CN110408772A - A kind of method of vanadium slag roasting cleaning vanadium extraction - Google Patents
A kind of method of vanadium slag roasting cleaning vanadium extraction Download PDFInfo
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- CN110408772A CN110408772A CN201810395587.9A CN201810395587A CN110408772A CN 110408772 A CN110408772 A CN 110408772A CN 201810395587 A CN201810395587 A CN 201810395587A CN 110408772 A CN110408772 A CN 110408772A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
- C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
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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 present invention relates to a kind of methods that vanadium slag roasts cleaning vanadium extraction, the vanadium in vanadium slag is converted to using calcification baking method the calcium vanadate of high temperatures, roasting clinker is leached using the ammonium sulfate and/or ammonium bisulfate solution of high concentration, it is mixed to form most ammonium metavanadate crystallizations and tailings containing brilliant slag, then it will contain brilliant slag and be dissolved in hydrothermal solution and obtain realizing the high efficiency extraction to vanadium containing vanadium solution.The problem of present invention is volatilized there is no high temperature vanadium, the comprehensive recovery of vanadium is higher, leaching process does not generate ammonia, compared with other labile ammonium salts, under same concentrations, identical extraction temperature, the conversion ratio of vanadium is higher, while can effectively avoid the problem that ammonium metavanadate solubility is small in ammonium salt solution, vanadium recovery rate is low.Later use sulfuric acid solution absorbs the ammonia that ammonium metavanadate calcining generates, and recombines ammonium sulfate, and recycling for ammonia may be implemented, and entire technical process cleaning greatly reduces production cost, with good economic efficiency and application prospect.
Description
Technical field
The present invention relates to vanadium field of chemical metallurgical technology, and in particular to a kind of method of vanadium slag roasting cleaning vanadium extraction.
Background technique
Traditional Leaching of Vanadium from Vanadium slag method is roasting-water seaoning vanadium extraction, and wherein vanadium slag sodium roasting-water logging vanadium extraction is the mainstream of vanadium extraction
Method.This method is to help trivalent vanadium to be oxidized to pentavalent vanadium and make its turn using sodium salt additive (such as salt, saltcake, soda ash)
Turn to soluble vanadate.Sodium roasting process needs to consume a large amount of sodium salt, and vanadium recovery is low, and single roasts vanadium recovery
It is 70% or so, the rate of recovery of vanadium is also only 80% after repeatedly roasting；It need to repeatedly roast, energy consumption is higher；In roasting process
Harmful SO can be generated2、HCl、Cl2Equal subversive gas, pollute environment；Simultaneously high-temperature calcination process be easy to produce material sintering,
Kiln body ring formation phenomenon hinders the further oxidation of vanadium, and vanadium conversion ratio reduces, while reducing production efficiency.During precipitation
Big vanadium wastewater is generated, these wastewater treatment costs are higher.
Sodium roasting there are aiming at the problem that, CN102560086A proposes what a kind of calcification baking clinker ammonium carbonate leached
Extraction vanadium method, vanadium slag is with CaO/V2O5Molar ratio be 2~3 carry out calcification bakings, roasting clinker concentration be 200~800g/L
Sal volatile leaches, and extraction temperature is 60~98 DEG C, is obtained by filtration containing vanadium leachate.Ammonium hydrogen carbonate belongs to volatile ammonium salt,
And enhance rapidly as concentration increases, problem improves volatility, is leached under temperature higher strip part, leachate volatilization,
Ammonium is lost seriously, and leaching agent consumption is big, at high cost.The ammonia carbon dioxide absorption synthesizing ammonium bicarbonate process needs of loss are pressurizeing
Under the conditions of carry out, ammonium salt synthesis technology is complicated, increases production cost.CN104164569A propose a kind of vanadium slag be added calcium salt or
The method leached after magnesium salts oxidizing roasting with ammonium salt aqueous solution, calcium salt and/or magnesium salts and V2O5Molar ratio be 0.5~1.2, oxygen
Vanadium bearing slag is 30~300g/L in ammonium salt concentration after change roasting, is leached in the leaching agent that temperature is 60~200 DEG C.This method is deposited
Main problem be that extraction temperature is higher, the volatile quantity of carbon ammonium aqueous solution ammonia is big, increases cost of material and operating environment
Difference；It is leached in high-pressure closed vessel and increases equipment cost.CN103146930A proposes a kind of vanadium slag calcification baking ammonium oxalate leaching
Method out, although the volatility of ammonium oxalate is smaller, ammonium oxalate belongs to unconventional ammonium salt, and price is apparently higher than other ammonium salts,
Cost is too high, is not suitable for large-scale industrial application.
