs, instead
Influence V leaching rate；Therefore, the slurry separation for needing to leach Pyatyi at this time, obtains leaching vanadium liquid A and residue, it is residue obtained with
Water phase mixing matches to leach slurry B containing vanadium, then passes sequentially through and adjust slurry pH, and successively the six of 1.5≤pH < 2.5 grade leach,
Seven grades of leachings of 1.0≤pH < 1.5, filter to leach vanadium liquid B, and leaching vanadium liquid B is low concentration vanadium liquid, can be used as classification and leach
In water phase be used for multiple times.
In addition, being found through practice, slurry A is leached after Pyatyi leaches containing vanadium, filters residue obtained middle V5+Content compared with
It is few, it can choose whether to carry out subsequent hierarchical leaching at this time with needs of production；In view of factors such as costs, it is classified by a wheel
Leaching residue obtained middle content of vanadium amount generally will not be too many, then can add up residue, when residue reaches it is a certain amount of after, then carry out six
Grade and seven grades of leachings；Residue can also be mixed with water, be formulated as the slurry of the vanadium liquid containing low concentration, as mixed with calcification baking clinker
The water phase of conjunction.
After clinker is mixed with water, when leaching slurry A needs since being leached six grades or seven grades containing vanadium, due to containing at this time
The pH that vanadium leaches slurry A is higher, it is therefore desirable to the pH for leaching slurry A containing vanadium is adjusted to accordingly to leach the pH requirement of rank, then into
Six grades or seven grades of row leachings.
For high vanadium clinker or middle vanadium clinker, terminal product is to leach to filter resulting darkorange leaching vanadium liquid through Pyatyi
(contain H2V10O28 4-), i.e. leaching vanadium liquid A, and/or (contain HV through the resulting orange leaching vanadium liquid of seven grades of leaching filterings10O28 5-), i.e.,
Leach vanadium liquid B；Although orange leaching vanadium liquid can be obtained (containing HV through level Four product10O28 5-), but due to vanadium concentration in the vanadium liquid
It is lower, therefore leached there is still a need for Pyatyi is continued, to obtain the leaching vanadium liquid A of high concentration；For low vanadium clinker or middle vanadium
Clinker, terminal product are to leach resulting orange leaching vanadium liquid through seven grades (to contain HV10O28 5-), i.e. leaching vanadium liquid A.
Water phase described in the method for the present invention is at least one of water or low concentration vanadium liquid；Wherein the pH of low concentration vanadium liquid is
2.5~4.0, vanadium concentration is 3~8g/L (in terms of V)；Which kind of therefore in actual production, can select that water used as the case may be
Phase；Liquid-solid ratio involved in the present invention be water phase by volume, solid is by mass.
Due to leach rank since one to Pyatyi leach start calcification baking clinker in content of vanadium it is higher, containing vanadium leaching slurry
Content of vanadium is higher in A, and the liquid-solid ratio needed is bigger；Leach rank vanadium since the calcification baking clinker six grades or seven grades leachings
Content is lower, and content of vanadium is lower in slurry, and the liquid-solid ratio needed is smaller；Therefore, when classification is leached from level-one, second level, three-level, four
When grade or Pyatyi start to leach, described leaches slurry A containing vanadium to be not less than with calcification baking clinker by liquid-solid ratio by water phase
2.5, preparation obtains；When classification, which is leached, leaches since six grades or seven grades, the slurry A containing vanadium leaching is by water phase and calcification
It roasts clinker and is not less than 2.0 by liquid-solid ratio, preparation obtains；It is described to leach slurry B containing vanadium to be pressed by water phase and calcification baking clinker
Liquid-solid ratio is not less than 2.0, and preparation obtains.
