CN103088207B - Efficient vanadium extraction method by performing alkali roasting on vanadium mineral - Google Patents
Efficient vanadium extraction method by performing alkali roasting on vanadium mineral Download PDFInfo
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Abstract
The invention discloses an efficient vanadium extraction method by performing alkali roasting on vanadium mineral. The method comprises the following processing steps of: (1) mixing the vanadium mineral with sodium hydroxide or potassium hydroxide for pellet fabrication, and oxidizing and roasting pellets at the temperature of 300-700 DEG C to obtain roasted clinker; (2) leaching the roasted clinker using water or aqueous alkali corresponding to the step 1, and then carrying out solid-liquid separation to obtain leaching residue and a vanadium dissolution solution; and (3) cooling and crystallizing silicon-removed vanadium digestion solution to obtain vanadate. The alkali roasting is used by the method provided by the invention, because alkali can function as a caking agent in the aggregating process, the caking agent can be saved; not only is the roasting temperature reduced largely and process flow largely shortened, but also no waste gas, ammonia-nitrogen wastewater and the like are discharged, as well as a leachate can be recycled; and a silicate phase can be directly destroyed to promote the destroy and the oxidization of a vanadium phase, and the oxidative enveloping and the leaching hindering of the silicate phase to the vanadium can be prevented so that the efficient vanadium leaching can be realized and the leaching rate can reach more than 95%.
Description
Technical field
The invention belongs to vanadium field of chemical metallurgical technology, especially a kind of method containing vanadium minerals alkaline process roasting efficient vanadium extracting.
Background technology
Vanadium titano-magnetite, vanadium slag, tailings in vanadium extraction, bone coal, silicite navajoite etc. are generally comprised containing the gangue ore deposit of vanadium and the vanadium containing slag of smelting containing vanadium minerals.In China's vanadium chemical industry, vanadium extraction raw material mainly adopts vanadium titano-magnetite and bone coal.Wherein, in the iron ore concentrate that vanadium titano-magnetite obtains after magnetic separation is separated, main component is iron and titanium, and vanadium grade in ore is very low, is about 0.5% ~ 0.8%.From iron ore concentrate, vanadium extraction mainly contains two kinds of methods at present, and one is directly vanadium extraction from iron ore concentrate; Another kind is first through ironmaking, steel-making vanadium extraction from slag again.Directly from iron ore concentrate vanadium extraction research more be sodium oxidation vanadium extracting, iron ore concentrate is through sodium roasting, water law vanadium extraction, and the rate of recovery of vanadium can reach 80%, and outstanding shortcoming is that after leaching, pelletizing can not enter blast-furnace smelting separately.From vanadium slag, vanadium extraction is the main technique of China's vanadium titano-magnetite vanadium extraction, namely vanadium slag is through the technique of rotary kiln sodium roasting, water logging, purification, precipitation, this technique is connected mutually with smelting iron and steel flow process, shortcoming is that the total recovery of vanadium is low, from concentrate to vanadium iron process, the rate of recovery of vanadium is 43% ~ 49%, and a part of vanadium has suffered to blast furnace slag, electric furnace slag and slag without fully extracting loss.
Take vanadium titano-magnetite as raw material production iron, the enterprise of vanadium product all adopts traditional vanadium slag sodium roasting technique vanadium extraction from vanadium slag at present, climbing steel, hold steel, sea, South Africa Wilder, New Zealand Steel Ltd. etc. as China.The technique ultimate principle of sodium roasting is with Na
2cO
3for additive, by high temperature sodium roasting (750-850 DEG C), the vanadium of lower valency is converted into the sodium salt of water-soluble pentavalent vanadium, then to the direct water logging of sodium roasting product, obtains the leaching liquid containing vanadium, after add ammonium salt obtain ammonium poly-vanadate precipitation, after reducing roasting, obtain the oxide product of vanadium.Sodium roasting technique vanadium recovery is low, and single roasting vanadium recovery is about 70%, and after repeatedly roasting, the rate of recovery of vanadium is also only 80%; Maturing temperature high (750 ~ 850 DEG C), and need repeatedly roasting, energy consumption is higher; Harmful HCl, Cl can be produced in roasting process
2deng aggressive gas, contaminate environment.
In sum, in prior art, high containing the maturing temperature existed general in vanadium minerals vanadium extracting process, the vanadium transformation efficiency rate of recovery is low, has the problem such as poisonous gas and a large amount of acid ammonia nitrogen waste water discharges in vanadium removal process.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method containing vanadium minerals alkaline process roasting efficient vanadium extracting that maturing temperature is low, leaching yield is high.
