CN103421959B - Method for extracting vanadium efficiently from vanadium slag by controlling particle diameter of additive - Google Patents
Method for extracting vanadium efficiently from vanadium slag by controlling particle diameter of additive Download PDFInfo
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Abstract
The invention discloses a method for extracting vanadium efficiently from vanadium slag by controlling the particle diameter of additive. A sodium salt roasting vanadium extraction technology is adopted in the method, and when the additive is added in the vanadium slag, the particle diameter of the additive is determined through the following steps of (1) calculating the ratio between the particle number of the vanadium slag and the particle number of the additive based on the stacking density of the vanadium, the stacking density of the additive and the dosage of the additive to obtain an ideal particle diameter of the additive, and (2) taking the particle diameter of the vanadium slag, an original particle diameter of the additive, the ideal particle diameter of the additive and a final particle diameter of the additive as boundary points to obtain the ranges of the three sections of the particle diameters of the additive, taking the particle diameter of the additive as a variable, carrying out comparison on sodium salt roasting leaching based on a single factor analysis method, and taking the particle diameter range with the optimal result as the final particle diameter of the additive. The method for extracting the vanadium efficiently from the vanadium slag by controlling the particle diameter of the additive can reduce the caking phenomenon of the additive, materials are mixed more evenly, and the utilization efficiency of the additive and the roasting conversion rate of the vanadium slag are improved.
Description
Technical field
The present invention relates to a kind of method that realizes vanadium slag efficient vanadium extracting by controlling additive particle diameter, belong to vanadium extraction technical field.Particularly, present method adopts rational additive particle diameter and processing parameter, by sodium roasting and water logging, processes, and the water-insoluble vanadium in vanadium slag is converted into water miscible vanadate and obtains, containing vanadium leachate, reaching the object of high efficiency extraction Vanadium in Vanadium Residue element.
Background technology
Vanadium is a kind of important valuable metal element, due to physical propertiess such as its excellent tensile strength, hardness and fatigue resistances, be widely used in the industries such as iron and steel, non-ferrous metal, chemical and electronics, in national economy and the daily productive life of people, bringing into play the effect of positive important.
Raw material for vanadium extraction has a lot, and this is the abundantest, the most widely used vanadium titano-magnetite that surely belongs to of reserves wherein, 88% of vanadium annual production from vanadium titano-magnetite, obtains in the world.From vanadium titano-magnetite, reclaim vanadium, conventional method is that vanadium titano-magnetite is obtained to vanadium-bearing hot metal through blast furnace or electrosmelting, by selective oxidation molten iron, makes to enter slag after vanadium oxidation, and this slag with certain content of vanadium is so-called vanadium slag.
A kind of slag that vanadium slag is comprised of ten multiple compounds.Chemical analysis shows, in vanadium slag, main chemical composition comprises FeO, SiO
2, V
2o
3, TiO
2, MnO and MgO.In addition, also contain a small amount of CaO, Cr
2o
3and Al
2o
3.Due to the difference of vanadium extraction raw material and vanadium-bearing hot metal process for extracting vanadium, different enterprises produce the vanadium slag composition obtaining and differ.
From vanadium slag, extracting vanadium is current main extraction vanadium method, and representative Leaching of Vanadium from Vanadium slag technique has following several: sodium roasting vanadium-extracting method, calcification baking vanadium extracting method, acid dipping-extraction vanadium extraction method and acidleach ion exchange resin vanadium extracting method etc.What wherein, be most widely used surely belongs to sodium roasting water logging vanadium extracting method.
