CN102851487A - Mixture, method for recovering ferro-vanadium bag dedusting material, and vanadium extraction method - Google Patents
Mixture, method for recovering ferro-vanadium bag dedusting material, and vanadium extraction method Download PDFInfo
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Abstract
The invention provides a method for recovering ferro-vanadium bag dedusting material, and a mixture obtained by the method. The method includes mixing ferro-vanadium bag dedusting material with oxidizing-sodiumizing-calcining return slag. The invention also provides a vanadium extraction method, which includes mixing the mixture with refined vanadium slag and sodiumizing agent, and performing oxidizing-sodiumizing-calcining to obtain clinker; leaching the clinker with water to obtain leachate; removing phosphorus and silicon from the leachate to obtain a qualified solution; and performing vanadium precipitation to the qualified solution with acidic ammonium salt to obtain red vanadium. The method for recovering ferro-vanadium bag dedusting material effectively realizes recovery of the ferro-vanadium bag dedusting material, without effect on the quality of the oxidizing-sodiumizing-calcining return slag. The vanadium extraction method effectively realizes the recovery of the ferro-vanadium bag dedusting material.
Description
Technical field
The present invention relates to a kind of method that reclaims vanadium iron bag-type dust material and a kind of mixture that is obtained by the method for this recovery vanadium iron bag-type dust material and a kind of method of vanadium extraction.
Background technology
When vanadium iron is smelted, smelting furnace top will produce a large amount of vanadium powder dirt that contain, this dust at first enters in the tornado dust collector under the dedusting wind action, heavy material just rests on becomes vanadium iron cyclone dust removal material in the tornado dust collector, the material that proportion is little just enters in the sack cleaner along the center of tornado dust collector whirlwind, because the cloth bag of sack cleaner intercepts, this material just rests on the sack cleaner bottom becomes vanadium iron bag-type dust material.Vanadium iron bag-type dust material is discharged by the discharging spiral of sack cleaner bottom, and its pack (fitted tube) is prepared for the processing of lower step.V in the vanadium iron bag-type dust material
2O
5Content is the 15-30 % by weight, and vanadium is important strategic materials, and does not reclaim and will produce serious environmental issue, therefore must reclaim it.
Current, generally by being sneaked into, vanadium iron bag-type dust material reclaims vanadium iron bag-type dust material in the corundum slag that produces in the smelting ferrovanadium process, this compound is used for vanadium extraction raw material or refractory materials, but this recovery method exists because of the meticulous difficult recovery of vanadium iron bag-type dust material, causes the defective of larger vanadium loss.Another kind of way is by adding binding agent ball processed in vanadium iron bag-type dust material, when vanadium iron is smelted spherical vanadium iron bag-type dust material being added in the smelting furnace to reclaim the vanadium in the vanadium iron bag-type dust material.But, therefore because the content of vanadium in the vanadium iron bag-type dust material is unstable and material gently affects the grade of vanadium iron finished product, and this dedusting material contains the elements such as higher Al, Mg, Mn, therefore affect the quality of vanadium iron finished product.Production has caused certain disadvantageous effect to vanadium iron for these.
This shows how effectively to reclaim vanadium iron bag-type dust material and remain problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of method of vanadium iron cloth dedusting material and method of a kind of mixture and a kind of vanadium extraction of reclaiming.
From background technology, learn, all there is defective in the method for the various recovery bag-type dust material of prior art, and the method for seeking a kind of effective recovery vanadium iron bag-type dust material remains problem demanding prompt solution, the present inventor finally finds through long-term groping, can reclaim vanadium iron bag-type dust material by utilizing the return slag in the sodium oxide baking stove.Finished the present invention based on this discovery.
The invention provides a kind of method that reclaims vanadium iron bag-type dust material, the method comprises: vanadium iron bag-type dust material is mixed with the sodium oxide baking return slag.
The mixture that the present invention also provides the method by above-mentioned recovery vanadium iron bag-type dust material to obtain.
