CN106521150B - A method of v element in roasting extraction vanadium-containing shale - Google Patents
A method of v element in roasting extraction vanadium-containing shale Download PDFInfo
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Abstract
A method of v element in roasting extraction vanadium-containing shale includes the following steps：Vanadium-containing shale is ground, and presses vanadium-containing shale：The concentrated sulfuric acid：Sulfate=1：0.1~4：0.1~4 mass ratio carries out dispensing；Dispensing is uniformly mixed, 0.5~5h is roasted at 200~400 DEG C；Roasting material is subjected to sulfuric acid solution leaching, a concentration of 0~10wt% of sulfuric acid solution at 30~100 DEG C, leaching time is 0.5~4h, is filtered, v element enters solution；V element in energy high efficiency extraction vanadium-containing shale of the invention, the leaching rate of vanadium>85%, there are rate of recovery height, easy to operate, low power consumption and other advantages.
Description
Technical field
The present invention relates to the decomposition of vanadium-containing shale extractions, in particular it relates in a kind of roasting extraction vanadium-containing shale
The method of v element.
Background technology
Prospects of Rare Metal Vanadium is a kind of important strategic resource, is known as the title of " metal vitamin ", is made in iron and steel metallurgical industry
It can be effectively improved the toughness elasticity, intensity, wearability etc. of alloy for additive, have a wide range of applications；In addition, vanadium is in glass
It can be used as colorant in glass, ceramic industry；In sulfuric acid and petrochemical industry production, catalyst can be used as.In recent years, with warp
The development of Ji and the progress of science and technology, market increases the demand of vanadium product year by year.
The vanadium resource in China is abundant, mainly exists in the form of vanadium titano-magnetite and vanadium-containing shale.Wherein, in vanadium-containing shale
Reserves of the vanadic anhydride grade in 0.5wt% or more are 7797.5 ten thousand tons, are 6.7 of vanadium reserves in China's vanadium titano-magnetite
Times, belong to a kind of peculiar resource in China.China is vanadium resource big country, even more vanadium demand big country.How from China's rich reserves
High efficiency extraction vanadium resource in vanadium-containing shale is always the research hotspot in metallurgy of rare metal field.
For the occurrence status of vanadium mostly based on trivalent, the vanadium under the valence state is relatively insoluble in water or acid, Chang Cai in vanadium-containing shale
It is oxidized to soluble tetravalence or pentavalent vanadium with the method for roasting.On the whole, main to these resources typical case's extraction vanadium method
Have following several：
Sodium roasting-acid 1. (water) soaking technology.The chlorine and Na that the fusion and decomposition of the technology utilization sodium chloride generates2O, will
The vanadium of lower valency is oxidized to pentavalent vanadium, and and Na2O is combined and is formed NaVO soluble easily in water3, the addition of NaCl is ore
10%~20%, calcination temperature is at 780~850 DEG C, 2~3h of roasting time.Water logging is carried out to material after having calcined, passes through acid adding
Red vanadium is sunk when adjusting pH to 1~1.5.It can be obtained refined vanadic anhydride after calcining.The flow is not high to equipment requirement, technology
Simply.But a large amount of pernicious gas is produced in technological process, environmental pollution is larger, and the rate of recovery of vanadium only~
50%, at present the method be eliminated.
Blank 2. (oxidation) roasting-acid (water) soaking technology.Blank roasting refers to the roasting technique for not adding any salt, is compared
It can reduce environmental pollution in sodium roasting.But, the calcination temperature control of this method is more sensitive, and temperature is excessively high to make bone coal
In low-melting-point material be sintered and wrap up vanadium therein, be unfavorable for the leaching of vanadium；Temperature is low and cannot destroy in isomorph and wraps
Wrap up in the crystal structure of vanadium.The method is preferable with vanadium effect existing for ADSORPTION STATE for handling.Generally speaking, the rate of recovery of the method vanadium
It is not high
3. calcification baking-alkali soaking technology.Calcification baking is that lime or lime stone are added to by a certain percentage in navajoite to mix
Material, then roasted, so that the vanadium in mine is oxidized to calcium vanadate not soluble in water but that carbonate solution can be dissolved in, is conducive to the leaching of vanadium
Go out.But, the problem of which has certain selectivity to roasting raw material, and that there are conversion ratios is relatively low for the method, high expensive, no
It is suitble to produce in enormous quantities.
4. compound additive roasting-acid (water) soaking technology.The method is mainly that the compound addition of sodium salt and calcium salt composition is added
Agent is roasted.Research shows that the leaching rate of the vanadium of the method can reach 70% or more, the discharge of pernicious gas can be reduced, is lacked
Point is still that the leaching rate of vanadium is not high.