It needs to develop a kind of low production cost, vanadium high conversion rate, the Leaching of Vanadium from Vanadium slag method of clean and environmental protection at present.
Summary of the invention
It is of the invention to provide a kind of method of vanadium slag roasting cleaning vanadium extraction in view of problems of the prior art, it is whole
The problem of a technical process is volatilized there is no high temperature vanadium, the comprehensive recovery of vanadium is higher, and leaching process does not generate ammonia, with other
Labile ammonium salt is compared, and under same concentrations, identical extraction temperature, the conversion ratio of vanadium is higher, while can effectively avoid ammonium salt
The problem that ammonium metavanadate solubility is small in solution, vanadium recovery rate is low.Later use sulfuric acid solution absorbs ammonium metavanadate calcining and generates
Ammonia, recombine ammonium sulfate, may be implemented recycling for ammonia, preparation process cleaning significantly reduces production cost, has
There are good economic benefit and application prospect.
To achieve this purpose, the present invention adopts the following technical scheme:
The present invention provides a kind of methods that vanadium slag roasts cleaning vanadium extraction, the described method comprises the following steps:
(1) it is roasted after mixing vanadium slag and lime；
(2) the roasting clinker for obtaining ammonium salt solution and step (1) mixes, and carries out ammonium reaction, after the reaction was completed solid-liquid
Separation obtains liquid and the slag containing crystalline substance after ammonium；The ammonium salt is ammonium sulfate and/or ammonium hydrogen sulfate, NH in ammonium salt solution4 +Concentration is
30-60g/L；
(3) it is leached, is obtained after separation of solid and liquid containing vanadium solution containing brilliant slag to what step (2) obtained using hydrothermal solution.
The present invention substitutes the sodium salt of traditional sodium roasting with lime, can not only reduce production cost, but also will not generate
Harmful kiln gas, roasting process not ring formation.Compared with blank roasting, blank product of roasting is vanadic anhydride, is held under high-temperature roasting
It is volatile, cause the loss of vanadium.And calcium salt can generate stable metavanadic acid calcium in conjunction with vanadium, vanadium is non-volatile under high temperature, facilitates
Improve the rate of recovery of vanadium.Reaction equation is as follows:
4CaO+4FeO.V2O3+5O2=2Fe2O3+4Ca(VO3)2
Clinker after roasting extracts vanadium therein: the first step using two-step method, and clinker is added ammonium salt solution and carries out ammonium, institute
The ammonium salt used is ammonium sulfate and/or ammonium hydrogen sulfate, its advantage is that operating under normal pressure, stablizes compared with other ammonium salt properties,
It does not decompose under high temperature reaction, under same reaction time, identical initial ammonium salt concentration, the conversion ratio of vanadium is higher.Ammonium sulfate with
Metavanadic acid calcium reaction in clinker generates calcium sulfate and ammonium metavanadate.Reaction equation is as follows:
(NH4)2SO4+Ca(VO3)2=CaSO4+2NH4VO3
In traditional ammonium salt extract technology, ammonium metavanadate is leached directly into solution and then separates with tailings, however due to
Ammonium metavanadate solubility in ammonium salt solution is not high, and in direct leaching process, ammonium metavanadate crystallization in part is mixed with tailings, cannot
Into in solution, the loss of vanadium resource is in turn resulted in.
In order to overcome the above problem, the present invention is operated using second step.The present invention utilizes NH4 +Concentration is the sulphur of 30-60g/L
Sour ammonium and/or ammonium bisulfate solution leach roasting clinker, in the ammonium sulfate and/or ammonium bisulfate solution of the concentration,
Ammonium metavanadate solubility is extremely low (lower than other ammonium salt solubility), and overwhelming majority crystallization and tailings are mixed to form after ammoniumization reaction
Containing brilliant slag, i.e. ammonium metavanadate crystal coexists with tailings.Then the heat of not liquid containing ammonium sulfate and/or ammonium hydrogen sulfate will be dissolved in containing brilliant slag
It is obtained in liquid containing vanadium solution.At this point, the solubility of ammonium metavanadate is higher, can effectively leach containing the vanadium in brilliant slag.