Calcification baking clinker main Types are (Ca, Mn) V2O7And/or Ca2V2O7Or Ca (VO3)2；When calcification baking clinker
Product is (Ca, Mn) V2O7Or Ca2V2O7At least one of when, according to it is above-mentioned to classification leach explanation it is found that (Ca, Mn)
V2O7、Ca2V2O7With cation identical with second level Leach reaction object, therefore level-one leaching need not be carried out again, but by water phase
It is mixed with calcification baking clinker by liquid-solid ratio 2.67~3, obtains leaching slurry A, directly since the second level, Pyatyi knot containing vanadium
Beam is obtained by filtration and leaches vanadium liquid A, and residue carries out six grades and seven grades leachings again；When calcification baking clinker product is Ca (VO3)2When,
According to the above-mentioned explanation leached to classification it is found that Ca (VO3)2It, can be by water with cation identical with six grades of Leach reaction objects
It is mutually mixed with calcification baking clinker by liquid-solid ratio 2.1~2.5, obtains leaching slurry A containing vanadium, adjust the pH for leaching slurry A containing vanadium
For 1.5≤pH < 2.5, directly since the 6th grade, seven grades terminate, and filter to leach vanadium liquid A；Other compounds, such as Fe
(VO3)2、Mn(VO3)2Deng, be referred to method choice leach rank.
By above-mentioned explanation it is found that as V in calcification baking clinker5+Existence form and one to seven grade of Leach reaction object there is phase
, then can be mixed with water by calcification baking clinker when with cation, it is formulated as the corresponding pH for leaching rank, is directly carried out corresponding
The leaching of rank reduces classification number, reduces cost so that flexible choice leaches rank.
The method of the present invention uses mass concentration to carry out classification leaching, the reaction heat of generation for 30~65% sulphur acid for adjusting pH
It measures moderate, avoids because extraction temperature is higher, leach and precipitation phenomenon occurs, caused vanadium loss.
In the method for the present invention, V5+It is different leaching pH in existence forms and color can fast transition, in order to improve vanadium
Leaching rate, while the time is saved, the extraction time of every grade of leaching is 5~10min.
Below by embodiment, invention is further described in detail, but does not therefore limit the scope of the present invention
Among the embodiment described range.
Add up leaching rate={ 1- [residue TV- (clinker TV- clinker V in the embodiment of the present invention5+)] ÷ clinker V5+}×
100%.
Embodiment 1
Calcification baking clinker is taken, being detected its full content of vanadium (TV meter) is 9.75%, clinker V5+It is 8.86%, by water and calcium
Salt roasting clinker is mixed by liquid-solid ratio 2.5, and obtaining pH is 11.5 containing vanadium leaching slurry A, is carried out classification leaching, is classified vanadium in leaching
Content and vanadium add up leaching rate and are shown in Table 1；It is as follows to be classified leaching operation:
Vanadium will be contained and leach slurry A progress level-one leaching, extraction time 10min, leaching product is colourless containing V2O7 4-Leaching
Slurry out；
Gained colourless leach is leached to level-one, the sulfuric acid that mass concentration is 38% is added in slurry, adjust slurry pH to 7.5,
Second level leaching is carried out, extraction time 10min, leaching product is colourless containing V4O12 4-Leach slurry；
Gained colourless leach is leached to second level, the sulfuric acid that mass concentration is 38% is added in slurry, adjust slurry pH to 6.5,
Three-level leaching is carried out, extraction time 10min, leaching product is orange containing V10O28 6-Leach slurry；
Gained orange leach is leached to three-level, the sulfuric acid that mass concentration is 38% is added in slurry, adjust slurry pH to 4.5,
Level Four leaching is carried out, extraction time 10min, leaching product is orange containing HV10O28 5-Leach slurry；
Gained orange leach is leached to level Four, the sulfuric acid that mass concentration is 38% is added in slurry, adjust slurry pH to 2.8,
Pyatyi leaching is carried out, extraction time 10min, leaching product is darkorange containing H2V10O28 4-Leach slurry；
Slurry A is leached containing vanadium to leach by level-one to Pyatyi, adds up V leaching rate up to 96.39%, Pyatyi leaches gained
Darkorange leach slurry in vanadium concentration it is higher (vanadium concentration 34.89g/L, in terms of V), if directly carry out six grades leach, easily
Hydrolysis precipitation occurs；
Pyatyi is leached into gained darkorange and leaches slurry filtration, obtains and leaches vanadium liquid A and residue, it is highly concentrated for leaching vanadium liquid A
Vanadium liquid is spent, subsequent precipitation process is can be directly used for and uses；Residue is then mixed with water by liquid-solid ratio 2.0, matches to leach slurry containing vanadium
B is added the sulfuric acid that mass concentration is 38% and adjusts slurry pH to 1.8, carries out six grades of leachings, and extraction time 10min is leached and produced
Product are lurid containing VO2 +Leach slurry；
To six grades leach gained it is light yellow leach slurries in be added mass concentration be 38% sulfuric acid, adjust slurry pH to
1.2, seven grades of leachings, extraction time 10min are carried out, leaching product is orange HV10O28 5-Leach slurry；It will be orange
HV10O28 5-Slurry filtration is leached, vanadium liquid B must be leached；Leaching vanadium liquid B is low concentration vanadium liquid (concentration is 3~8g/L, in terms of V), can
It is used for multiple times as the water phase in classification leaching, is high concentration vanadium liquid to concentration enrichment (vanadium concentration is not less than 25g/L, in terms of V)
When, it is used further to precipitation process.
