CN104894370B - The method for leaching solvable vanadium from roasted vanadic slag with low-concentration sulfuric acid - Google Patents
The method for leaching solvable vanadium from roasted vanadic slag with low-concentration sulfuric acid Download PDFInfo
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- CN104894370B CN104894370B CN201510285781.8A CN201510285781A CN104894370B CN 104894370 B CN104894370 B CN 104894370B CN 201510285781 A CN201510285781 A CN 201510285781A CN 104894370 B CN104894370 B CN 104894370B
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- sulfuric acid
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Abstract
Method the invention discloses solvable vanadium is leached from roasting clinker with low-concentration sulfuric acid.The processing step is：1）Leach：Roasted vanadic slag is added into hot water leaching, leaching solid-liquid mass ratio is 1：2.5 3.0,10 20min are stirred, adjust pH value to stir 5 10min to continuation after 6.5 7.5 with sulfuric acid, obtain roasting clinker leaching liquor；2）Filtering：By roasted vanadic slag leachate filtering, filtrate and filter residue are obtained, solid-liquid mass ratio 1 is washed in filter residue hot wash：2.0 2.5, cleaning solution is merged with filtrate, obtain filter residue and solvable vanadium leachate.The inventive method can quickly leach high-silicon high basicity clinker, isolate solvable vanadium in clinker, low to solve the problems, such as high-silicon high basicity clinker leaching efficiency.
Description
Technical field
The invention belongs to vanadium-bearing hot metal metallurgical technology field, and in particular to soaked from roasted vanadic slag with low-concentration sulfuric acid
The method for going out solvable vanadium.
Background technology
Vanadium slag or residue containing vanadium add mixing sodium salt through crushing grinding to certain particle size (- 120 mesh)（Industrial sodium carbonate, work
Industry sodium chloride, industrial sulphuric acid sodium）It is calcined in 600 DEG C~800 DEG C of rotary kiln as additive and vanadium is converted into solubility
Sodium metavanadate, the material after roasting is clinker, and generally with water logging, water logging is by the soluble inclined vanadium in clinker for the leaching of clinker
Sour sodium is dissolved into the process of formation solution in water, and filtering is needed while water logging, reaches the purpose of separation of solid and liquid.Filtrate containing vanadium passes through
Ammonium salt is added to obtain ammonium poly-vanadate precipitation after removal of impurities, ammonium poly-vanadate is heated or high temperature melting is made the five of different conditions and aoxidizes two
Vanadium finished product.Because vanadium slag granularity is smaller in actual production, the dioxide-containing silica alkali allocated into high also can be high, it is fired after it is ripe
Material can form colloidal silica, and in filtering, solid-liquid is difficult to realize is kept completely separate, and have a large amount of slag charge slurry spillings to cause " running dilute " phenomenon, work
People will often clear up ground slurry material, and labour intensity is big.Because liquid can not be leached fully, soluble vanadium and water in filter residue are caused
Divide content substantially higher, production efficiency is reduced and pollutes to environment
To sum up, water logging filter both soluble vanadium is confined to that silicone content is relatively low, the relatively low clinker of basicity.Therefore one kind is developed to contain from silicon
Amount is higher, and the method for leaching separation soluble vanadium is very important in basicity roasted vanadic slag also higher.
The content of the invention
For above-mentioned technical problem, leached from roasted vanadic slag the invention discloses one kind low-concentration sulfuric acid solvable
The method of vanadium, the method can quickly leach high-silicon high basicity roasted vanadic slag, isolate solvable vanadium in clinker, to solve silicon high
The low problem of high alkalinity roasting clinker leaching efficiency.
In order to solve the above technical problems, the method that present invention low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag
Take following technical proposals：
1）Leach：Roasted vanadic slag is added into hot water leaching, leaching solid-liquid mass ratio is 1：2.5-3.0, stirs 10-
20min, adjusts pH value to stir 5-10min to continuation after 6.5-7.5 with sulfuric acid, obtains roasting clinker leaching liquor；
2）Filtering：By roasted vanadic slag leachate filtering, filtrate and filter residue are obtained, filter residue hot wash will
Cleaning solution merges with filtrate, obtains filter residue and solvable vanadium leachate.
Step 1 of the present invention）In hot water temperature >=90 DEG C.
Step 1 of the present invention）In sulfuric acid be low-concentration sulfuric acid, collocation method is：98% concentrated sulfuric acid and the volume of water
Than being 1:4.0, addition sulfuric acid process is persistently stirred.