The present invention extracts the vanadium in roasted vanadic slag using two-step method, and it is molten to can effectively avoid ammonium metavanadate in ammonium salt solution
The problem that Xie Du is small, vanadium recovery rate is low.
Vanadic anhydride product and ammonia, ammonia are generated after ammonium metavanadate crystal calcining and decomposing can be given birth to again with sulfuric acid absorption
At ammonium sulfate or ammonium hydrogen sulfate, ammonium chemical industry sequence is returned to after being concentrated by evaporation, therefore, ammonia realizes interior in entire process flow
Circulation, without any exhaust gas, discharge of wastewater.
According to the present invention, according to CaO/V2O5For (1-1.9): 1 molar ratio in step (1) lime and vanadium slag carry out
Proportion, the molar ratio can be 1:1,1.1:1,1.2:1,1.3:1,1.4:1,1.5:1,1.6:1,1.7:1,1.8:1 or
Specific point value between 1.9:1 and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature of step (1) described roasting is 800-950 DEG C, such as can be 800 DEG C, 830 DEG C, 850
DEG C, 880 DEG C, 900 DEG C, 920 DEG C or the specific point value between 950 DEG C and above-mentioned numerical value, examining as space is limited and for concise
Consider, the present invention no longer exclusive list.
According to the present invention, the time of step (1) described roasting be 0.5-2h, such as can be 0.5h, 0.8h, 1h, 1.2h,
Specific point value between 1.5h, 1.8h or 2h and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is no longer
Exclusive list.
According to the present invention, NH in step (2) described ammonium salt solution4 +Concentration is 30-60g/L, for example, can be 30g/L,
33g/L, 35g/L, 40g/L, 43g/L, 45g/L, 48g/L, 50g/L, 53g/L, 55g/L, 58g/L or 60g/L and above-mentioned number
Specific point value between value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, it is (3-5) that the liquid of step (2) ammonium salt solution and roasting clinker, which consolidates mass ratio: 1, such as can
To be specific between 3:1,3.3:1,3.5:1,3.7:1,4:1,4.2:1,4.5:1,4.8:1 or 5:1 and above-mentioned numerical value
Value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature of step (2) the ammoniumization reaction is 85-95 DEG C, such as can be 85 DEG C, 86 DEG C, 87
DEG C, 88 DEG C, 89 DEG C, 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C, 94 DEG C or the specific point value between 95 DEG C and above-mentioned numerical value, be limited to a piece
Width and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the time of step (2) ammoniumization reaction is 0.1-0.48h, for example, can be 0.1h, 0.15h,
Specific point value between 0.2h, 0.25h, 0.3h, 0.35h, 0.4h, 0.45h or 0.48h and above-mentioned numerical value, as space is limited and
For concise consideration, the present invention no longer exclusive list.
According to the present invention, the concentration of ammonium metavanadate is 1-2g/L in liquid after the ammonium that step (2) obtains, such as be can be
1g/L, 1.1g/L, 1.2g/L, 1.3g/L, 1.4g/L, 1.5g/L, 1.6g/L, 1.7g/L, 1.8g/L, 1.9g/L or 2g/L, with
And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, it before step (3) hydrothermal solution leaches, is washed to containing brilliant slag, the washing is three stage countercurrents
Washing, wash water dosage are 0.5-1 times containing brilliant slag butt quality.
Step (3) the of the present invention hydrothermal solution is the process water of heating, liquid after the subsequent ammonium metavanadate crystallization preferably heated
(circulation crystallization mother liquor).
According to the present invention, the temperature that step (3) hydrothermal solution leaches is 80-98 DEG C, such as can be 80 DEG C, 83 DEG C, 85
DEG C, 88 DEG C, 90 DEG C, 93 DEG C, 95 DEG C or the specific point value between 98 DEG C and above-mentioned numerical value, as space is limited and for concise
Consider, the present invention no longer exclusive list.
According to the present invention, the time that step (3) hydrothermal solution leaches is 1-3h, for example, can be 1h, 1.3h, 1.5h,
Specific point value between 1.8h, 2h, 2.3h, 2.5h, 2.8h or 3h and above-mentioned numerical value is examined as space is limited and for concise
Consider, the present invention no longer exclusive list.
According to the present invention, the concentration containing ammonium metavanadate in vanadium solution that step (3) obtains is 20-50g/L, such as be can be
Specific point value between 20g/L, 25g/L, 30g/L, 35g/L, 40g/L, 45g/L or 50g/L and above-mentioned numerical value, is limited to a piece
Width and for concise consideration, the present invention no longer exclusive list.