1 content of vanadium of table and vanadium add up leaching rate
From the data in table 1, it can be seen that the present embodiment calcification baking clinker is leached by one to Pyatyi, accumulative V leaching rate reaches
96.39%, it is leached using six to seven grades, adds up V leaching rate up to 99.66%, greatly improve clinker V leaching rate.
Embodiment 2
Calcification baking clinker is taken, being detected its full content of vanadium (TV meter) is 7.78%, clinker V5+It is 6.68%, by low concentration
Vanadium liquid (vanadium concentration is 3.26g/L, in terms of V) is mixed with calcification baking clinker by liquid-solid ratio 2.5, and obtaining pH is 6.5 containing vanadium leaching
Slurry A carries out classification leaching, and content of vanadium and the accumulative leaching rate of vanadium are shown in Table 2 in classification leaching；It is as follows to be classified leaching operation:
Vanadium will be contained and leach slurry A progress three-level leaching, extraction time 10min, leaching product is orange containing V10O28 6-
Leach slurry；
Gained orange leach is leached to three-level, the sulfuric acid that mass concentration is 38% is added in slurry, adjust slurry pH to 4.5,
Level Four leaching is carried out, extraction time 10min, leaching product is orange containing HV10O28 5-Leach slurry；
Gained orange leach is leached to level Four, the sulfuric acid that mass concentration is 38% is added in slurry, adjust slurry pH to 2.8,
Pyatyi leaching is carried out, extraction time 10min, leaching product is darkorange containing H2V10O28 4-Leach slurry；
Slurry is leached containing vanadium to leach by three-level to Pyatyi, adds up V leaching rate up to 91.47%, Pyatyi leaches resulting
Vanadium concentration is higher (vanadium concentration is 28.57g/L) in darkorange leaching vanadium liquid, directly carries out six grades of leachings, and easily generation hydrolysis is heavy
Vanadium；
Pyatyi is leached into gained darkorange and leaches slurry filtration, vanadium liquid A and residue must be leached, leaching vanadium liquid A is high concentration
Vanadium liquid can be directly used for subsequent precipitation process and use；Residue then presses liquid with low concentration vanadium liquid (vanadium concentration is 3.26g/L, in terms of V)
Admittedly matching to leach slurry B containing vanadium than 2.0 mixing, the sulfuric acid adjusting slurry pH to 1.8 that mass concentration is 38% is added, carries out six
Grade leaches, extraction time 10min, and leaching product is lurid containing VO2 +Leach slurry；
To six grades leach gained it is light yellow leach slurries in be added mass concentration be 38% sulfuric acid, adjust slurry pH to
1.2, seven grades of leachings, extraction time 10min are carried out, leaching product is orange HV10O28 5-Leach slurry；It will be orange
HV10O28 5-Slurry filtration is leached, vanadium liquid B must be leached；Leaching vanadium liquid B is low concentration vanadium liquid (vanadium concentration is 4.97g/L, in terms of V),
The water phase that can be used as in classification leaching is used for multiple times, and is that (vanadium concentration is not less than 25g/L to high concentration vanadium liquid, with V to concentration enrichment
Meter) when, it is used further to precipitation process.