Under sodium roasting water logging vanadium extraction processing condition, vanadium slag mixes and is incorporated to stove roasting with appropriate additive after the pre-treatment such as broken deironing.Roasting is carried out under oxidizing atmosphere, in roasting process, vanadium slag at a middle or low price state vanadium by oxidation conversion be+5 valencys vanadium compound and with the additive water miscible vanadate of generation that reacts, additive except the vanadium with vanadium slag reacts can also with other impurity component partial reaction.The material of vanadium slag after oxidizing roasting is called grog, describes the quality of roasting process and mainly by " roasting conversion rate ", weighs, and roasting conversion rate refers to after roasting that the amount of soluble vanadium in grog accounts for the ratio of whole vanadium amounts.Leaching process is mainly that water contacts with roasting grog later, thereby it is separated with most indissoluble impurity to make vanadium enter solution, obtains containing vanadium leachate.The effect leaching represents by leaching yield conventionally, the per-cent of the vanadium transforming while entering the vanadium of solution and roasting in leaching process.
In vanadium slag sodium roasting process, additive plays vital effect, is indispensable.Generally, the Main Function of additive is to react with vanadium slag to form soluble vanadium compound, and further research shows that it also has great impact to the oxidation rate of vanadium slag.The oxidizing reaction of Vanadium in Vanadium Residue belongs to region reaction, and reaction occurs in solid interface, and the particle diameter of speed of reaction and reactant is closely related, increases the oxidation ratio that the contact area between additive and vanadium slag can effectively be improved roasting condition and improve vanadium.Contact area between this additive and vanadium slag can be adjusted by the size that changes the two, and current investigator's vanadium slag reacting dynamics condition that generally particle diameter by research vanadium slag obtains there is not yet report for the research of additive particle diameter.
As everyone knows, the amount of allocating into of additive is also one of important factor affecting vanadium slag roasting conversion rate.When the amount of allocating into is very few, vanadium slag oxidizing roasting reaction is insufficient, and roasting conversion rate is low; The words that the amount of allocating into is too much, additive can react with the impurity component in vanadium slag and generate a large amount of low melting points, and under high-temperature roasting, produce a large amount of liquid phases, and cause roasting material to occur bonding, wrap up even the fault in productions such as sintering, affect equally the roasting conversion rate of vanadium.
For the problems referred to above, the vanadium slag based on different, investigators often pass through to optimize the processing parameter of roasting process, thereby reach higher vanadium extraction yield as the consumption of the particle diameter of vanadium slag, additive, maturing temperature and roasting time etc. obtain suitable processing condition.Yet this method that improves V leaching rate by Optimizing Process Parameters can not improve the utilising efficiency of additive, can not fundamentally reduce the consumption of additive, reduce production costs.In actual production process, due in vanadium slag, exist some can with the impurity component of additive reaction, the add-on of additive be all often need excessive.And, if vanadium slag and additive batch mixing are even not, also can cause that local additive level is too high, cause productivity low, to producing, bring disadvantageous effect.In addition, how under the condition that does not affect roasting conversion rate, can suitably reduce again the consumption of additive, reduce production costs, these are all the problems that is worth investigator to consider.
Summary of the invention
The above-mentioned technical problem existing for prior art, the object of the present invention is to provide a kind of method that realizes vanadium slag efficient vanadium extracting by controlling additive particle diameter.Present method can reduce additive caking phenomenon, and batch mixing is more even, improves the utilising efficiency of additive and the roasting conversion rate of vanadium slag.
To achieve these goals, the technical solution used in the present invention is as follows:
Control additive particle diameter and realize a method for vanadium slag efficient vanadium extracting, present method Leaching of Vanadium from Vanadium slag technique is sodium roasting vanadium-extracting method, in vanadium slag, adds additive and mixes, and obtains compound; By compound roasting under oxidizing atmosphere, obtain containing vanadium roasting grog; By levigate to certain particle diameter after roasting clinker cooling, water leaches and is obtained residue and containing vanadium leachate, containing vanadium leachate, through precipitation technique, can be obtained vanadium finished product by suction filtration again; It is characterized in that: described additive particle diameter is determined as follows.