The present invention also provides a kind of method of vanadium extraction, and the method comprises: with mixture of the present invention with carry out sodium oxide baking after smart vanadium slag, sodium agent mix and obtain grog; Described grog leaching is obtained leach liquor; To obtain qualifying liquid behind described leach liquor dephosphorization, the silica removal; Described qualifying liquid is carried out the acid ammonium salt precipitation obtain red vanadium.
The method of recovery vanadium iron bag-type dust material of the present invention has effectively realized the recovery of vanadium iron bag-type dust material, and, can not affect the quality of sodium oxide baking return slag.
The method of vanadium extraction of the present invention has effectively realized the recovery of vanadium in the vanadium iron bag-type dust material.Adopt method of the present invention to carry out vanadium extraction, the sodium oxide baking process is smooth, filtration procedure smoothly, acid ammonium salt precipitation process is smooth, whole production process, steady running, and the finished product V that obtains of reduction
2O
3Or the sheet vanadium (V that obtains of fusing
2O
5) quality controllable.And adopt method of the present invention, the K in the vanadium iron bag-type dust material approximately 90% enters in waste and the waste water, only has an appointment 10% to enter finished product V
2O
3Or sheet vanadium (V
2O
5) in.
Embodiment
The method of recovery vanadium iron bag-type dust material of the present invention comprises: vanadium iron bag-type dust material is mixed with the sodium oxide baking return slag.
According to method of the present invention, can be so that vanadium iron bag-type dust material be effectively reclaimed as long as vanadium iron bag-type dust material is mixed with the sodium oxide baking return slag, and the particle owing to vanadium iron bag-type dust material is very thin in the industrial production, therefore cause that easily thereby dust raising phenomenon causes environmental pollution, therefore, the present inventor's research is thought, under the preferable case, should select the suitable return slag of water content, more preferably described sodium oxide baking return slag contains the above water of 10 % by weight, and in order to make vanadium iron bag-type dust material of the present invention obtain more effective recovery, under the preferable case, the water that contains the 15-25 % by weight in the described sodium oxide baking return slag more preferably contains the water of 18-22 % by weight.
Among the present invention, optional a wider range of the weight ratio of described vanadium iron bag-type dust material and sodium oxide baking return slag, under the preferable case, the weight ratio of described vanadium iron bag-type dust material and sodium oxide baking return slag is not higher than 1: 4, is preferably not to be higher than 1: 10.
Among the present invention, described sodium oxide baking return slag refers to return in the industry tailings (also claiming waste) that the sodium oxide baking grog of roasting system obtains after leaching, be called the sodium oxide baking return slag according to the method for those skilled in the art's custom.
The present invention to the kind of described sodium oxide baking return slag without particular requirement, meeting the sodium oxide baking return slag that the present invention requires and all can realize purpose of the present invention in the existing various sodium oxide baking stove, under the preferable case, in oxide compound, with the dry weight basis of sodium oxide baking return slag, contain the V of 0.9-5.5 % by weight in the described sodium oxide baking return slag
2O
5, the 3-10 % by weight Na
2The K of O, 0.05-0.3 % by weight
2The SiO of O, 5-25 % by weight
2, the MnO of 4-10 % by weight, the MgO of 2-8 % by weight, the Fe of 20-50 % by weight
2O
3, the CaO of 0.5-6 % by weight, the TiO of 5-25 % by weight
2, the 1-6 % by weight Al
2O
3And the Cr of 0.5-8 % by weight
2O
3
Without particular requirement, existing various vanadium iron bag-type dust material all can reclaim by method of the present invention, in oxide compound, with the dry weight basis of vanadium iron bag-type dust material, contain the V of 15-30 % by weight to the kind of described vanadium iron bag-type dust material in the present invention
2O
5, the 10-40 % by weight Na
2The K of O, 5-20 % by weight
2The SiO of O, 0.5-5 % by weight
2, the 0.5-5 % by weight Fe
2O
3, the MnO of 0.2-4 % by weight, the Al of 5-20 % by weight
2O
3, the MgO of 10-30 % by weight and 0.5-8 % by weight the described vanadium iron bag-type dust material of CaO can access better recovery by method of the present invention, therefore, under the preferable case, in oxide compound, with the dry weight basis of vanadium iron bag-type dust material, described vanadium iron bag-type dust material contains the V of 15-30 % by weight
2O
5, the 10-40 % by weight Na
2The K of O, 5-20 % by weight
2The SiO of O, 0.5-5 % by weight
2, the 0.5-5 % by weight Fe
2O
3, the MnO of 0.2-4 % by weight, the Al of 5-20 % by weight
2O
3, the MgO of 10-30 % by weight, the CaO of 0.5-8 % by weight.