It is worth noting that, roasting technique above-mentioned it is all different degrees of there is calcination temperature height, V leaching rate it is low (<
80%) the problems such as.Therefore, seek a kind of method gesture of relatively inexpensive vanadium resource rationally and in high efficiency extraction vanadium-containing shale must
Row.
Invention content
The deficiency of process for extracting vanadium technology is roasted for existing vanadium-containing shale, the present invention provides a kind of roasting extraction vanadium-containing shale
The method of middle v element.The method not only can efficiently extract the v element in vanadium-containing shale, but also can effectively reduce roasting temperature
Degree.The required raw material concentrated sulfuric acid, sulfate derive from a wealth of sources and at low cost, and experiment is easily operated and low for equipment requirements, to environment
Close friend meets requirement of the green metallurgical to clean manufacturing.
To achieve the above object, the present invention uses following technical scheme：It is a kind of to roast v element in extraction vanadium-containing shale
Method includes the following steps：
1) it grinds, dispensing：Vanadium-containing shale is ground, until granularity is the mesh of -200 mesh~-400, and presses vanadium-containing shale：Dense sulphur
Acid：Sulfate=1：0.1~4：0.1~4 quality compares dispensing；
2) it roasts：Dispensing in step 1) is uniformly mixed, 0.5~5h is roasted at 200~400 DEG C, is obtained roasting
Material；
3) acidleach, filtering：Material roasting in step 2) is subjected to sulfuric acid solution leaching, sulfuric acid at 30~100 DEG C
Solution concentration is 0~20wt%, and extraction time is 0.5~4h；The filtrate containing v element is obtained by filtration.
Further, the vanadium-containing shale in the step 1), the concentrated sulfuric acid, sulfate mass ratio be 1：0.1~1：0.1~
1。
Further, the sulfate in the step 1) is sodium sulphate, potassium sulfate, ammonium sulfate, one kind in magnesium sulfate or
It is several.
Further, it is roasted to 1~3h of roasting at 200~300 DEG C in the step 2).
Further, when carrying out sulfuric acid solution leaching in the step 3), a concentration of 0~10wt% of sulfuric acid solution,
Solid-to-liquid ratio (g/mL) is 1:4~1:5, temperature is 50~90 DEG C, and leaching time is 0.5~2h.
The key parameter for influencing v element leaching rate in the method for the present invention has vanadium-containing shale：The concentrated sulfuric acid：Sulfate mass ratio,
Calcination temperature, roasting time, acidleach concentration, acidleach temperature, leaching time and solid-to-liquid ratio etc..If calcination temperature is excessively high, the concentrated sulfuric acid
It can partly evaporate, to reduce the sulfuric acid amount for participating in reaction, be unfavorable for effective progress of reaction.The addition of sulfate can be strengthened
Destruction decomposition of the concentrated sulfuric acid to ore internal structure is added to reaction by the similar sulfate of one or more of chemical property
In system, the leaching rate of vanadium can be significantly improved.In addition, it is found that vanadium-containing shale：The concentrated sulfuric acid：Sulfate mass ratio, calcination temperature and
Roasting time limits the influence for having to V leaching rate when variation in range and slightly being reduced after first increase in parameter；It is dense to control acidleach
Degree, acidleach temperature, leaching time and solid-to-liquid ratio can play the role of increasing v element leaching rate.
The beneficial effects of the present invention are：The present invention provides it is a kind of roasting extraction vanadium-containing shale in v element method,
The efficient leaching to v element in vanadium-containing shale is realized, the leaching rate of vanadium greatly improves the utilization of resource 85% or more
Rate.Technical process reaction temperature is low, and energy consumption is significantly reduced for the conventional method that compares；Flow is simple, easy to operate；Raw material
It is at low cost and environmentally safe, there is huge environmental benefit and economic benefit, current green metallurgical can be met to cleaning
The requirement of production.
Description of the drawings
Fig. 1 is that the process flow chart of vanadium resource in vanadium-containing shale is extracted in the roasting of the present invention.
Specific implementation mode
Below in conjunction with the accompanying drawings and the present invention is discussed in detail in specific embodiment.But embodiment below is only limitted to explain this hair
Bright, protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.
Embodiment 1
Technological process is as shown in Figure 1, Hubei province vanadium-containing shale (main chemical compositions are as shown in table 1) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 10g, ammonium sulfate 10g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 200 DEG C, roasting time 1h.Obtained material is added to after having roasted
In sulfuric acid solution (concentration~10wt%), solid-to-liquid ratio (g/mL) is 1:5, it is filtered, is contained after stirring 2h at 90 DEG C
The filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is examined
It surveys, also needs to be detected the v element in filter residue in addition.