1) particle diameter is first fixed: suppose that vanadium slag and additive are and have the spherical of certain diameter, and vanadium slag uniform particle diameter, diameter is
, and both additive granules and vanadium slag particle inscribes of becoming square to arrange while mixing; Consumption by the tap density of vanadium slag, the tap density of additive and additive calculates the ratio of vanadium slag and the granule number of additive, and then obtains perfect additive particle diameter;
2) ultimate size is determined: the minimum grain size that the additive of usining is of practical significance is as ultimate additive particle diameter, using vanadium slag particle diameter, original additive particle diameter, perfect additive particle diameter and ultimate additive particle diameter respectively as frontier point, obtain three sections of different additive particle size range; Using additive particle diameter as variable, adopt single-factor analysis therapy to carry out sodium roasting and leach comparison, using that section of particle size range of result optimal as final additive particle size range;
If the perfect additive particle diameter calculating is greater than original additive particle diameter, using vanadium slag particle diameter, original additive particle diameter and ultimate additive particle diameter as frontier point, obtain two sections of different additive particle size range; Using additive particle diameter as variable, adopt single-factor analysis therapy to carry out sodium roasting and leach comparison, using that section of particle size range of result optimal as final additive particle size range.
The tap density of described vanadium slag is 2.5-3g/cm
3, additive is sodium salt additive, the tap density of additive is 0.85-0.90 g/cm
3, the 15-20% that additive amount is vanadium slag quality, calculating vanadium slag is 1.5-2.4 with the ratio of the granule number of additive, perfect additive particle diameter
(diameter) is:
.
Described ultimate additive particle diameter is 200 orders (0.075mm).
Adopt single-factor analysis therapy to carry out sodium roasting while leaching comparison, the vanadium of usining turn the rate of soaking the highest as optimal result.
Described sodium salt additive is a kind of in sodium carbonate, sodium-chlor and sodium sulfate.
As preferred control parameter, in described sodium roasting technique, maturing temperature 800-850 ℃, roasting time 1.5-2.5h; After roasting finishes, roasting grog is come out of the stove and is cooled to room temperature, then by its levigate screening and by 160 orders; The grog water sieving out is leached, and water and roasting grog liquid-solid ratio are 5 ~ 10ml/g (being preferably 8ml/g), and extraction temperature is 80-95 ℃, and constant temperature extraction time is 25-60min.
Compared to existing technology, the present invention has following beneficial effect:
(1) present method is by adopting rational additive particle diameter, reduced the caking of additive, and because additive particle diameter is less, make in itself and vanadium slag batch mixing and rotary kiln baking process, to be difficult for producing segregation, can realize more easily evenly batch mixing, thereby reduce, because local additive level is too high, cause when roasting, occurring bonding, wrap up even the fault in productions such as sintering;
(2) the definite additive particle diameter of present method, can make itself and vanadium slag have more sufficient contact area, accelerates the speed of calcination, shortens roasting time, improves the utilising efficiency of additive and the roasting conversion rate of vanadium slag;
(3) due to the raising of additive utilising efficiency, thereby can in the impregnable situation of roasting conversion rate, suitably reduce the consumption of additive, and then reduce production cost guaranteeing, realize the production becoming more meticulous.
Accompanying drawing explanation
Fig. 1-vanadium slag is desirable piles up model;
Fig. 2-vanadium slag and the additive graph of a relation (additive granules and the vanadium slag particle inscribe that becomes square to arrange) of arranging; Light color represent additive granules, black represent vanadium slag particle; Wherein A is vanadium slag and the additive integral body graph of a relation of arranging; B is a circumgranular distribution of additives figure of vanadium slag; C is additive granules vanadium slag distribution plan around;
Embodiment
The present invention proposes a kind of method that additive particle diameter is realized the leaching of vanadium slag high-efficient roasting that considers.Present method is by determining the particle size range of reasonable additive, and then the caking of minimizing additive, make more easily even batch mixing of itself and vanadium slag, prevent that local additive level is too high or too low, thereby make additive can reach higher utilising efficiency, and the consumption that suitably reduces on this basis additive reduces production costs, and reduce fault in production, finally realize the production becoming more meticulous.