According to the present invention, liquid after the crystallisation by cooling containing vanadium solution that step (3) obtains being obtained ammonium metavanadate crystal and crystallized,
It calcines the ammonium metavanadate crystal to obtain vanadic anhydride and ammonia, by gained ammonia using obtaining ammonium sulfate after sulfuric acid absorption
And/or ammonium bisulfate solution, liquid, which mixes to be back in step (2) after evaporation and concentration, after the ammonium obtained with step (2) carries out ammonium
Change reaction.
According to the present invention, it will be used in step (3) leach to containing brilliant slag as hydrothermal solution after liquid heating after the crystallization.
According to the present invention, the crystallization outlet temperature of the ammonium metavanadate is 30-40 DEG C, such as can be 30 DEG C, 31 DEG C, 32
DEG C, 33 DEG C, 34 DEG C, 35 DEG C, 36 DEG C, 37 DEG C, 38 DEG C, 39 DEG C or the specific point value between 40 DEG C and above-mentioned numerical value, be limited to a piece
Width and for simple consideration, the present invention no longer exclusive list.
According to the present invention, the ammonium metavanadate crystal seed of 0.2-1.0g/L is added in the ammonium metavanadate crystallization process.
According to the present invention, the concentration of the sulfuric acid solution be 50-100g/L, such as can be 50g/L, 55g/L, 60g/L,
Specific point value between 65g/L, 70g/L, 75g/L, 80g/L, 85g/L, 90g/L or 100g/L and above-mentioned numerical value, is limited to a piece
Width and for simple consideration, the present invention no longer exclusive list.
According to the present invention, temperature is 30- during the ammonia and sulfuric acid synthesize ammonium sulfate and/or ammonium bisulfate solution
70 DEG C, such as can be between 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C or 70 DEG C and above-mentioned numerical value
Specific point value, as space is limited and for simple consideration, the present invention no longer exclusive list.
As a preferred technical solution, the method for the invention the following steps are included:
(1) according to CaO/V2O5For (1-1.9): 1 molar ratio mixes vanadium slag and lime, in 800-950 DEG C of roasting 0.5-
2h；
(2) consolidating mass ratio according to liquid is (3-5): the 1 roasting clinker for obtaining ammonium salt solution and step (1) mixes, 85-95
Ammoniumization is carried out at DEG C and reacts 0.1-0.48h, is separated by solid-liquid separation after the reaction was completed, after obtaining the ammonium that ammonium metavanadate concentration is 1-2g/L
Liquid and the slag containing crystalline substance；The ammonium salt is ammonium sulfate and/or ammonium hydrogen sulfate, NH in ammonium salt solution4 +Concentration is 30-60g/L；
(3) three-level countercurrent washing is carried out containing brilliant slag to what step (2) obtained, wash water dosage is containing brilliant slag butt quality
It 0.5-1 times, is then leached using hydrothermal solution to containing brilliant slag, extraction temperature is 80-98 DEG C, time 1-3h, after separation of solid and liquid
Obtaining ammonium metavanadate concentration is 20-50g/L containing vanadium solution；
(4) liquid after the crystallisation by cooling containing vanadium solution that step (3) obtains being obtained ammonium metavanadate crystal and crystallized, crystallizes terminal
Temperature is 30-40 DEG C, and the ammonium metavanadate crystal seed of 0.2-1.0g/L is added in crystallization process；Make after liquid heating after gained is crystallized
It is hydrothermal solution for being leached in step (3) to containing brilliant slag；
(5) it calcines the ammonium metavanadate crystal that step (4) obtains to obtain vanadic anhydride and ammonia, it, will at 30-70 DEG C
Gained ammonia is using ammonium sulfate and/or ammonium bisulfate solution is obtained after the sulfuric acid absorption that concentration is 50-100g/L, with step (2)
Liquid mixing is back in step (2) after being concentrated by evaporation and carries out ammonium reaction after obtained ammonium.
Compared with prior art, the present invention is at least had the advantages that
(1) present invention converts the vanadium in vanadium slag to using calcification baking method the calcium vanadate of high temperatures, less adds
The problem of blank of any additive roasts, and there is no the volatilizations of high temperature vanadium, the comprehensive recovery of vanadium is higher.