Among the present invention, dry weight refers to the weight after mixture is sloughed water, refer to weight after the sodium oxide baking return slag is sloughed water such as the dry weight of sodium oxide baking return slag, the dry weight of vanadium iron bag-type dust material refers to the weight after vanadium iron bag-type dust material is sloughed water, and the dry weight of smart vanadium slag refers to the weight after smart vanadium slag is sloughed water.
The present invention also provides a kind of mixture that obtains according to the method for recovery vanadium iron bag-type dust material of the present invention, and the sodium oxide baking return slag that this mixture can be used as in the industrial production uses.
The invention provides a kind of method of vanadium extraction, the method comprises: with mixture of the present invention with carry out sodium oxide baking after smart vanadium slag, sodium agent mix and obtain grog; Described grog leaching is obtained leach liquor; To obtain qualifying liquid behind described leach liquor dephosphorization, the silica removal; Described qualifying liquid is carried out the acid ammonium salt precipitation obtain red vanadium.
Under the preferable case, method of the present invention also comprises; Described red vanadium press filtration, dry rear reduction are obtained vanadous oxide, or will obtain sheet vanadium (described vanadium also claims Vanadium Pentoxide in FLAKES) after the fusing after the described red vanadium press filtration.
Among the present invention, described mixture of the present invention can be carried out with reference to prior art with the method for carrying out sodium oxide baking after smart vanadium slag, sodium agent mix and obtain grog, for example described mixture, smart vanadium slag can be sent into after the sodium agent mixes and be carried out sodium oxide baking in the retort furnace and obtain grog; Also smart vanadium slag and sodium agent can be mixed to get the mixture that contains smart vanadium slag and sodium agent, then the described mixture of smart vanadium slag and sodium agent, mixture of the present invention of containing be sent into respectively wedge furnance (rotary kiln) and carried out sodium oxide baking and obtain grog.
Among the present invention, optional a wider range of the amount ratio of described smart vanadium slag, sodium agent and mixture, can select according to concrete needs, under the preferable case, described smart vanadium slag, sodium agent and mixture are mixed into furnace charge in stoving oven, so that the TV of furnace charge is the 3.5-6.0 % by weight, the Na/V mol ratio is 1.2-2, more preferably the TV of furnace charge is the 4.2-4.8 % by weight, and the Na/V mol ratio is 1.4-1.6.Generally speaking, when take yellow soda ash as the sodium agent, the weight ratio of controlling described smart vanadium slag, sodium agent and mixture is 10: 2-3: 8-12, more preferably 10: 2.3-2.5: during 9.5-10.5, the TV that can realize described furnace charge is the 3.5-6.0 % by weight, the Na/V mol ratio is 1.2-2, and more preferably the TV of furnace charge is the 4.2-4.8 % by weight, and the Na/V mol ratio is 1.4-1.6.
Furnace charge described in the present invention namely refers to the material that smart vanadium slag, sodium agent and mixture are mixed to get in stoving oven, those skilled in the art's custom is referred to as furnace charge.
Among the present invention to the method for described leaching without particular requirement (those skilled in the art also often claim to leach), can carry out according to prior art, it can also can be the leaching method of continous way for step leaching method.