The concrete technical scheme of the present invention is, in vanadium slag, adds the sodium salt additive of certain appropriate particle size and mixes, and obtains compound; By compound roasting under oxidizing atmosphere, obtain containing vanadium roasting grog; Again that roasting grog is levigate to certain particle diameter, water leaches and is obtained residue and containing vanadium leachate, containing vanadium leachate, can be obtained vanadium finished product again through precipitation by suction filtration.
Wherein, additive sodium salt can be sodium carbonate, in sodium-chlor and sodium sulfate at least one.
Definite method of above-mentioned appropriate addn particle diameter is divided into " the first of particle diameter determined " and " ultimate size is determined " two steps.Concrete grammar is as follows:
(1) additive particle diameter first determined method
For certain given vanadium slag, its particle diameter is set.General, according to the requirement of roasting condition, China measures the particle diameter of vanadium slag conventionally with 120 mesh sieves (0.074mm), and requirement has 80% vanadium slag by 120 orders.Based on particular case, consider that different manufacturers requires the difference of the composition of inconsistent and vanadium slag for the particle diameter of vanadium slag, simultaneously in order to simplify calculating, suppose that in advance vanadium slag and additive are have certain diameter spherical, and vanadium slag particle diameter (diameter) homogeneous is all
.Now vanadium slag is set up to a simple desirable model of piling up as shown in Figure 1.
The tap density that records by experiment vanadium slag is 2.5-3g/cm
3, the tap density of additive (take industrial sodium carbonate) is 0.85-0.90 g/cm
3.The consumption of additive is generally the 15-20% of vanadium slag quality.With this understanding, according to calculating, the ratio of the granule number of vanadium slag and additive is between 1.5-2.4.Comprehensive this calculation result, the present invention proposes to be while arranging as shown in Figure 2 (additive granules and become the vanadium slag particle inscribe of square arrangement) when vanadium slag and additive, and both have good reaction contact area.The present invention proposes, and the additive particle diameter in this situation is desirable particle size
.
Therefore, desirable additive particle diameter
(diameter) is:
To sum up, the additive particle diameter of initial optimization is slightly decided to be the perfect additive particle diameter that above-mentioned model calculates
,
vanadium slag particle diameter doubly.
(2) definite method of additive ultimate size
Generally, the particle diameter of industrial additive requires as 70%-80% is by 80 orders (0.180mm) or 100 orders (0.150mm).If consider, additive particle diameter is too low, may produce dust from flying, has reduced on the contrary its utilization ratio, and grind away cost also can increase thereupon, therefore the ultimate particle diameter of additive is set, is 200 orders (0.075mm).That is to say, if additive particle diameter is less than 0.075mm, there is no larger practical significance.
In order further to adjust the particle size range of appropriate addn, the present invention proposes to carry out relevant experimental analysis, to obtain final suitable additive particle diameter.Using vanadium slag particle diameter, original additive particle diameter, perfect additive particle diameter and ultimate additive particle diameter respectively as frontier point, and the scope of usining between them is as the object of considering.Concrete situation is as follows:
(a) when above-mentioned four kinds of particle diameters are from big to small with original additive particle diameter, vanadium slag particle diameter, during the sequence of perfect additive particle diameter and ultimate additive particle diameter, the scope that additive particle diameter is considered is: 1. original additive particle diameter ~ vanadium slag particle diameter; 2. vanadium slag particle diameter ~ perfect additive particle diameter; 3. perfect additive particle diameter ~ ultimate additive particle diameter.
(b) when above-mentioned four kinds of particle diameters are during from big to small with vanadium slag particle diameter, original additive particle diameter, perfect additive particle diameter and the sequence of ultimate additive particle diameter, the scope that additive particle diameter is considered is: 1. vanadium slag particle diameter ~ original additive particle diameter; 2. original additive particle diameter ~ perfect additive particle diameter; 3. perfect additive particle diameter ~ ultimate additive particle diameter.