2 content of vanadium of table and vanadium add up leaching rate
From the data in table 2, it can be seen that the present embodiment calcification baking clinker is leached by three to Pyatyi, accumulative V leaching rate reaches
91.47%, then leached through six to seven grades, add up V leaching rate up to 98.65%, greatly improves clinker V leaching rate.
Embodiment 3
Calcification baking clinker is taken, being detected its full content of vanadium (TV meter) is 4.85%, clinker V5+It is 3.78%, by embodiment
It is mixed by liquid-solid ratio 2.0 with calcification baking clinker that 2 gained leach vanadium liquid B (i.e. low concentration vanadium liquid, vanadium concentration is 4.97g/L, in terms of V)
It closes, obtains and leach slurry A containing vanadium, carry out classification leaching, content of vanadium and the accumulative leaching rate of vanadium are shown in Table 2 in classification leaching；Classification is leached
It operates as follows:
The sulfuric acid adjusting slurry pH to 1.8 that mass concentration is 38% is added in slurry A to leaching containing vanadium, carries out six grades of leachings
Out, extraction time 10min, leaching product are light yellow leaching vanadium liquid (VO2 +)；
To six grades leach gained it is light yellow leach slurries in be added mass concentration be 38% sulfuric acid, adjust slurry pH to
1.2, seven grades of leachings, extraction time 10min are carried out, leaching product is orange leaching vanadium liquid (HV10O28 5-)；
The orange leaching slurry filtration of gained will be leached to get the leaching vanadium liquid for arriving the present embodiment calcification baking clinker through seven grades
A, leaching vanadium liquid A can be directly used for subsequent precipitation technique；The present embodiment calcification baking clinker adds up vanadium by six to seven grades of leachings
Leaching rate greatly improves clinker V leaching rate up to 97.88%.
3 content of vanadium of table and vanadium add up leaching rate
| Leach series | Leach pH | Clinker TV/% | Clinker V5+/ % | Residue TV/% | Accumulative leaching rate/% |
| 6th grade | [1.5,2.5) | 4.85 | 3.78 | 2.35 | 66.14 |
| 7th grade | [1,1.5) | 1.15 | 97.88 |
Claims (14)
1. the method that vanadium classification is leached, it is characterised in that: the following steps are included:
Water phase and calcification baking clinker are mixed to get and leach slurry A containing vanadium, classification leaching is successively carried out according to slurry pH；It is described
Classification is leached the level-one including 10≤pH < 13 and is leached, and the second level of 7≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, 4≤pH
The level Four of < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；The operation that the classification is leached are as follows:
When the slurry A containing vanadium leaching is 10≤pH < 13, level-one leaching is carried out, then pass sequentially through and adjust slurry pH, successively carry out 7
The second level of≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, the Pyatyi leaching of 2.5≤pH < 3
Out, it filters to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 7≤pH < 10, directly progress second level leaching, then pass sequentially through and adjust slurry pH,
The three-level for successively carrying out 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches, and filters to leach
Vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 6≤pH < 7, directly progress three-level leaching, then pass sequentially through and adjust slurry pH, according to
The secondary level Four for carrying out 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches, and filters to leach vanadium liquid A；
Or: when the slurry A containing vanadium leaching is 4≤pH < 5, directly progress level Four leaching, then pass sequentially through and adjust slurry pH, into
The Pyatyi of 2.5≤pH of row < 3 leaches, and filters to leach vanadium liquid A；
When classification, which is leached, leaches since level-one, second level, three-level or level Four, it is described containing vanadium leach slurry A be by water phase with
Calcification baking clinker is not less than 2.5 by liquid-solid ratio, and preparation obtains；By volume for water phase, solid is by mass for the liquid-solid ratio；
The calcification baking clinker is high vanadium clinker or middle vanadium clinker, and the full content of vanadium of the high vanadium clinker is 6~10%, the middle vanadium
The full content of vanadium of clinker is 5~6%.