Wherein known step leaching method has three to soak four and wash leaching method or three and soak three and wash leaching method, described three soak four washes to refer to and adopt to leach reagent and leach, filter afterwards, obtain for the first time leach liquor, the solid that again filtration is obtained hockets and leaches and filter, triplicate like this, the filtrate that obtains is merged as leach liquor for follow-up vanadium extraction, filter cake after the filtration then washes with water four times again, the washings (those skilled in the art's custom is called thin liquid) that obtains is collected the leaching reagent as next batch, and filter cake is then discarded as waste.Described three soak three washes similarly, and the number of times that just washes with water is three times.Wherein no matter be three soak four wash leaching method or three soak three wash the equal preferably water of leaching method and leach temperature of reagent be not less than 85 ℃, each leaching time is not less than 15min.Under the preferable case, with respect to the grog that will leach, the consumption of water and leaching reagent is preferably 28-32g/L so that [V] of leach liquor is 20-40g/L; And the TV that grog is leached rear gained tailings is not higher than 0.15%, for the consumption realizing water and leach reagent so that [V] of leach liquor is 20-40g/L, be preferably 28-32g/L; And the TV that grog is leached rear gained tailings is not higher than 0.15%, and the consumption that generally can control water or leaching reagent is 1-2 times of clinker quality.
Leach reagent among the present invention and can be the various leaching reagent of prior art, for example can be water and/or above-mentioned washings (also claiming thin liquid).Adopt above-mentioned washings when leaching reagent, can improve on the one hand the concentration of vanadium in the leach liquor of next batch, consumption that on the other hand can also conserve water.Those skilled in the art all can know this.
Generally speaking, for step leaching operation, next batch leaches thin liquid that operation all can last consignment of time as leaching reagent.And step first leaches operation because can't obtain described thin liquid, therefore general all take water as leaching reagent, and, for last batch is leached, if do not need to obtain thin liquid, then only need three leachings not need to carry out again three washings and can realize purpose of the present invention.For the leaching operation of continous way, generally also all take water as leaching reagent.
Described continous way leaching method is leaching method well known in the art also, does not repeat them here.
Among the present invention, under the preferable case, the condition of described sodium oxide baking comprises: the temperature of roasting is 300-1000 ℃, and the time of roasting is 30-300min, the consumption of oxygenant so that in the tail gas after the roasting oxygen content be not less than 10 % by weight.
Further under the preferable case, the temperature of described roasting can be in 300-900 ℃ the scope.The method according to this invention, described sodium oxide baking preferably includes a plurality of stages of carrying out continuously and carrying out under differing temps, therefore, along the traffic direction of described furnace charge in described oxidizing roasting stove, temperature in the described sodium oxide baking stove can improve (namely in gradient gradually, can be divided into a plurality of temperature sections that temperature raises gradually in the described sodium oxide baking stove), the thermograde between each temperature section can be 50-200 ℃.
Aforementioned a plurality of stage roasting is generally carried out in wedge furnance.The stove of sodium oxide baking described in the present invention is the general designation of carrying out the roasting apparatus of sodium oxide baking of the present invention.
Among the present invention, described oxygenant can be this area various oxygenants commonly used.Preferably, described oxygenant can be in oxygen-containing gas, Vanadium Pentoxide in FLAKES and the Manganse Dioxide one or more.According to the present invention, described oxygenant is preferably oxygen-containing gas.Adopt oxygen-containing gas can further reduce on the one hand the cost of method of the present invention as oxygenant, enhance productivity, on the other hand then can be so that the method according to this invention be more simple and easy to do.
