CN106756007B - A kind of leaching method for extracting vanadium from stone coal - Google Patents
A kind of leaching method for extracting vanadium from stone coal Download PDFInfo
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- CN106756007B CN106756007B CN201611104969.9A CN201611104969A CN106756007B CN 106756007 B CN106756007 B CN 106756007B CN 201611104969 A CN201611104969 A CN 201611104969A CN 106756007 B CN106756007 B CN 106756007B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to a kind of leaching methods for extracting vanadium from stone coal.Its technical solution is：By bone coal ore fine grinding, bone coal powder is obtained.Hydrochloric acid solution with the bone coal powder by liquid-solid ratio for 1.2~1.7L/kg is mixed, is activated, ore pulp after being activated.Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, obtain leaching preceding ore pulp.Wherein：The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.09~0.15)；The mass ratio of sulfate ion and the bone coal powder is (0.019 ~ 0.058) in the exciting agent: 1；The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.005~0.022）∶1.Ore pulp before the leaching is fed in autoclave, leaches 1~3h under conditions of 130~160 DEG C and partial pressure of oxygen is 0.5~1.5MPa, separation of solid and liquid obtains pickle liquor and acid leaching residue.The present invention has the characteristics that efficient, environmental-friendly and V leaching rate is high.
Description
Technical field
The invention belongs to extracting vanadium from stone coal technical fields.More particularly to a kind of leaching method for extracting vanadium from stone coal.
Background technology
Bone coal is that China is a kind of important containing vanadium resource, and in China's rich reserves, the reserves of contained vanadium are calculated as with V2O5
1.18 hundred million tons, account for the 87% of domestic gross reserves.Mica-type Rock coal containing alum is a kind of intractable primary bone coal navajoite, and vanadium is mostly with V
（Ⅲ）Based on, preservation is in the lattice structure of mica mineral, V（Ⅳ）And V（Ⅴ）Content is relatively low.To ensure that high vanadium leaches
Rate, the sour dosage needed for the direct acidleach of traditional normal pressure is big, and extraction time is long, causes leaching efficiency low and is unfavorable for subsequently adjusting pH
Value.Therefore, the novel leaching method of exploitation efficiently, environmentally friendly is very necessary to the development of extracting vanadium from stone coal industry.
In recent years, stone coal oxygen pressure was acid-leaching vanadium-extracted obtains the concern of many technical staff, it is proposed that some oxygen press the new work of acidleach
Skill.Such as the introducing of pressure field, Leach reaction temperature is improved, though reaction rate is accelerated to a certain extent and is conducive to improve
V leaching rate, but there are still the problems such as sour dosage height and long extraction time." a kind of method of leaching vanadium in ore deposit from Rock coal containing alum "
（CN101481755A）Patented technology, the technique that acidleach is pressed using two sections of oxygen, the leaching vanadium under the action of oxygen and sulfuric acid are improved
V leaching rate, but two sections of oxygen pressure leaching times are longer, and equipment investment cost is high." conversion is aoxidized from bone coal under pressure field
The method of Leaching Vanadium "（CN1904092A）Patented technology adds in oxidant during oxygen presses acidleach（Oxygen or air）.The oxygen
Agent is routinely easy to get, environmental-friendly, but the direct transformation efficiency of vanadium is low, and leaching effect is not notable.A kind of " the joint leaching of bone coal
The method of vanadium "（CN200710066424.8）Patented technology, using preneutralization-normal pressure preimpregnation-oxygen leaching combined vanadium leaching
Method, vanadium extraction effect is preferable, but complex process, and extraction time is long, and leaching efficiency is relatively low.A kind of " Rock coal containing alum pressure leaching
With catalyst "（CN200710066335.3）Patented technology, using ferrous sulfate as catalyst, the divalent under the action of oxygen
Iron ion is oxidized to ferric ion, and trivalent vanadium is oxidized to high price vanadium and molten using the strong oxidizing property of ferric ion
Go out, obtain preferable V leaching rate.But due in bone coal mica group mineral structure stablize, trivalent vanadium by mica lattice beam
It ties up, only relies on the oxidation of ferric ion, trivalent vanadium is difficult to be released effectively.
Invention content
The present invention is directed to overcome prior art defect, it is therefore an objective to provide it is a kind of it is efficient, environmental-friendly and V leaching rate is high
For the leaching method of extracting vanadium from stone coal.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 75~90wt% less than 74 μm, obtains bone coal powder.
Step 2: hydrochloric acid activation
Hydrochloric acid solution and the bone coal powder mixs by liquid-solid ratio for 1.2~1.7L/kg, activation 30 under room temperature~
60min, ore pulp after being activated.
The volumetric concentration of the hydrochloric acid solution is 4~8%.
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, leached
Preceding ore pulp.Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.09~0.15)；
The mass ratio of sulfate ion and the bone coal powder is (0.019 ~ 0.058) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.005~0.022）∶1.
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, in the condition of 130~160 DEG C and partial pressure of oxygen for 0.5~1.5MPa
1~3h of lower leaching obtains acidleach slurry.
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue.
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；
V2O5Grade is 0.6~1.2wt%.
The exciting agent is one kind in potassium sulfate, sodium sulphate, magnesium sulfate, copper sulphate and zinc sulfate.
The calcium base carrier is one or more of calcium chloride and dead plaster.
Due to using the above method, the generated advantageous effect of the invention compared with existing acidleach method is：
1st, under room temperature bone coal raw ore is enhanced in advance using calcite and pyrite in hydrochloric acid solution removing bone coal raw ore
The surface texture defect of grain, is conducive to the dissolving of muscovite particle, vanadium is made to be easier to be leached, extraction time foreshortens to 1~3h.