(2) present invention is using ammonium sulfate and/or ammonium hydrogen sulfate as leaching agent, and ammonium salt medium is stablized, in normal pressure leaching mistake
Journey does not generate ammonia, can significantly improve leaching environment, improves the operability of leaching process.Also, with other labile ammoniums
Salt is compared, and under same concentrations, identical extraction temperature, the conversion ratio of vanadium is higher.
(3) present invention leaches roasting clinker using the ammonium sulfate and/or ammonium bisulfate solution of high concentration, makes big absolutely
The crystallization of part ammonium metavanadate and tailings are mixed to form containing brilliant slag, then will be contained brilliant slag and are dissolved in hydrothermal solution and obtain containing vanadium solution, can
Effectively to leach the recovery rate for substantially increasing vanadium containing the vanadium in brilliant slag.
(4) ammonia that ammonium metavanadate calcining of the present invention generates, carries out absorption using sulfuric acid solution and recombines ammonium sulfate, can
To realize recycling for ammonia, entire technical process non-wastewater discharge.Ammonium sulfate synthesis can be carried out in normal pressure.
(5) Si, S and P in vanadium slag can effectively fix by calcium being added in roasting process, ammonium leaching avoid in the process these impurity into
Enter vanadium liquid, the vanadium product of high-purity can be prepared.
(6) reagent of this method actual consumption is sulfuric acid, and reagent consumption is few, and vanadium extraction cost is extremely low.
Detailed description of the invention
Fig. 1 is the process flow chart that a kind of specific embodiment of the present invention provides.
The present invention is described in more detail below.But following examples is only simple example of the invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, of the invention is typical but non-limiting
Embodiment is as follows:
Embodiment 1
As shown in Figure 1, the present invention carries out vanadium extraction in accordance with the following methods:
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1:1 is uniformly mixed, and high temperature roasting is carried out in rotary kiln
It burns, maturing temperature is 900 DEG C, calcining time 1h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 50g/L, ammoniumization temperature
Degree is 80 DEG C, and it is 3:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.1h, is filtered after the reaction was completed, and obtaining ammonium metavanadate concentration is 2g/L
Ammonium after liquid and containing brilliant slag；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.5 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 80 DEG C, extraction time 3h, is filtered after the completion of leaching
It obtains containing vanadium solution, is 30g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 30 DEG C, crystallization process
Middle addition crystal seed 0.3g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 50 DEG C, uses 50g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium sulfate, is concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
98.2%, purity of vanadium pentoxide 99.66%.
Embodiment 2
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.2:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 800 DEG C, calcining time 0.8h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 40g/L, ammoniumization temperature
Degree is 82 DEG C, and it is 3.5:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.2h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1.6g/L；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.55 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 85 DEG C, extraction time 2.4h, mistake after the completion of leaching
Filter is obtained containing vanadium solution, is 25g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 38 DEG C, crystallization process
Middle addition crystal seed 0.3g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 40 DEG C, uses 65g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium sulfate, is concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
97.9%, purity of vanadium pentoxide 99.56%.
Embodiment 3
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.7:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 850 DEG C, calcining time 0.5h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 50g/L, ammoniumization temperature
Degree is 85 DEG C, and it is 4.6:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.3h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1g/L；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.5 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 90 DEG C, extraction time 2.2h, mistake after the completion of leaching
Filter is obtained containing vanadium solution, is 30g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 32 DEG C, crystallization process
Middle addition crystal seed 0.4g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 50 DEG C, uses 55g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium sulfate, is concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
98.1%, purity of vanadium pentoxide 99.76%.
Embodiment 4
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.4:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 910 DEG C, calcining time 1.2h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 60g/L, ammoniumization temperature
Degree is 86 DEG C, and it is 4.2:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.4h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1.8g/L；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.6 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 86 DEG C, extraction time 2h, is filtered after the completion of leaching
It obtains containing vanadium solution, is 35g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 33 DEG C, crystallization process
Middle addition crystal seed 0.5g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 60 DEG C, uses 60g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium sulfate, is concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
97.8%, purity of vanadium pentoxide 99.86%.
Embodiment 5
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.5:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 930 DEG C, calcining time 1.5h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 55g/L, ammoniumization temperature
Degree is 88 DEG C, and it is 3.6:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.48h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1g/L；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.7 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 94 DEG C, extraction time 1.6h, mistake after the completion of leaching
Filter is obtained containing vanadium solution, is 40g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 35 DEG C, crystallization process
Middle addition crystal seed 0.6g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 60 DEG C, uses 70g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium sulfate, is concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
97.9%, purity of vanadium pentoxide 99.96%.