The present invention without particular requirement, can be the various smart vanadium slags commonly used of prior art, and the present inventor finds, in oxide compound, with the dry weight basis of smart vanadium slag, when described smart vanadium slag is the V that contains the 12-20 % by weight to the kind of described smart vanadium slag and character
2O
5, the 12-30 % by weight SiO
2, the MnO of 5-10 % by weight, the MgO of 3-7 % by weight, the Fe of 35-50 % by weight
2O
3, the CaO of 1-5 % by weight, the TiO of 10-20 % by weight
2, the 2-5 % by weight Al
2O
3, the 2-5 % by weight Cr
2O
3Smart vanadium slag the time can make the vanadium in the vanadium iron bag-type dust material of the present invention obtain more effective recovery, therefore, under the preferable case, with the dry weight basis of smart vanadium slag, contain the V of 12-20 % by weight in the described smart vanadium slag
2O
5, the 12-30 % by weight SiO
2, the MnO of 5-10 % by weight, the MgO of 3-7 % by weight, the Fe of 35-50 % by weight
2O
3, the CaO of 1-5 % by weight, the TiO of 10-20 % by weight
2, the 2-5 % by weight Al
2O
3, the 2-5 % by weight Cr
2O
3
The present invention is not particularly limited for the kind of described sodium agent, can be this area various sodium agent commonly used.For example, described sodium agent can be the sodium salt of mineral acid and/or the superoxide of sodium.Preferably, described sodium agent is one or more in yellow soda ash, sodium-chlor, sodium sulfate, SODIUMNITRATE, sodium peroxide and the clorox.From reducing the angle of environmental pollution, described sodium agent is yellow soda ash more preferably.
The method that described leach liquor dephosphorization, silica removal is obtained qualifying liquid among the present invention can be carried out with reference to prior art, for example can by in leach liquor, add dephosphorization agent, desiliconizing agent carries out dephosphorization, silica removal.The present invention to the kind of described dephosphorization agent, desiliconizing agent without particular requirement, as long as realize dephosphorization, silica removal.
The present invention, can determine according to concrete needs without particular requirement the consumption of described dephosphorization agent, desiliconizing agent.
Adopt in the qualifying liquid that method of the present invention obtains the V/Na mol ratio greater than 1/2, [Na]＜30g/L, [K]＜1g/L, [P]≤0.015g/L, [Si]≤1g/L.
Among the present invention, described qualifying liquid refers to the roasting grog after leaching (also claiming leaching) to obtain liquid and the liquid of clear that its dephosphorization, silica removal are obtained, is called qualifying liquid according to the method for those skilled in the art's custom.
Among the present invention, described qualifying liquid is carried out the method that the acid ammonium salt precipitation obtains red vanadium can carry out with reference to prior art, do not repeat them here.
Among the present invention, described red vanadium press filtration, dry method all can be carried out with reference to prior art, not repeat them here.
Among the present invention, the method for reducing that reduces after described red vanadium press filtration, the drying without particular requirement, is not repeated them here.
Among the present invention, the method that melts after the described red vanadium press filtration without particular requirement, is not repeated them here.
Red vanadium is also referred to as APV among the present invention, and it specifically refers to the poly ammonium vanadate.TV represents total content of vanadium among the present invention, and SV represents soluble vanadium content.
The present invention will be described in detail below by specific embodiment.
Among the embodiment, as specifying, use be chemically pure reagent.
Among the embodiment, the content of soluble vanadium refers to the content of soluble vanadium in the grog with respect to the percentage ratio of total content of vanadium in the grog, i.e. SV/TV * 100 % by weight)
Among the present invention, MFe represents: in the metallic iron of element; TFe represents: in whole iron of element, comprise metallic iron and the iron that exists with the form of compound.
Add the mass ratio that the ammonium coefficient refers to vanadium in ammonium sulfate and the solution among the present invention.
Embodiment 1
(water content is 20.3 % by weight with 100g vanadium iron bag-type dust material (chemical composition sees Table 1), 1000g return slag, see Table 10 concrete the composition), 1000g essence vanadium slag (main chemical compositions sees Table 2), 150g yellow soda ash mix rear Sheng and enter in the crucible, in 800 ℃ retort furnace, take air as oxygenant, carry out sodium oxide baking 60min and obtain grog, soluble vanadium content is 88.54 % by weight in this grog, and oxygen content is 15 % by weight in the tail gas of retort furnace.This grog is leached (three leachings, condition: water is for leaching reagent, water temperature is that the weight ratio of 90 ℃, water and grog is 1: 1, carry out suction filtration after each the leaching, the vacuum tightness of suction filtration is 0.04MPa, the time of carrying out suction filtration is 5 minutes, the leaching condition of all the other embodiment is identical with the present embodiment), be the waste of 0.73 % by weight for 16.46g/L, [K] for the qualifying liquid of 0.71g/L and TV for 28.19g/L, [Na] with obtaining [V] behind leach liquor (namely three suction filtrations obtain total liquid) dephosphorization, the silica removal.Qualifying liquid is carried out the acid ammonium salt precipitation (after namely qualifying liquid being heated to 65 ℃, add ammonium sulfate, adding the ammonium coefficient is 2.0, adding the vitriol oil makes its pH reach 2.3, precipitation finishes after leaving standstill 30min under 90 ℃, and the precipitation condition of all the other embodiment is identical with the present embodiment), after precipitation finishes, APV to gained filters and washs, and the APV water content that obtains is that 21.4 % by weight, TV are 49.6 % by weight, Na
2O+K
2O is 0.7 % by weight, and S is 0.21 % by weight.This APV is the smelting V of high-quality
2O
3Or the raw material of sheet vanadium.