For solving the problems of the technologies described above, the present invention takes following processing step: (1) containing vanadium minerals and sodium hydroxide or potassium hydroxide mixed pelletizing, then 300 ~ 700 DEG C of oxidizing roastings, will obtain roasting grog;
(2) the roasting grog described in utilizes the alkaline solution of water or corresponding step (1) to leach, then solid-liquid separation, obtains leached mud and contains vanadium dissolution fluid;
(3) described in containing vanadium dissolution fluid crystallisation by cooling after silica removal, can vanadate be obtained.
Sodium hydroxide in step of the present invention (1) or the addition of potassium hydroxide are 1% ~ 200% of vanadium minerals quality.Oxidizing roasting atmosphere is one or more in air, oxygen, oxygen-rich air and ozone.The oxidizing roasting time is 0.1 ~ 10h.Preferred maturing temperature is 350 ~ 600 DEG C.Described roasting apparatus is rotary kiln, van-type kiln, retort furnace, pushed bat kiln, tunnel furnace or normal-pressure reaction kettle.
Extraction temperature in step of the present invention (2) is 20 ~ 100 DEG C.Preferred extraction temperature is for being 70 ~ 90 DEG C.Described alkaline concentration is 1 ~ 600g/L.
Carry out desiliconization removal of impurities containing vanadium dissolution fluid by adding desiliconization agent in step of the present invention (3), after removal of impurities, liquid is directly cooled to 0 ~ 50 DEG C to carry out crystallisation by cooling.
Principle of the present invention is: containing vanadium minerals in the basic conditions oxidizing roasting time, alkali not only easily decomposes silicate phase, forms solvend, and then breaks the obstruction to vanadium in the oxidation parcel of vanadium and leaching process; Alkali lye easily decomposes destruction containing vanadium phase simultaneously, easily forms the vanadate of solubility; Form solvable vanadic acid salt face by alkali roasting and destroy silicate parcel phase, and then the efficient stripping of vanadium can be realized.
The beneficial effect adopting technique scheme to produce is: the present invention adopts the method for alkaline process roasting-water or alkaline solution leaching-Crystallization Separation vanadium, can be used for reclaiming vanadium titano-magnetite, vanadium slag, tailings in vanadium extraction, bone coal, silicite navajoite etc. containing the vanadium in the gangue ore deposit of vanadium and the vanadium containing slag of smelting.
The present invention adopts alkaline process roasting, because alkali has the effect of binding agent in the group's of making process, so can save binding agent; Compare traditional sodium-salt calcination, not only maturing temperature reduces greatly, technical process shortens greatly, simultaneously without the discharge of waste gas, ammonia nitrogen waste water etc., leach liquor can recycle; Alkaline process roasting directly can destroy silicate phase, promotes destruction and the oxidation of vanadium phase, and avoid silicate phase to the oxidation parcel of vanadium and leach obstruction, thus realizing the efficient leaching of vanadium, leaching yield can reach more than 95%.
The present invention has that maturing temperature is low, vanadium transformation efficiency is high, the feature of energy-conserving and environment-protective, can be widely used in the vanadium extraction containing vanadium minerals; Can obtain vanadic acid sodium or potassium vanadate product, vanadic acid sodium can be converted into calcium vanadate or V
2o
5, and potassium vanadate can directly be sold as high purity product.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is process flow diagram of the present invention.
Embodiment
Shown in embodiment 1: Fig. 1, this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
(1) prepare burden: the NaOH of 1kg vanadium titano-magnetite and 100g is carried out pelletizing in granulating disc, obtains pelletizing feed; Wherein, V is contained in vanadium titano-magnetite
2o
51.2wt%, SiO
26.5wt%;
(2) react: pelletizing feed is put into box kiln and be heated to 350 DEG C of reaction 5h, after reaction, Low Valent Vanadium is oxidized to pentavalent and reacts with NaOH and generates vanadic acid sodium, obtains roasting grog;
(3) leach: step (2) gained roasting grog is leached in water in 80 DEG C, roasting grog: water=5:1(weight); Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add conventional aluminum desiliconization agent desiliconization in step (3) gained dissolution fluid, filters and obtains liquid after removal of impurities slag and removal of impurities;
(5) vanadium is reclaimed: leaching liquid after step (4) gained removal of impurities being used for next step (3), Vanadium Concentrationin concentration is higher than after 7g/L, and 25 DEG C of crystallisation by cooling obtain 28.5g sodium vanadate crystal, Na
3vO
43H
2o purity is 98%.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 90%.