2. the method that vanadium according to claim 1 classification is leached, it is characterised in that: it further includes 1.5 that the classification, which is leached ,≤
Six grades of leachings of pH < 2.5, seven grades of leachings of 1.0≤pH < 1.5, the operation that the classification is leached are as follows:
When the slurry A containing vanadium leaching is 10≤pH < 13, level-one leaching is carried out, then pass sequentially through and adjust slurry pH, successively carry out 7
The second level of≤pH < 10 leaches, and the three-level of 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, the Pyatyi leaching of 2.5≤pH < 3
Out；The slurry separation that Pyatyi is leached obtains leaching vanadium liquid A and residue, residue obtained mixed with water, matches to obtain leached material containing vanadium
B is starched, then passes sequentially through and adjusts slurry pH, successively the six of 1.5≤pH < 2.5 grade leach, seven grades of leachings of 1.0≤pH < 1.5, mistake
It filters to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 7≤pH < 10, directly progress second level leaching, then pass sequentially through and adjust slurry pH,
The three-level for successively carrying out 6≤pH < 7 leaches, and the level Four of 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；Pyatyi is leached
Slurry separation, obtain leaching vanadium liquid A and residue, it is residue obtained mixed with water, with leach slurry B containing vanadium, then successively lead to
Slurry pH is overregulated, successively the six of 1.5≤pH < 2.5 grade leach, and seven grades of leachings of 1.0≤pH < 1.5 filter to leach vanadium liquid
B；
Or: when the slurry A containing vanadium leaching is 6≤pH < 7, directly progress three-level leaching, then pass sequentially through and adjust slurry pH, according to
The secondary level Four for carrying out 4≤pH < 5 leaches, and the Pyatyi of 2.5≤pH < 3 leaches；The slurry separation that Pyatyi is leached, obtains Leaching Vanadium
Liquid A and residue, it is residue obtained mixed with water, with leach slurry B containing vanadium, then pass sequentially through and adjust slurry pH, successively 1.5≤
Six grades of leachings of pH < 2.5, seven grades of leachings of 1.0≤pH < 1.5, filter to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 4≤pH < 5, directly progress level Four leaching, then by adjusting slurry pH, progress
The Pyatyi of 2.5≤pH < 3 leaches；The slurry separation that Pyatyi is leached, obtains leaching vanadium liquid A and residue, residue obtained and water phase
Mixing matches to leach slurry B containing vanadium, then passes sequentially through and adjust slurry pH, and successively the six of 1.5≤pH < 2.5 grade leach, 1.0≤
Seven grades of leachings of pH < 1.5, filter to leach vanadium liquid B；
Or: when the slurry A containing vanadium leaching is 2.5≤pH < 3, directly progress Pyatyi leaching；The slurry separation that Pyatyi is leached,
It obtains leaching vanadium liquid A and residue, it is residue obtained mixed with water, match to leach slurry B containing vanadium, then pass sequentially through adjusting slurry
PH, successively the six of 1.5≤pH < 2.5 grade leach, and seven grades of leachings of 1.0≤pH < 1.5 filter to leach vanadium liquid B；
Or: adjusting the pH for leaching slurry A containing vanadium is 1.5≤pH < 2.5, directly carries out six grades of leachings, then by adjusting slurry
PH carries out seven grades of leachings of 1.0≤pH < 1.5, filters to leach vanadium liquid A；
Or: adjusting the pH for leaching slurry A containing vanadium is 1.0≤pH < 1.5, directly carries out seven grades of leachings, filters to leach vanadium liquid
A；
When classification, which is leached, leaches since level-one, second level, three-level or level Four, it is described containing vanadium leach slurry A be by water phase with
Calcification baking clinker is not less than 2.5 by liquid-solid ratio, and preparation obtains；By volume for water phase, solid is by mass for the liquid-solid ratio；
The calcification baking clinker is high vanadium clinker or middle vanadium clinker, and the full content of vanadium of the high vanadium clinker is 6~10%, the middle vanadium
The full content of vanadium of clinker is 5~6%；
When classification, which is leached, leaches since six grades or seven grades, the slurry A containing vanadium leaching is by water phase and calcification baking clinker
It is not less than 2.0 by liquid-solid ratio, preparation obtains；The slurry B containing vanadium leaching is to be not less than 2.0 by liquid-solid ratio by water phase and residue,
Preparation obtains；By volume for water phase, solid is by mass for the liquid-solid ratio；The calcification baking clinker be low vanadium clinker or in
Vanadium clinker, the full content of vanadium of the low vanadium clinker are 1~5%, and the full content of vanadium of the middle vanadium clinker is 5~6%.