Step 2 of the present invention）In hot wash step be：After filter residue water purification to be filtered point, hot wash filter residue is used, always
Washing solid-liquid mass ratio 2.0-2.5, point 3 washings, is finally filtered dry filter residue moisture.
Step 2 of the present invention）In hot water temperature >=80 DEG C.
Step 2 of the present invention）In be filtered into vacuum filtration.
Step 1 of the present invention）In leaching solid-liquid mass ratio be 1：2.5-3.0.
Step 2 of the present invention）In the total solid-liquid mass ratio 1 of hot wash：2.0-2.5.
Step 1 of the present invention）In roasted vanadic slag in silicone content scope with SiO2% is counted：10.0-20.0%, preferably
15.0-20.0%；Alkali content scope is with Na2CO3% is counted：7.5-20.0%, preferably 12.0-20.0%.
Mentality of designing of the invention：The present invention is high according to silicone content in roasted vanadic slag or alkali proportioning height causes clinker
Grain Surface Creation sodium silicate colloidal, makes water logging be difficult to the problem for completing, by allocating low-concentration sulfuric acid liquid leaching clinker into, so that broken
Bad sodium silicate colloidal is easily isolated vanadium liquid, hence it is evident that shorten leaching filtration time, and filtration time water consumption is leached not same
Under conditions of change, 0.30 is averagely declined compared to solvable vanadium in traditional handicraft water logging clinker filter residue~0.40%, moisture declines 4.20%,
Process cycle is shortened, reaching reduces cost increases benefit, reduce the multi-party effect such as environmental pollution.System after adjustment PH is through filling
Divide reaction finally will not still impact in alkalescence to equipment.Low equally applicable this law of clinker is matched to low silicon or alkali.Reduce
Leaching solid-to-liquid ratio improve washing solid-to-liquid ratio filter residue in can content of vanadium decline effect it is more notable.
The present invention is for middle silicone content（With SiO2% is counted）10.0-20.0%, alkali content（With Na2CO3% is counted）7.5-20.0%,
Especially to silicone content（With SiO2% is counted）15.0-20.0%；Alkali content（With Na2CO3% is counted）：The vanadium slag roasting of 12.0-20.0% is ripe
Material effect becomes apparent from, it is possible to increase 2-4 times of the rate of filtration, the solvable vanadium reduction by 0.4% of filter residue, and moisture reduction by 4% is left in filter residue
It is right.The present invention can to greatest extent isolate solvable vanadium in clinker, while solution high-silicon high basicity clinker leaching efficiency is low to cross filtering velocity
The slow problem of degree.
It is using the beneficial effect produced by above-mentioned technical proposal：
1st, solvable vanadium in clinker can be isolated more, content of vanadium in filter residue is reduced, the yield of vanadium is improved.
2nd, quick leaching high-silicon high basicity roasted vanadic slag, to solve, high-silicon high basicity clinker leaching efficiency is low to cross filtering velocity
The slow problem of degree.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
Sulfuric acid Analysis about Selection bright sulfur acid in each example of the present invention, water is industrial water, prepares low-concentration sulfuric acid volume ratio and is
Sulfuric acid：Water=1:4.
Embodiment 1
A kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag：
1）Leach：100g roasted vanadic slags are added into 90 DEG C of hot water leachings, leaching solid-liquid mass ratio is 1：3.0, stirring
(rotating speed 310r-320r/min) 10min, adjusts pH value to stir 5min to continuation after 6.5 with sulfuric acid, obtains roasting clinker leaching liquor；
Silicone content scope is with SiO in roasting clinker2% is counted：10.0%；Alkali content scope is with Na2CO3% is counted：15.0%, in clinker
The full V=5.00% of main chemical, can V=3.75%；
2）Filtering：By the filtering of roasted vanadic slag leachate, filtrate and filter residue are obtained, filter residue is with 80 DEG C of hot water 200ml
Wash in three times, wash solid-liquid mass ratio 1：2.0, material suction filtration to surface merges cleaning solution with filtrate without liquid phase, is filtered
Slag and solvable vanadium leachate.
Filter residue is removed and is checked after drying in drying baker.The full V of assay：1.39%, can V：0.130%, moisture
13.85%, filtering total elapsed time 7min（Funnel lower end has water droplet to start timing when flowing out, similarly hereinafter）.