(c), if vanadium slag particle diameter is larger, when the perfect additive particle diameter calculating is greater than original additive particle diameter, using the particle diameter of original additive particle diameter as appropriate addn.General, in order there to be good oxidizing roasting effect, suggestion considers that whether former vanadium slag particle diameter is excessive and it is adjusted to (conventionally adjusting to the general requirement of current industry to vanadium slag: have 80% vanadium slag by 120 mesh sieves), to reaching higher vanadium slag roasting conversion rate.
Based on above-mentioned different situations, using additive particle diameter as variable, adopt single-factor analysis therapy to carry out Roasting And Leaching experiment, and using that group of experimental result optimum as the particle size range of final reasonable additive.Result optimal turns with vanadium the rate of soaking to be considered.
To sum up, adopt aforesaid method can obtain the additive particle size range (the definite additive particle diameter of present method can be applicable to any vanadium slag raw material) that is applicable to this vanadium slag.
The particle size range of the reasonable additive of determining based on aforesaid method, will be described in detail below a preferred method of vanadium slag Roasting And Leaching of the present invention.Specific experiment step is:
(1) vanadium slag is ground and magnetic separation pre-treatment, obtain 80% and can be no more than by 120 mesh sieves and metal Ferrum content the vanadium slag powder of 5wt%.
(2) for size distribution and the constituent structure of corresponding vanadium slag raw material, by slightly determining method and final definite two steps of method, research obtains rational additive particle size range.Sodium salt additive is ground to screening and process, obtain being applicable to the additive particle diameter of this vanadium slag.
(3) in vanadium slag, add the sodium salt additive (this content is determined according to concrete vanadium slag constituent structure, in the category of not considering in the present invention) after a certain amount of screening, mix, obtain compound; Compound is joined in roasting apparatus and carries out roasting, keep air atmosphere during roasting, maturing temperature is controlled at 800-850 ℃, and roasting time is 1.5-2.5h (being preferably 2h), obtains containing vanadium roasting grog.
(4) grog after sodium roasting is carried out to levigate screening, get 160 order screen underflows, make the particle diameter of vanadium slag grog be less than 0.1mm.Then by liquid-solid ratio, be that 5 ~ 10ml/g (being preferably 8ml/g) mixes distilled water with roasting grog, in thermostatically heating magnetic agitation water-bath, leach, extraction temperature is 80 ~ 95 ℃, extraction time 25 ~ 60min (being preferably 30min).After leaching finishes, adopt vacuum filtration device to carry out suction filtration to mixture, filter and obtain, containing vanadium leachate and residue, containing vanadium leachate, through precipitation technique, can obtaining vanadium finished product.
Below in conjunction with specific embodiment, the present invention is described in further detail.
The vanadium slag that Jiang Mou enterprise produces is (containing V
2o
513.6wt%, CaO4.4wt%) levigate screening, require to have 80% by 120 orders.It is 160 orders that the method proposing by the present invention calculates this vanadium slag perfect additive particle diameter, existing by additive grind screening for (a) original additive (without grinding screening), (b)-original additive particle diameter ~+120 order, order ~+160, (c)-120 order, four parts, order ~+200, (d)-160 order stand-by.Each 3.8g of additive that gets above-mentioned four kinds of particle size range, mixes them respectively with 20g vanadium slag, be placed in retort furnace roasting 2h at 800 ℃, keeps fire door crack to guarantee that roasting process is in oxidizing atmosphere when roasting.After roasting finishes, take out roasting sample and be cooled to room temperature, the grog after roasting is ground to screening, get 160 order screen underflows.Measure 40mL distilled water and be placed in three-necked bottle, and heat in the thermostatically heating magnetic agitation water-bath of 90 ℃, until water temperature in three-necked bottle, reach after bath temperature, in three-necked bottle, add the grog after 5g roasting, leach 30min.After leaching finishes, adopt immediately vacuum filtration device to filter, adopt distilled water repeatedly to rinse residue during filtration, the V leaching rate that filtration is obtained packs in 500mL volumetric flask, and is settled to 500mL with distilled water, obtains containing vanadium leachate, to be detected.Through titration experiments, detect, and by calculating: it is 89.02% that vanadium (a) turns the rate of soaking, and it is 89.40% that vanadium (b) turns the rate of soaking, and it is 90.45% that vanadium (c) turns the rate of soaking, and it is 90.22% that vanadium (d) turns the rate of soaking.In sum, the additive particle size range of applicable this vanadium slag is between-120 order ~+160 orders.