Embodiment 2
5 tons of vanadium iron bag-type dust material (chemical composition sees Table 3) and 100 tons of return slags (water content is 20 % by weight, and see Table 10 concrete the composition) are mixed to get mixture, this mixture is sent into separately in the wedge furnance (10 layers).Then 24.5 tons in 100 tons of smart vanadium slags (main chemical compositions sees Table 4) and yellow soda ash is mixed, send into the wedge furnance from another entrance of wedge furnance, take air as oxygenant, carry out sodium oxide baking [maturing temperature of each layer and roasting time in the wedge furnance: the first layer 300-330 ℃, second layer 440-460 ℃, the 3rd layer 550-570 ℃, the 4th layer 600-630 ℃, layer 5 680-700 ℃, layer 6 740-760 ℃, layer 7 780-790 ℃, the 8th layer 770-780 ℃, the 9th layer 730-740 ℃, the tenth layer 590-610 ℃, each layer roasting time is 15min], obtain grog (main chemical compositions sees Table 5), soluble vanadium content is 89.47% in this grog, and in roasting process, occur without abnormal conditions, and oxygen content is 13 % by weight in the tail gas of wedge furnance.This grog is delivered to upper filtration of horizontal vacuum band-type filter machine (using the aperture is 120 purpose filter clothes) with recirculated water (water quality sees Table 6) after wet ball mill grinds, obtain waste (main chemical compositions sees Table 7) and qualifying liquid ([V]=30.85g/L, [Na]=20.11g/L, [K]=0.49g/L) in the qualifying liquid.This qualifying liquid is carried out the acid ammonium salt precipitation, its Upper-liquor of Precipitating Vanadate Process contains Na, K, the V situation sees Table 8, the red vanadium (APV) that obtains uses recirculated water (water quality sees Table 6) press filtration washing on sheet frame, and red vanadium (APV) main chemical compositions before and after the washing sees Table 9.Entering reduction kiln after the red vanadium (APV) after the press filtration washing enters the dehumidification system drying reduces and produces V again
2O
3, the V that obtains
2O
3In Na
2O+K
2O fluctuates between the 0.3-0.6 % by weight, and average is 0.42 % by weight; S fluctuates between the 0.01-0.03 % by weight, and average is 0.02 % by weight; Be qualified product.This V
2O
3It is the raw material of the smelting ferrovanadium of high-quality.
Embodiment 3
According to the method vanadium extraction of embodiment 2, different is, the return slag that uses is the return slag of 18 % by weight as water content, and see Table 10 concrete the composition, obtains that soluble vanadium content is 90.21% in the grog, the V that finally obtains
2O
3In Na
2O+K
2O fluctuates between the 0.2-0.5 % by weight, and average is 0.37 % by weight; S fluctuates between the 0.01-0.03 % by weight, and average is 0.02 % by weight; Be qualified product.This V
2O
3It is the raw material of the smelting ferrovanadium of high-quality.This result is suitable with embodiment 2 effects.