Embodiment 6
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.6:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 950 DEG C, calcining time 1.6h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 44g/L, ammoniumization temperature
Degree is 90 DEG C, and it is 3.5:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.25h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1.6g/L；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.8 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 96 DEG C, extraction time 1.5h, mistake after the completion of leaching
Filter is obtained containing vanadium solution, is 45g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 36 DEG C, crystallization process
Middle addition crystal seed 0.7g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 65 DEG C, uses 80g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium sulfate, is concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
98.2%, purity of vanadium pentoxide 99.68%.
Embodiment 7
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.8:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 830 DEG C, calcining time 1.8h；
(2) clinker after roasting is added in ammonium bisulfate solution and carries out ammonium, NH in solution4 +Concentration is 33g/L, ammonium
Temperature is 92 DEG C, and it is 4:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.35h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1.5g/L；
(3) three-level countercurrent washing is carried out to containing brilliant slag with 0.9 times of its dry weight of wash water, liquid is mixed after washing lotion and ammonium
It closes, by leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 98 DEG C, extraction time 1.2h, mistake after the completion of leaching
Filter is obtained containing vanadium solution, is 50g/L containing ammonium metavanadate concentration in vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 38 DEG C, crystallization process
Middle addition crystal seed 0.8g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 55 DEG C, uses 90g/
The sulfuric acid solution of L absorbs the ammonia that calcining and decomposing generates and obtains ammonium bisulfate solution, evaporates after it is mixed with liquid after ammonium dense
Contracting is then return to step (2) circulation for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
97.7%, purity of vanadium pentoxide 99.73%.
Embodiment 8
(1) by lime and vanadium slag according to CaO:V2O5The molar ratio of=1.9:1 is uniformly mixed, and high temperature is carried out in rotary kiln
Roasting, maturing temperature are 860 DEG C, calcining time 2h；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 35g/L, ammoniumization temperature
Degree is 95 DEG C, and it is 5:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.45h, is filtered after the reaction was completed, obtaining ammonium metavanadate concentration is
Liquid and the slag containing crystalline substance after the ammonium of 1.3g/L；
(3) three-level countercurrent washing being carried out to containing brilliant slag with 1 times of its dry weight of wash water, washing lotion is mixed with liquid after ammonium,
By leaching after washing containing brilliant slag addition hydrothermal solution, extraction temperature is 95 DEG C, extraction time 3h, is obtained by filtration after the completion of leaching
It is 48g/L containing ammonium metavanadate concentration in vanadium solution containing vanadium solution；
(4) vanadium solution will be contained, ammonium metavanadate crystal is obtained by crystallisation by cooling, control outlet temperature is 40 DEG C, crystallization process
Middle addition crystal seed 1g/L, calcines obtained ammonium metavanadate crystal to obtain high-purity vanadium pentoxide, at 45 DEG C, uses 100g/L
Sulfuric acid solution absorb calcining and decomposing generate ammonia obtain ammonium sulfate, be concentrated by evaporation after it is mixed with liquid after ammonium,
Step (2) circulation is then return to for ammonium.
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
98.3%, purity of vanadium pentoxide 99.59%.
Comparative example 1
Compared with Example 1, in addition to the ammonium carbonate that leaching agent ammonium sulfate is replaced with same concentrations in step (2) is molten
Outside liquid, other steps and condition are identical with embodiment 1 (except step 4), and as a result the leaching rate that turns of vanadium is 88.3%, and is soaked
Ammonium bicarbonate is easy to decompose obvious during out, can smell strong impulse ammonia taste.
Compared with Example 1, the leaching rate that turns of vanadium is only 88.3% in this comparative example, than reducing nearly in embodiment 1
10%, this is because in identical NH4 +Concentration, temperature and under conditions of the reaction time, ammonium carbonate are easier to occur point than ammonium sulfate
Solution generates ammonia, and with temperature and NH4 +Concentration is higher, and decomposition is more violent, causes NH4 +Concentration is decomposed loss, NH4 +
Concentration reduces the leaching rate for influencing vanadium, and therefore, under same initial ammonium salt concentration, vanadium turns leaching rate not as good as ammonium sulfate.