Embodiment 2
A kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag：
1）Leach：100g roasted vanadic slags are added into 90 DEG C of hot water leachings, leaching solid-liquid mass ratio is 1：3.0, stirring
(rotating speed 310r-320r/min) 15min, adjusts pH value to stir 10min to continuation after 7.0 with sulfuric acid, obtains roasting clinker leaching liquor；
Silicone content scope is with SiO in roasting clinker2% is counted：20.0%；Alkali content scope is with Na2CO3% is counted：20.0%, in clinker
The full V=5.21% of main chemical, can V=3.90%；
2）Filtering：By the filtering of roasted vanadic slag leachate, filtrate and filter residue are obtained, filter residue is with 85 DEG C of hot water 200ml
Wash in three times, wash solid-liquid mass ratio 1：2.0, material suction filtration to surface merges cleaning solution with filtrate without liquid phase, is filtered
Slag and solvable vanadium leachate.
Filter residue is removed and is checked after drying in drying baker.The full V of assay：1.48%, can V：0.151%, moisture
14.08%, filtering total elapsed time 8min.
Embodiment 3：
A kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag：
1）Leach：100g roasted vanadic slags are added into 100 DEG C of hot water leachings, leaching solid-liquid mass ratio is 1：3.0, stirring
(rotating speed 310r-320r/min) 20min, adjusts pH value to stir 10min to continuation after 7.5 with sulfuric acid, obtains roasting clinker leaching liquor；
Silicone content scope is with SiO in roasting clinker2% is counted：13.0%；Alkali content scope is with Na2CO3% is counted：7.5%, in clinker
The full V=4.50% of main chemical, can V=3.47%；
2）Filtering：By the filtering of roasted vanadic slag leachate, filtrate and filter residue are obtained, filter residue is with 90 DEG C of hot water 200ml
Wash in three times, wash solid-liquid mass ratio 1：2.0, material suction filtration to surface merges cleaning solution with filtrate without liquid phase, is filtered
Slag and solvable vanadium leachate.
Filter residue is removed and is checked after drying in drying baker.The full V of assay：1.18%, can V：0.136%, moisture
13.97%, filtering total elapsed time 7min.
Embodiment 4
A kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag：
1）Leach：100g roasted vanadic slags are added into 95 DEG C of hot water leachings, leaching solid-liquid mass ratio is 1：3.0, stirring
(rotating speed 310r-320r/min) 12min, adjusts pH value to stir 5min to continuation after 7.5 with sulfuric acid, obtains roasting clinker leaching liquor；
Silicone content scope is with SiO in roasting clinker2% is counted：15.0%；Alkali content scope is with Na2CO3% is counted：18.5%, in clinker
The full V=4.62% of main chemical, can V=3.58%；
2）Filtering：By the filtering of roasted vanadic slag leachate, filtrate and filter residue are obtained, filter residue is with 88 DEG C of hot water 200ml
Wash in three times, wash solid-liquid mass ratio 1：2.0, material suction filtration to surface merges cleaning solution with filtrate without liquid phase, is filtered
Slag and solvable vanadium leachate.
Filter residue is removed and is checked after drying in drying baker.The full V of assay：1.20%, can V：0.155%, moisture
13.92%, filtering total elapsed time 8min.
Embodiment 5
A kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag：
1）Leach：100g roasted vanadic slags are added into 93 DEG C of hot water leachings, leaching solid-liquid mass ratio is 1：2.5, stirring
(rotating speed 310r-320r/min) 18min, adjusts pH value to stir 8min to continuation after 7.0 with sulfuric acid, obtains roasting clinker leaching liquor；
Silicone content scope is with SiO in roasting clinker2% is counted：18.0%；Alkali content scope is with Na2CO3% is counted：12.5%, in clinker
The full V=5.54% of main chemical, can V=4.14%；
2）Filtering：By the filtering of roasted vanadic slag leachate, filtrate and filter residue are obtained, filter residue is with 89 DEG C of hot water 250ml
Wash in three times, wash solid-liquid mass ratio 1：2.5, material suction filtration to surface merges cleaning solution with filtrate without liquid phase, is filtered
Slag and solvable vanadium leachate.
Filter residue is removed and is checked after drying in drying baker.The full V of assay：1.52%, can V：0.131%, moisture
13.79%, filtering total elapsed time 8min.