It is computed, the leaching rate of vanadium is 85.7%.
1. Hubei province vanadium-containing shale ingredient of table, wt%
Embodiment 2
Technological process is as shown in Figure 1, Hubei province vanadium-containing shale (main chemical compositions are as shown in table 1) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 40g, magnesium sulfate 40g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 250 DEG C, roasting time 1.5h.Obtained material is added after having roasted
Into sulfuric acid solution (concentration~8wt%), solid-to-liquid ratio (g/mL) is 1:5, it is filtered, is contained after stirring 1.5h at 70 DEG C
There is the filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is carried out
Detection.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 87.8%.
Embodiment 3
Technological process is as shown in Figure 1, Hubei province vanadium-containing shale (main chemical compositions are as shown in table 1) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 70g, potassium sulfate 70g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 300 DEG C, roasting time 2h.Obtained material is added to after having roasted
In sulfuric acid solution (concentration~5wt%), solid-to-liquid ratio (g/mL) is 1:4, it is filtered, is obtained containing vanadium after stirring 1h at 60 DEG C
The filtrate of element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is detected.
In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 92.1%.
Embodiment 4
Technological process is as shown in Figure 1, Hubei province vanadium-containing shale (main chemical compositions are as shown in table 1) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 100g, sodium sulphate 100g and be uniformly mixed, put
Enter in Muffle furnace and roasted, control calcination temperature is 300 DEG C, roasting time 3h.Obtained material is added after having roasted
Into sulfuric acid solution (concentration~1wt%), solid-to-liquid ratio (g/mL) is 1:4, it is filtered, is contained after stirring 0.5h at 50 DEG C
There is the filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is carried out
Detection.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 93.4%.
Embodiment 5
Technological process is as shown in Figure 1, Hubei province vanadium-containing shale (main chemical compositions are as shown in table 1) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 100g, sodium sulphate 50g, ammonium sulfate 50g and mix
It closes uniformly, is put into Muffle furnace and is roasted, control calcination temperature is 300 DEG C, roasting time 3h.It will be obtained after having roasted
Material is added in sulfuric acid solution (concentration~1wt%), and solid-to-liquid ratio (g/mL) is 1:4, it was carried out after stirring 0.5h at 50 DEG C
Filter, obtains the filtrate containing v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and to wherein v element
Content is detected.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 94.8%.
Embodiment 6
Technological process is as shown in Figure 1, Jiangxi Area vanadium-containing shale (main chemical compositions are as shown in table 2) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 30g, ammonium sulfate 30g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 200 DEG C, roasting time 1.5h.Obtained material is added after having roasted
Into sulfuric acid solution (concentration~10wt%), solid-to-liquid ratio (g/mL) is 1:5, it is filtered, is contained after stirring 2h at 90 DEG C
There is the filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is carried out
Detection.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 86.1%.
2. Jiangxi Area vanadium-containing shale ingredient of table, wt%
Embodiment 7
Technological process is as shown in Figure 1, Jiangxi Area vanadium-containing shale (main chemical compositions are as shown in table 2) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 50g, magnesium sulfate 50g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 250 DEG C, roasting time 1.5h.Obtained material is added after having roasted
Into sulfuric acid solution (concentration~6wt%), solid-to-liquid ratio (g/mL) is 1:5, it is filtered, is contained after stirring 1h at 80 DEG C
The filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is examined
It surveys.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 88.7%.
Embodiment 8
Technological process is as shown in Figure 1, Jiangxi Area vanadium-containing shale (main chemical compositions are as shown in table 2) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 80g, potassium sulfate 80g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 300 DEG C, roasting time 2.5h.Obtained material is added after having roasted
Into sulfuric acid solution (concentration~3wt%), solid-to-liquid ratio (g/mL) is 1:4, it is filtered, is contained after stirring 1h at 60 DEG C
The filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is examined
It surveys.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 93.1%.
Embodiment 9
Technological process is as shown in Figure 1, Jiangxi Area vanadium-containing shale (main chemical compositions are as shown in table 2) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 90g, sodium sulphate 90g and be uniformly mixed, be put into
It is roasted in Muffle furnace, control calcination temperature is 300 DEG C, roasting time 3h.Obtained material is added to after having roasted
In sulfuric acid solution (concentration~1wt%), solid-to-liquid ratio (g/mL) is 1:4, it is filtered, is contained after stirring 0.5h at 50 DEG C
The filtrate of v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and the content of wherein v element is examined
It surveys.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 95.2%.