Comparative example 2
(1) with 1 step of embodiment (1)；
(2) clinker after roasting is added in ammonium sulfate and carries out ammonium, NH in solution4 +Concentration is 8g/L, ammoniumization temperature
Degree is 80 DEG C, and it is 3:1 that liquid, which consolidates mass ratio, and the ammonium time is 0.1h, is filtered after the reaction was completed, is obtained containing vanadium solution and tailings；
(3) with 1 step of embodiment (4).
Compared with Example 1, this comparative example leaches clinker using the ammonium sulfate of low concentration, leaches and completes
Afterwards, solution and tailings containing ammonium metavanadate are directly obtained, after testing, the leaching rate that turns of vanadium is 86.1%, it is clear that be lower than real
Apply example 1.
Comparative example 3
(1) with 1 step of embodiment (1)；
(2) leaching agent ammonium sulfate is replaced with to the ammonium oxalate solution of same concentrations, remaining condition is identical；Leaching process
It is middle to find the phenomenon that scabs, it finds that the main component to scab is calcium oxalate after analyzing, is filtered after reaction, it is dense to obtain ammonium metavanadate
Liquid and the slag containing crystalline substance after the ammonium that degree is 8g/L.
(3) same to embodiment step (3), the concentration of ammonium metavanadate containing vanadium solution is 22g/L after leaching；
(4) with 1 step of embodiment (4).
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
91.2%.
Compared with Example 1, the leaching rate that turns of vanadium is only 91.2% in this comparative example, than reducing nearly in embodiment 1
10%, it is seen then that ammonium oxalate leaching rate is obviously not so good as ammonium sulfate.The ammonium metavanadate of liquid is at concentrations up to 8g/L after ammonium, and ammonium sulfate
Ammonium metavanadate concentration is only 2g/L in system, this illustrates that a big chunk ammonium metavanadate recycles in system always, and entrance is next
The ammonium metavanadate for walking molten vanadium is less, and the vanadium recovery recycled every time is lower, and extraction efficiency is low.In addition, calcium oxalate scabs, problem will
The continuity of leaching process can be seriously affected.
Comparative example 4
(1) with 1 step of embodiment (1)；
(2) leaching agent ammonium sulfate is replaced with to the ammonium phosphate solution of same concentrations, remaining condition is identical, mistake after reaction
Filter obtains liquid and the slag containing crystalline substance after the ammonium that ammonium metavanadate concentration is 12g/L；
(3) same to embodiment step (3), it is 20g/L that ammonium metavanadate concentration in vanadium solution is contained after leaching；
(4) with 1 step of embodiment (4).
By tailings through the content of vanadium in hot water washing, drying, weighing post analysis tailings, the leaching rate that turns through detecting vanadium is
83.2%.
Compared with Example 1, the leaching rate that turns of vanadium is only 83.2% in this comparative example, more many than reducing in embodiment 1, can
See, ammonium phosphate leaching rate is obviously not so good as ammonium sulfate.The ammonium metavanadate of liquid is at concentrations up to 12g/L after ammonium, and in ammonium sulphate system
Ammonium metavanadate concentration is only 2g/L, this illustrates that a big chunk ammonium metavanadate recycles in system always, into molten vanadium in next step
Ammonium metavanadate it is less, the vanadium recovery recycled every time is lower, and extraction efficiency is low.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of method of vanadium slag roasting cleaning vanadium extraction, which is characterized in that the described method comprises the following steps:
(1) it is roasted after mixing vanadium slag and lime；
(2) the roasting clinker for obtaining ammonium salt solution and step (1) mixes, and carries out ammonium reaction, is separated by solid-liquid separation after the reaction was completed,
Obtain after ammonium liquid and containing brilliant slag；The ammonium salt is ammonium sulfate and/or ammonium hydrogen sulfate；
(3) it is leached, is obtained after separation of solid and liquid containing vanadium solution containing brilliant slag to what step (2) obtained using hydrothermal solution.
2. the method as described in claim 1, which is characterized in that according to CaO/V2O5For (1-1.9): 1 molar ratio is to step
(1) lime and vanadium slag in are matched.
3. method according to claim 1 or 2, which is characterized in that the temperature of step (1) described roasting is 800-950 DEG C；
Preferably, the time of step (1) described roasting is 0.5-2h.