3. the method that vanadium classification according to claim 1 or 2 is leached, it is characterised in that: the water phase is water or low concentration
At least one of vanadium liquid；The pH of the low concentration vanadium liquid is 2.5~4.0, and vanadium concentration is 3~8g/L.
4. the method that vanadium according to claim 1 or 2 classification is leached, it is characterised in that: when calcification baking clinker is (Ca,
Mn)V2O7Or Ca2V2O7At least one of when, water phase is mixed with calcification baking clinker by liquid-solid ratio 2.67~3, is obtained containing vanadium
Slurry A is leached, is directly leached since leaching second level；By volume for water phase, solid is by mass for the liquid-solid ratio.
5. the method that vanadium classification according to claim 3 is leached, it is characterised in that: when calcification baking clinker is (Ca, Mn)
V2O7Or Ca2V2O7At least one of when, water phase is mixed with calcification baking clinker by liquid-solid ratio 2.67~3, obtain containing vanadium soak
Slurry A out is directly leached since leaching second level；By volume for water phase, solid is by mass for the liquid-solid ratio.
6. the method that vanadium classification according to claim 2 is leached, it is characterised in that: when calcification baking clinker is Ca (VO3)2
When, water phase is mixed with calcification baking clinker by liquid-solid ratio 2.1~2.5, obtains leaching slurry A containing vanadium, adjusts leached material containing vanadium
The pH for starching A is 1.5≤pH < 2.5, is directly leached since being leached six grades；The liquid-solid ratio by volume for water phase, press by solid
Quality meter.
7. the method that vanadium classification according to claim 3 is leached, it is characterised in that: when calcification baking clinker is Ca (VO3)2
When, water phase is mixed with calcification baking clinker by liquid-solid ratio 2.1~2.5, obtains leaching slurry A containing vanadium, adjusts leached material containing vanadium
The pH for starching A is 1.5≤pH < 2.5, is directly leached since being leached six grades；The liquid-solid ratio by volume for water phase, press by solid
Quality meter.
8. the according to claim 1, method that the described in any item vanadium classifications in 2,5,6 or 7 are leached, it is characterised in that: use quality
The sulphur acid for adjusting pH that concentration is 30~65%.
9. the method that vanadium classification according to claim 3 is leached, it is characterised in that: use mass concentration for 30~65%
Sulphur acid for adjusting pH.
10. the method that vanadium classification according to claim 4 is leached, it is characterised in that: use mass concentration for 30~65%
Sulphur acid for adjusting pH.
11. the according to claim 1, method that the described in any item vanadium classifications in 2,5,6,7,9 or 10 are leached, it is characterised in that: every
The extraction time that grade leaches is 5~10min.
12. the method that vanadium according to claim 3 classification is leached, it is characterised in that: the extraction time of every grade of leaching is 5~
10min。
13. the method that vanadium according to claim 4 classification is leached, it is characterised in that: the extraction time of every grade of leaching is 5~
10min。
14. the method that vanadium according to claim 8 classification is leached, it is characterised in that: the extraction time of every grade of leaching is 5~
10min。
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| CN105274336A (en) * | 2015-11-27 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for stabilizing leaching solution in calcification vanadium extraction process |
| CN106987716A (en) * | 2017-06-05 | 2017-07-28 | 攀钢集团研究院有限公司 | The continuous acidic leaching method of vanadium slag calcification baking clinker |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2090640C1 (en) * | 1995-10-25 | 1997-09-20 | Акционерное общество открытого типа "Ванадий-Тулачермет" | Method of recovering vanadium from slags |
| CN101412539A (en) * | 2008-11-18 | 2009-04-22 | 攀钢集团研究院有限公司 | Clean production process for vanadium oxide |
| CN105219976A (en) * | 2015-11-19 | 2016-01-06 | 攀钢集团西昌钢钒有限公司 | Improve the method for vanadium slag calcification baking grog leaching yield |
| CN105274336A (en) * | 2015-11-27 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for stabilizing leaching solution in calcification vanadium extraction process |
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