The above embodiment of the present invention is to be only explanation example of the present invention, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make on the basis of the above description other multi-form variation and changes.Here cannot give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention amplifies out or change that belong to.
Claims (5)
1. control additive particle diameter and realize a method for vanadium slag efficient vanadium extracting, present method Leaching of Vanadium from Vanadium slag technique is sodium roasting vanadium-extracting method, in vanadium slag, adds additive and mixes, and obtains compound; By compound roasting under oxidizing atmosphere, obtain containing vanadium roasting grog; By levigate to certain particle diameter after roasting clinker cooling, water leaches and is obtained residue and containing vanadium leachate, containing vanadium leachate, through precipitation technique, can be obtained vanadium finished product by suction filtration again; It is characterized in that: described additive particle diameter is definite as follows,
1) particle diameter is first fixed: suppose that vanadium slag and additive are and have the spherical of certain diameter, and vanadium slag uniform particle diameter, diameter is
, and both additive granules and vanadium slag particle inscribes of becoming square to arrange while mixing; Consumption by the tap density of vanadium slag, the tap density of additive and additive calculates the ratio of vanadium slag and the granule number of additive, and then obtains perfect additive particle diameter;
2) ultimate size is determined: the minimum grain size that the additive of usining is of practical significance is as ultimate additive particle diameter, using vanadium slag particle diameter, original additive particle diameter, perfect additive particle diameter and ultimate additive particle diameter respectively as frontier point, obtain three sections of different additive particle size range; Using additive particle diameter as variable, adopt single-factor analysis therapy to carry out sodium roasting and leach comparison, using that section of particle size range of result optimal as final additive particle size range;
If the perfect additive particle diameter calculating is greater than original additive particle diameter, using vanadium slag particle diameter, original additive particle diameter and ultimate additive particle diameter as frontier point, obtain two sections of different additive particle size range; Using additive particle diameter as variable, adopt single-factor analysis therapy to carry out sodium roasting and leach comparison, using that section of particle size range of result optimal as final additive particle size range;
The tap density of described vanadium slag is 2.5-3g/cm
3, additive is sodium salt additive, the tap density of additive is 0.85-0.90 g/cm
3, the 15-20% that additive amount is vanadium slag quality, calculating vanadium slag is 1.5-2.4 with the ratio of the granule number of additive, perfect additive particle diameter
for:
.
2. control additive particle diameter according to claim 1 is realized the method for vanadium slag efficient vanadium extracting, it is characterized in that: described ultimate additive particle diameter is 200 orders.
3. control additive particle diameter according to claim 1 is realized the method for vanadium slag efficient vanadium extracting, it is characterized in that: adopt single-factor analysis therapy to carry out sodium roasting while leaching comparison, the vanadium of usining turn the rate of soaking the highest as optimal result.
4. according to the arbitrary described control additive particle diameter of claim 1-3, realize the method for vanadium slag efficient vanadium extracting, it is characterized in that: described sodium salt additive is a kind of in sodium carbonate, sodium-chlor and sodium sulfate.
5. control additive particle diameter according to claim 4 is realized the method for vanadium slag efficient vanadium extracting, it is characterized in that: in described sodium roasting technique, and maturing temperature 800-850 ℃, roasting time 1.5-2.5h; After roasting finishes, roasting grog is come out of the stove and is cooled to room temperature, then by its levigate screening and by 160 orders; The grog water sieving out is leached, and water and roasting grog liquid-solid ratio are 5 ~ 10ml/g, and extraction temperature is 80-95 ℃, and constant temperature extraction time is 25-60min.
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