4. the method according to claim 1, which is characterized in that NH in step (2) described ammonium salt solution4 +Concentration is
30-60g/L；
Preferably, it is (3-5) that the liquid of step (2) ammonium salt solution and roasting clinker, which consolidates mass ratio: 1；
Preferably, the temperature of step (2) the ammoniumization reaction is 85-95 DEG C；
Preferably, the time of step (2) the ammoniumization reaction is 0.1-0.48h；
Preferably, the concentration of ammonium metavanadate is 1-2g/L in liquid after the ammonium that step (2) obtains.
5. method according to any of claims 1-4, which is characterized in that before step (3) hydrothermal solution leaches, to containing brilliant slag
It is washed；
Preferably, the washing is three-level countercurrent washing, and wash water dosage is 0.5-1 times containing brilliant slag butt quality.
6. the method according to claim 1 to 5, which is characterized in that the temperature that step (3) hydrothermal solution leaches is 80-
98℃；
Preferably, the time that step (3) hydrothermal solution leaches is 1-3h；
Preferably, the concentration containing ammonium metavanadate in vanadium solution that step (3) obtains is 20-50g/L.
7. as the method according to claim 1 to 6, which is characterized in that the cooling containing vanadium solution for obtaining step (3) is tied
Crystalline substance obtains liquid after ammonium metavanadate crystal and crystallization, calcines the ammonium metavanadate crystal to obtain vanadic anhydride and ammonia, by institute
Ammonia is obtained using ammonium sulfate and/or ammonium bisulfate solution is obtained after sulfuric acid absorption, liquid mixes steaming after the ammonium obtained with step (2)
It is back in step (2) after hair concentration and carries out ammonium reaction.
8. the method for claim 7, which is characterized in that the crystallization outlet temperature of the ammonium metavanadate is 30-40 DEG C；
Preferably, the ammonium metavanadate crystal seed of 0.2-1.0g/L is added in the ammonium metavanadate crystallization process；
Preferably, it will be used in step (3) leach to containing brilliant slag as hydrothermal solution after liquid heating after the crystallization.
9. method as claimed in claim 7 or 8, which is characterized in that the concentration of the sulfuric acid solution is 50-100g/L；
Preferably, temperature is 30-70 DEG C during the ammonia and sulfuric acid synthesize ammonium sulfate and/or ammonium bisulfate solution.
10. such as the described in any item methods of claim 1-9, which is characterized in that the described method comprises the following steps:
(1) according to CaO/V2O5For (1-1.9): 1 molar ratio mixes vanadium slag and lime, in 800-950 DEG C of roasting 0.5-2h；
(2) consolidating mass ratio according to liquid is (3-5): the 1 roasting clinker for obtaining ammonium salt solution and step (1) mixes, at 85-95 DEG C
Carry out ammoniumization react 0.1-0.48h, be separated by solid-liquid separation after the reaction was completed, obtain ammonium metavanadate concentration be 1-2g/L ammonium after liquid and
Containing brilliant slag；The ammonium salt is ammonium sulfate and/or ammonium hydrogen sulfate, NH in ammonium salt solution4 +Concentration is 30-60g/L；
(3) three-level countercurrent washing is carried out containing brilliant slag to what step (2) obtained, wash water dosage is the 0.5-1 containing brilliant slag butt quality
Times, it is then leached using hydrothermal solution to containing brilliant slag, extraction temperature is 80-98 DEG C, time 1-3h, is obtained after separation of solid and liquid partially
Vanadic acid ammonium concentration is 20-50g/L containing vanadium solution；
(4) liquid after the crystallisation by cooling containing vanadium solution that step (3) obtains being obtained ammonium metavanadate crystal and crystallized, crystallizes outlet temperature
It is 30-40 DEG C, the ammonium metavanadate crystal seed of 0.2-1.0g/L is added in crystallization process；As heat after liquid heating after gained is crystallized
Liquid in step (3) to containing brilliant slag for leaching；
(5) it calcines the ammonium metavanadate crystal that step (4) obtains to obtain vanadic anhydride and ammonia, at 30-70 DEG C, by gained
Ammonia is obtained using ammonium sulfate and/or ammonium bisulfate solution is obtained after the sulfuric acid absorption that concentration is 50-100g/L with step (2)
Ammonium after liquid mixing be concentrated by evaporation after be back in step (2) and carry out ammonium reaction.
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| CN114644357A (en) * | 2022-03-11 | 2022-06-21 | 万循材料科技有限公司 | Method for preparing ammonium metavanadate by sodium modification vanadium extraction combined alkali preparation and low-cost vanadium slag utilization |
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