Embodiment 2: this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
(1) prepare burden: the NaOH of 1kg vanadium slag and 500g is carried out pelletizing in granulating disc, obtains pelletizing feed; Wherein, V is contained in vanadium slag
2o
512wt%, SiO
220wt%;
(2) react: pelletizing feed is put into pushed bat kiln, in oxygen, be heated to 500 DEG C of reaction 3h, after reaction, Low Valent Vanadium is oxidized to pentavalent and reacts with NaOH and generates vanadic acid sodium, obtains roasting grog;
(3) leach: by step (2) gained roasting grog in 90 DEG C, leach in the NaOH solution of 300g/L, liquid-solid ratio is 5:1(weight); Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add conventional calcium desiliconization agent removal of impurities in step (3) gained dissolution fluid, filtration obtains liquid after removal of impurities slag and removal of impurities;
(5) reclaim vanadium: by liquid after removal of impurities in 0 DEG C of crystallisation by cooling, can obtain 305g sodium vanadate crystal, its purity is 85%, through the washing of vanadic acid sodium saturated solution, its purity can reach 98%.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 96%.
Embodiment 3: this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
(1) prepare burden: the KOH of 1000g tailings in vanadium extraction and 300g is carried out pelletizing in granulating disc, obtains pelletizing feed; Wherein, V is contained in tailings in vanadium extraction
2o
52wt%, SiO
220wt%;
(2) react: pelletizing feed is put into rotary kiln, in oxygen-rich air, be heated to 700 DEG C of reaction 1h, after reaction, barium oxide and KOH react and generate potassium vanadate, obtain roasting grog;
(3) leach: by step (2) gained roasting grog in 50 DEG C, leach in the KOH solution of 600g/L, liquid-solid ratio is 5:1(weight); Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add the removal of impurities of calcium desiliconization agent in step (3) gained dissolution fluid, filters and obtains liquid after removal of impurities slag and removal of impurities;
(5) vanadium is reclaimed: liquid after removal of impurities is cooled to 10 DEG C, and crystallization obtains 46g potassium vanadate crystal, and its purity is 96%.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 95%.
Embodiment 4: this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
(1) prepare burden: the NaOH of 1kg bone coal and 200g is carried out pelletizing in granulating disc, obtains pelletizing feed; Wherein, V is contained in bone coal
2o
51.2wt%;
(2) react: pelletizing feed is put into tunnel furnace, in ozone, be heated to 600 DEG C of reaction 3h, after reaction, Low Valent Vanadium oxide compound and NaOH react and generate vanadic acid sodium, obtain roasting grog;
(3) leach: by step (2) gained roasting grog in 85 DEG C, leach in the NaOH solution of 200g/L, liquid-solid ratio is 5:1(weight); Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add the removal of impurities of calcium desiliconization agent in step (3) gained dissolution fluid, filters and obtains liquid after removal of impurities slag and removal of impurities;
(5) vanadium is reclaimed: be used for by liquid after step (4) gained removal of impurities leaching next time, after Vanadium Concentrationin to 6g/L, be cooled to 50 DEG C, crystallization obtains 28g vanadic acid sodium crystal, and its purity is 98.5%.After the crystallization obtained after crystallization, liquid can be used as the leach liquor that next time leaches operation.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 90%.
Embodiment 5: this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
(1) prepare burden: the NaOH of 500g vanadium slag and 1kg is ground, obtains powder-mixed material; Wherein, V is contained in vanadium slag
2o
515wt%, SiO
225wt%;
(2) react: powder is put into atmospheric agitation reactor, in oxygen and ozone gas mixture, be heated to 300 DEG C of reaction 10h, after reaction, Low Valent Vanadium oxide compound and NaOH react and generate vanadic acid sodium, obtain roasting grog;
(3) leach: by step (2) gained roasting grog in 70 DEG C, leach in the NaOH solution of 1g/L, liquid-solid ratio is 8:1(weight); Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add the removal of impurities of aluminum desiliconization agent in step (3) gained dissolution fluid, filters and obtains liquid after removal of impurities slag and removal of impurities;
(5) vanadium is reclaimed: liquid after step (4) gained removal of impurities is cooled to 40 DEG C, and crystallization obtains 196g sodium vanadate crystal, and its purity is 98%.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 99%.