Embodiment 4
According to the method vanadium extraction of embodiment 2, different is that the return slag that uses is the return slag of 32 % by weight as water content, see Table 10 concrete the composition, the first layer windrow of wedge furnance is serious as a result, and the first layer temperature (200-240 ℃) on the low side, causes roasting system to produce not direct motion.Soluble vanadium content is 81.78% in the grog that obtains, the V that finally obtains
2O
3In Na
2O+K
2O fluctuates between the 0.3-0.8 % by weight, and average is 0.51 % by weight; S fluctuates between the 0.02-0.05 % by weight, and average is 0.04 % by weight; Be qualified product.This V
2O
3It is the raw material of the smelting ferrovanadium of high-quality.The present embodiment is with respect to embodiment 2, and roasting system produces not direct motion and the vanadium yield is on the low side.
Comparative Examples 1
100g vanadium iron bag-type dust material (chemical composition sees Table 1) is contained in the crucible, in 800 ℃ retort furnace, take air as oxygenant, carry out sodium oxide baking 60min and obtain grog, soluble vanadium content is 98.4% in this grog, and oxygen content is 15 % by weight in the tail gas of retort furnace; This grog is leached (leaching condition is with embodiment 1), be the qualifying liquid of 24.47g/L for 28.64g/L, [Na] for 48.01g/L, [K] with obtaining [V] behind leach liquor dephosphorization, the silica removal, [Na] of this qualifying liquid, [K] concentration are too high, can't carry out normal acid ammonium salt precipitation to it, therefore lower step test can't be carried out; And in the test, crucible is etched terribly.
Comparative Examples 2
(water content is 20 % by weight with the 1000g return slag with 100g vanadium iron bag-type dust material (chemical composition sees Table 1), see Table 10 concrete the composition) contain in the crucible, in 800 ℃ retort furnace, take air as oxygenant, carry out sodium oxide baking 60min and obtain grog, soluble vanadium content is 85.01% in this grog, and oxygen content is 15 % by weight in the tail gas of retort furnace.This grog is leached (leaching condition is with embodiment 1), and obtaining [V] behind dephosphorization, the silica removal is the waste of 0.46 % by weight for 39.54g/L, [K] for the qualifying liquid of 22.36g/L and TV for 30.18g/L, [Na].[Na] of this qualifying liquid, [K] concentration are high, can't carry out normal acid ammonium salt precipitation to it; TV is lower in the waste that obtains, and knows that sodium in the vanadium iron bag-type dust material with the part vanadium in the return slag reaction has occured and obtained SV.
Table 1
Table 2
Table 3
Table 4
Table 5
In the table 5, the content of grog main chemical compositions is the mean value that 4 sub-samplings are analyzed.
Table 6
In the table 6, the content of recirculated water chemical composition is the mean value that 4 sub-samplings are analyzed.
Table 7
In the table 7, the content of the main chemical compositions of waste is the mean value that 4 sub-samplings are analyzed.
Table 8
In the table 8, the content of the some chemical properties of Upper-liquor of Precipitating Vanadate Process is the mean value that 4 sub-samplings are analyzed.
Table 9
In the table 9, the content of the main chemical compositions before and after the APV washing is the mean value that 4 sub-samplings are analyzed.
Table 10
Claims (14)
1. method that reclaims vanadium iron bag-type dust material, the method comprises: vanadium iron bag-type dust material is mixed with the sodium oxide baking return slag.
2. method according to claim 1 wherein, contains the water of 15-25 % by weight in the described sodium oxide baking return slag.
3. method according to claim 2 wherein, contains the water of 18-22 % by weight in the described sodium oxide baking return slag.
4. the described method of any one according to claim 1-3, wherein, the weight ratio of described vanadium iron bag-type dust material and sodium oxide baking return slag is not higher than 1: 4.
5. method according to claim 4, wherein, the weight ratio of described vanadium iron bag-type dust material and sodium oxide baking return slag is not higher than 1: 10.