Embodiment 10
Technological process is as shown in Figure 1, Jiangxi Area vanadium-containing shale (main chemical compositions are as shown in table 2) 100g is ground
It is the mesh of -200 mesh~-400 to granularity, carries out dispensing with the concentrated sulfuric acid (content 98%) 90g, potassium sulfate 60g, magnesium sulfate 30g and mix
It closes uniformly, is put into Muffle furnace and is roasted, control calcination temperature is 300 DEG C, roasting time 2h.It will be obtained after having roasted
Material is added in sulfuric acid solution (concentration~1wt%), and solid-to-liquid ratio (g/mL) is 1:5, it was carried out after stirring 0.5h at 50 DEG C
Filter, obtains the filtrate containing v element.Obtained filtrate is moved to respectively and carries out constant volume in volumetric flask, and to wherein v element
Content is detected.In addition it also needs to be detected the v element in filter residue.
It is computed, the leaching rate of vanadium is 91.3%.
In conclusion the method that v element in vanadium-containing shale is extracted in roasting proposed by the present invention, realizes to vanadium-containing shale
The efficient leaching of middle v element, the leaching rate of vanadium greatly improve the utilization rate of resource, process engineering operation 85% or more
Simply, there is huge environmental benefit and economic benefit, meet requirement of the current green metallurgical to cleanly production.
Part of that present invention that are not described in detail belong to the well-known technology of those skilled in the art.
Claims (5)
1. a kind of method of v element in roasting extraction vanadium-containing shale, which is characterized in that this approach includes the following steps：
1) it grinds, dispensing：Vanadium-containing shale is ground, until granularity is the mesh of -200 mesh~-400, and presses vanadium-containing shale：The concentrated sulfuric acid：Sulphur
Hydrochlorate=1：0.1~4：0.1~4 quality compares dispensing；
2) it roasts：Dispensing in step 1) is uniformly mixed, 0.5~5h is roasted at 200~400 DEG C, obtains roasting object
Material；
3) acidleach, filtering：Material roasting in step 2) is subjected to sulfuric acid solution leaching, sulfuric acid solution at 30~100 DEG C
A concentration of 0~20wt%, extraction time are 0.5~4h；The filtrate containing v element is obtained by filtration；
Wherein, the sulfate in the step 1) is sodium sulphate, and potassium sulfate is one or more in magnesium sulfate.
2. the method for v element in roasting extraction vanadium-containing shale according to claim 1, which is characterized in that the step
1) mass ratio of vanadium-containing shale, the concentrated sulfuric acid, sulfate in is 1：0.1~1：0.1~1.
3. the method for v element in roasting extraction vanadium-containing shale according to claim 1, which is characterized in that the step 2)
In be roasted at 200~300 DEG C 1~3h of roasting.
4. the method for v element in roasting extraction vanadium-containing shale according to claim 1, which is characterized in that the step
3) when carrying out sulfuric acid solution leaching in, a concentration of 0~10wt% of sulfuric acid solution, solid-to-liquid ratio 1:4~1:5g/mL, temperature are
50~90 DEG C, leaching time is 0.5~2h.
5. the method for v element in the roasting extraction vanadium-containing shale according to any one of claim 1-4, which is characterized in that
The vanadium-containing shale is V2O5Content is more than 0.5wt%.
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| WO2009144382A2 (en) * | 2008-05-30 | 2009-12-03 | Helsinki University Of Technology | Method of producing calcium carbonate from waste and byproducts |
| CN101597697A (en) * | 2009-06-29 | 2009-12-09 | 湘潭大学 | A kind of process for cleanly preparing that from contain the scherbinaite colliery, extracts Vanadium Pentoxide in FLAKES |
| CN102134649A (en) * | 2011-03-03 | 2011-07-27 | 东北大学 | Comprehensive utilization method for vanadium slag |
| CN104388679A (en) * | 2014-09-30 | 2015-03-04 | 边悟 | Method for extracting vanadium from vanadium-containing raw material |
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2015
- 2015-09-09 CN CN201510571454.9A patent/CN106521150B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260464A (en) * | 2008-04-11 | 2008-09-10 | 中南大学 | Stone coal vanadium-extracting ore decomposition method |
| WO2009144382A2 (en) * | 2008-05-30 | 2009-12-03 | Helsinki University Of Technology | Method of producing calcium carbonate from waste and byproducts |
| CN101597697A (en) * | 2009-06-29 | 2009-12-09 | 湘潭大学 | A kind of process for cleanly preparing that from contain the scherbinaite colliery, extracts Vanadium Pentoxide in FLAKES |
| CN102134649A (en) * | 2011-03-03 | 2011-07-27 | 东北大学 | Comprehensive utilization method for vanadium slag |
| CN104388679A (en) * | 2014-09-30 | 2015-03-04 | 边悟 | Method for extracting vanadium from vanadium-containing raw material |
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