Embodiment 6: this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
(1) prepare burden: 1kg vanadium titano-magnetite and 10g KOH are carried out pelletizing in granulating disc, obtains pelletizing feed; Wherein, V is contained in vanadium titano-magnetite
2o
51.2wt%, SiO
26.5wt%;
(2) react: pelletizing feed is put into retort furnace, in air and ozone gas mixture, be heated to 650 DEG C of reaction 0.1h, after reaction, Low Valent Vanadium is oxidized to pentavalent and reacts with KOH and generates potassium vanadate, obtains roasting grog;
(3) leach: by step (2) gained roasting grog in 100 DEG C, leach in the KOH solution of 1.0g/L, roasting grog: water=5:1(weight); Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add conventional aluminum desiliconization agent desiliconization in step (3) gained dissolution fluid, filters and obtains liquid after removal of impurities slag and removal of impurities;
(5) vanadium is reclaimed: liquid after step (4) gained removal of impurities is cooled to 50 DEG C, and crystallization obtains 27g potassium vanadate product, and its purity is 98.5%.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 89%.
Embodiment 7: this processing step containing the method for vanadium minerals alkaline process roasting efficient vanadium extracting is as described below.
The present embodiment is except step (3), and all the other steps are identical with embodiment 2;
Step (3): by 1kg V
2o
5taste for 10wt% roasting grog in 20 DEG C, leach in the NaOH solution of 100g/L, then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium, dissolution fluid obtains 241g vanadic acid sodium crystal through crystallisation by cooling.
After testing, calculate, in the present embodiment, the rate of recovery of vanadium is 92%.
Claims (5)
1., containing a method for vanadium minerals alkaline process roasting efficient vanadium extracting, it is characterized in that, the method adopts following processing step:
(1) will containing vanadium minerals vanadium slag and sodium hydroxide or potassium hydroxide mixed pelletizing, then 300 ~ 500 DEG C of oxidizing roastings, the oxidizing roasting time is 0.1 ~ 10h, obtains roasting grog; The addition of sodium hydroxide or potassium hydroxide is 1% ~ 50% of vanadium slag quality;
(2) the roasting grog described in utilizes the alkaline solution of water or corresponding step (1) to leach, then solid-liquid separation, obtains leached mud and contains vanadium dissolution fluid; Extraction temperature is 70 ~ 90 DEG C, and alkaline concentration is 1 ~ 600g/L;
(3) described in containing vanadium dissolution fluid crystallisation by cooling after silica removal, can vanadate be obtained; Carry out desiliconization removal of impurities containing vanadium dissolution fluid by adding desiliconization agent, after removal of impurities, liquid is directly cooled to 0 ~ 50 DEG C to carry out crystallisation by cooling.
2. the method containing vanadium minerals alkaline process roasting efficient vanadium extracting according to claim 1, is characterized in that: in described step (1), oxidizing roasting atmosphere is one or more in air, oxygen, oxygen-rich air and ozone.
3. the method containing vanadium minerals alkaline process roasting efficient vanadium extracting according to claim 1, is characterized in that: described maturing temperature is 350 ~ 500 DEG C.
4. the method containing vanadium minerals alkaline process roasting efficient vanadium extracting according to claim 1-3 any one, is characterized in that: described roasting apparatus is rotary kiln, van-type kiln, retort furnace, pushed bat kiln, tunnel furnace or normal-pressure reaction kettle.
5. the method containing vanadium minerals alkaline process roasting efficient vanadium extracting according to claim 1-3 any one, is characterized in that: processing step is as described below:
(1) prepare burden: the NaOH of 1kg vanadium slag and 500g is carried out pelletizing in granulating disc, obtains pelletizing feed; Wherein, V is contained in vanadium slag
2o
512wt%, SiO
220wt%;
(2) react: pelletizing feed is put into pushed bat kiln, in oxygen, be heated to 500 DEG C of reaction 3h, after reaction, Low Valent Vanadium is oxidized to pentavalent and reacts with NaOH and generates vanadic acid sodium, obtains roasting grog;
(3) leach: by step (2) gained roasting grog in 90 DEG C, leach in the NaOH solution of 300g/L, solvent and solute weight ratio is 5:1; Then carry out filtering and obtain leached mud and the dissolution fluid containing vanadium;
(4) removal of impurities: add conventional calcium desiliconization agent removal of impurities in step (3) gained dissolution fluid, filtration obtains liquid after removal of impurities slag and removal of impurities;
(5) reclaim vanadium: by liquid after removal of impurities in 0 DEG C of crystallisation by cooling, can obtain 305g sodium vanadate crystal, its purity is 85%, through the washing of vanadic acid sodium saturated solution, its purity is 98%.
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