6. the described method of any one according to claim 1-3 wherein, in oxide compound, with the dry weight basis of sodium oxide baking return slag, contains the V of 0.9-5.5% in the described sodium oxide baking return slag
2O
5, 3-10% Na
2The K of O, 0.05-0.3%
2The SiO of O, 5-25%
2, 4-10% MgO, the Fe of 20-50% of MnO, 2-8%
2O
3, the CaO of 0.5-6%, the TiO of 5-25%
2, 1-6% Al
2O
3And the Cr of 0.5-8%
2O
3
7. the described method of any one according to claim 1-3 wherein, in oxide compound, with the dry weight basis of vanadium iron bag-type dust material, contains the V of 15-30% in the described vanadium iron bag-type dust material
2O
5, 10-40% Na
2The K of O, 5-20%
2The SiO of O, 0.5-5%
2, 0.5-5% Fe
2O
3, the MnO of 0.2-4%, the Al of 5-20%
2O
3, the MgO of 10-30%, the CaO of 0.5-8%.
8. the mixture that is obtained by the described method of any one among the claim 1-7.
9. the method for a vanadium extraction, the method comprises: with mixture claimed in claim 8 with carry out sodium oxide baking after smart vanadium slag, sodium agent mix and obtain grog; Described grog leaching is obtained leach liquor; To obtain qualifying liquid behind described leach liquor dephosphorization, the silica removal; Described qualifying liquid is carried out the acid ammonium salt precipitation obtain red vanadium.
10. method according to claim 9, wherein, the method also comprises: with described red vanadium press filtration, dry after reduction obtain vanadous oxide, or will melt after the described red vanadium press filtration and obtain the sheet vanadium.
11. according to claim 9 or 10 described methods, wherein, described smart vanadium slag, sodium agent and described mixture are mixed into furnace charge in stoving oven, so that the TV of furnace charge is the 3.5-6.0 % by weight, the Na/V mol ratio is 1.2-2.
12. according to claim 9 or 10 described methods, wherein, the condition of described sodium oxide baking comprises: the temperature of roasting is 300-1000 ℃, and the time of roasting is 30-300min, the consumption of oxygenant so that in the tail gas after the roasting oxygen content be not less than 10 % by weight.
13. according to claim 9 or 10 described methods, wherein, in oxide compound, with the dry weight basis of smart vanadium slag, contain the V of 12-20% in the described smart vanadium slag
2O
5, 12-30% SiO
2, 5-10% MgO, the Fe of 35-50% of MnO, 3-7%
2O
3, the CaO of 1-5%, the TiO of 10-20%
2, 2-5% Al
2O
3, 2-5% Cr
2O
3
14. according to claim 9 or 10 described methods, wherein, described sodium agent is one or more in yellow soda ash, sodium-chlor, sodium sulfate, SODIUMNITRATE, sodium peroxide and the clorox, and oxygenant is one or more in oxygen-containing gas, Vanadium Pentoxide in FLAKES and the Manganse Dioxide.
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| CN110453065A (en) * | 2019-09-12 | 2019-11-15 | 内蒙古工业大学 | The method of vanadium extraction in vanadium titano-magnetite, the leachate containing sodium vanadate extracted using this method and its application |
| CN111394569A (en) * | 2020-04-20 | 2020-07-10 | 承德燕北冶金材料有限公司 | Roasting method for producing vanadium pentoxide |
| CN112095024A (en) * | 2020-08-12 | 2020-12-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of sodium-modified vanadium extraction tailings |
| CN113088712A (en) * | 2021-04-01 | 2021-07-09 | 东北大学 | Method for extracting vanadium from vanadium slag by water leaching through large-scale treatment of vanadium slag |
| CN115927844A (en) * | 2022-11-14 | 2023-04-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for continuously leaching vanadium-containing clinker |
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| CN105177278A (en) * | 2015-10-27 | 2015-12-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium slag sodium salt roasting method |
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| CN112095024B (en) * | 2020-08-12 | 2022-08-05 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of sodium-modified vanadium extraction tailings |
| CN113088712A (en) * | 2021-04-01 | 2021-07-09 | 东北大学 | Method for extracting vanadium from vanadium slag by water leaching through large-scale treatment of vanadium slag |
| CN115927844A (en) * | 2022-11-14 | 2023-04-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for continuously leaching vanadium-containing clinker |
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