Embodiment 6
A kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag：
1）Leach：100g roasted vanadic slags are added into 97 DEG C of hot water leachings, leaching solid-liquid mass ratio is 1：2.5, stirring
(rotating speed 310r-320r/min) 14min, adjusts pH value to stir 10min to continuation after 7.5 with sulfuric acid, obtains roasting clinker leaching liquor；
Silicone content scope is with SiO in roasting clinker2% is counted：17.0%；Alkali content scope is with Na2CO3% is counted：12.0%, in clinker
The full V=4.83% of main chemical, can V=3.59%；
2）Filtering：By the filtering of roasted vanadic slag leachate, filtrate and filter residue are obtained, filter residue is with 92 DEG C of hot water 250ml
Wash in three times, wash solid-liquid mass ratio 1：2.5, material suction filtration to surface merges cleaning solution with filtrate without liquid phase, is filtered
Slag and solvable vanadium leachate.
Filter residue is removed and is checked after drying in drying baker.The full V of assay：1.35%, can V：0.120%, moisture
14.05%, filtering total elapsed time 8min.
Comparative example 1：
Under with the equal conditions of embodiment 1, check experiment is carried out with water logging roasted vanadic slag, leaching solid-to-liquid ratio is 1：3,
Washing solid-to-liquid ratio 1：2, to be filtered after water logging stirring 15min, assay is respectively full V after filter residue drying：1.40%, 1.61%,
1.23%, 1.24%, 1.54%, 1.33%；Can V：0.136%, 0.285%, 0.162%, 0.191%, 0.126%, 0.119%；Moisture point
It is not：14.30%, 15.10%, 14.10%, 14.66%, 13.98%, 14.25%；Filtration time is respectively 23min, 32min,
16min, 27min, 23min, 22min.
Comparative example 2：
Under with the equal conditions of embodiment 1, check experiment is carried out with water logging roasted vanadic slag, leaching solid-to-liquid ratio is 1：3,
Washing solid-to-liquid ratio 1：2, filtered after water logging stirring 15min, washing filtering total used time i.e. 8min identical with acidleach, this kind of method washing
Time relative reduction, water scouring water is also accordingly reduced, and material can not be washed fully, and the full V of assay is respectively after filter residue drying:
1.69%, 1.85%, 1.31%, 1.51%, 1.79%, 1.64%；Can V be respectively：0.421%, 0.532%, 0.262%, 0.483%,
0.361%, 0.396%；Moisture is respectively 17.96%, 19.85%, 15.98%, 19.22%, 18.16%, 17.88%.
Claims (3)
1. a kind of method that use low-concentration sulfuric acid leaches solvable vanadium from roasted vanadic slag, it is characterised in that the technique step
It is rapid as follows：
1）Leach：Roasted vanadic slag is added >=90 DEG C of hot water leaching, leaching solid-liquid mass ratio is 1：2.5-3.0, stirring
10-20min, adjusts pH value to stir 5-10min to continuation after 6.5-7.0 with sulfuric acid, obtains roasting clinker leaching liquor；The sulfuric acid is low
Concentration sulphuric acid, collocation method is：98% concentrated sulfuric acid is 1 with the volume ratio of water:4, addition sulfuric acid process is persistently stirred；The vanadium
Silicone content scope is with SiO in slag roasting clinker2% is counted：10.0-20.0%；Alkali content scope is with Na2CO3% is counted：7.5-20.0%；
2）Filtering：By roasted vanadic slag leachate filtering, filtrate and filter residue, the hot water wash of filter residue use >=80 DEG C are obtained
Wash, wash solid-liquid mass ratio 1：2.0-2.5, cleaning solution is merged with filtrate, obtains filter residue and solvable vanadium leachate；The hot water
Washing step is：After filter residue water purification to be filtered point, hot wash filter residue, solid-liquid mass ratio 1 are used：2.0-2.5, point 3 washings, finally
It is filtered dry filter residue moisture.
2. the method that use low-concentration sulfuric acid according to claim 1 leaches solvable vanadium from roasted vanadic slag, its feature
It is, the step 2）In be filtered into vacuum filtration.
3. the method that use low-concentration sulfuric acid according to claim 1 and 2 leaches solvable vanadium from roasted vanadic slag, it is special
Levy and be, the step 1）In roasted vanadic slag in silicone content scope with SiO2% is counted：15.0-20.0%；Alkali content scope
With Na2CO3% is counted：12.0-20.0%.
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| US4115110A (en) * | 1977-04-08 | 1978-09-19 | Earth Sciences, Inc. | Vanadium recovery process |
| US4678557A (en) * | 1985-09-09 | 1987-07-07 | Intevep, S.A. | Process for the regeneration of spent catalyst used in the upgrading of heavy hydrocarbon feedstocks |
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