2nd, external excitation agent and calcium base carrier under the high temperature conditions, improve the solution degree of supersaturation of calcium sulfate, realize
Nucleation and growth of the calcium sulphate crystal in bone coal grain structure fault location, especially in crack or nook, produce stress with
Strain makes bone coal particle that local deformation occur, and promotes the cracking of bone coal particle, increases the reaction interface of mica and acid, realize V
(III) efficient release.After measured, V leaching rate is 84.27~95.45%, significantly improves the leaching of vanadium for obtained pickle liquor
Extracting rate.
3rd, the exciting agent and calcium base carrier selected by the present invention, is routinely easy to get, environmental-friendly, leaching process does not generate pollution
Property gas.
4th, calcium content is high in the acid leaching residue of present invention gained, is conducive to the comprehensive utilization of tailings.
Therefore, the present invention has the characteristics that efficient, environmental-friendly and V leaching rate is high.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limitation of its protection domain.
Embodiment 1
A kind of leaching method for extracting vanadium from stone coal.Leaching method described in the present embodiment comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 75~81wt% less than 74 μm, obtains bone coal powder.
Step 2: hydrochloric acid activation
Hydrochloric acid solution and the bone coal powder mixs by liquid-solid ratio for 1.2~1.5L/kg, activation 30 under room temperature~
51min, ore pulp after being activated.
The volumetric concentration of the hydrochloric acid solution is 4~8%.
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, leached
Preceding ore pulp.Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.09~0.11)；
The mass ratio of sulfate ion and the bone coal powder is (0.019 ~ 0.040) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.005~0.012）∶1.
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, in the condition of 130~140 DEG C and partial pressure of oxygen for 0.5~1.1MPa
1~1.3h of lower leaching obtains acidleach slurry.
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue.
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；
V2O5Grade is 0.6~0.8wt%.
The exciting agent is potassium sulfate.
The calcium base carrier is calcium chloride.
After measured, V leaching rate is 84.27~91.02% for pickle liquor obtained by the present embodiment.
Embodiment 2
A kind of leaching method for extracting vanadium from stone coal.Leaching method described in the present embodiment comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 77~83wt% less than 74 μm, obtains bone coal powder.
Step 2: hydrochloric acid activation
Hydrochloric acid solution and the bone coal powder mixs by liquid-solid ratio for 1.25~1.55L/kg, activation 32 under room temperature~
53min, ore pulp after being activated.
The volumetric concentration of the hydrochloric acid solution is 4~8%.
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, leached
Preceding ore pulp.Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.10~0.12)；
The mass ratio of sulfate ion and the bone coal powder is (0.024 ~ 0.045) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.008~0.015）∶1.
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, in the condition of 135~145 DEG C and partial pressure of oxygen for 0.6~1.2MPa
1.2~1.7h of lower leaching obtains acidleach slurry.
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue.
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；
V2O5Grade is 0.65~0.9wt%.
The exciting agent is sodium sulphate.
The calcium base carrier is calcium chloride.
After measured, V leaching rate is 86.11~92.34% for pickle liquor obtained by the present embodiment.
Embodiment 3
A kind of leaching method for extracting vanadium from stone coal.Leaching method described in the present embodiment comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 79~85wt% less than 74 μm, obtains bone coal powder.
Step 2: hydrochloric acid activation
Hydrochloric acid solution and the bone coal powder mixs by liquid-solid ratio for 1.3~1.6L/kg, activation 34 under room temperature~
55min, ore pulp after being activated.
The volumetric concentration of the hydrochloric acid solution is 4~8%.
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, leached
Preceding ore pulp.Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.11~0.13)；
The mass ratio of sulfate ion and the bone coal powder is (0.029 ~ 0.050) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.011~0.017）∶1.
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, in the condition of 140~150 DEG C and partial pressure of oxygen for 0.7~1.3MPa
1.4~2.1h of lower leaching obtains acidleach slurry.
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue.
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；
V2O5Grade is 0.7~1.0wt%.
The exciting agent is magnesium sulfate.
The calcium base carrier is calcium chloride and the mixture of dead plaster.
After measured, V leaching rate is 88.02~93.23% for pickle liquor obtained by the present embodiment.
Embodiment 4
A kind of leaching method for extracting vanadium from stone coal.Leaching method described in the present embodiment comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 81~87wt% less than 74 μm, obtains bone coal powder.
Step 2: hydrochloric acid activation
Hydrochloric acid solution and the bone coal powder mixs by liquid-solid ratio for 1.35~1.65L/kg, activation 36 under room temperature~
57min, ore pulp after being activated.
The volumetric concentration of the hydrochloric acid solution is 4~8%.
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, leached
Preceding ore pulp.Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.12~0.14)；
The mass ratio of sulfate ion and the bone coal powder is (0.034 ~ 0.054) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.014~0.019）∶1.
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, in the condition of 145~155 DEG C and partial pressure of oxygen for 0.8~1.4MPa
1.6~2.5h of lower leaching obtains acidleach slurry.
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue.
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；
V2O5Grade is 0.75~1.1wt%.
The exciting agent is copper sulphate.
The calcium base carrier is dead plaster.
After measured, V leaching rate is 90.02~94.75% for pickle liquor obtained by the present embodiment.
Embodiment 5
A kind of leaching method for extracting vanadium from stone coal.Leaching method described in the present embodiment comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 83~90wt% less than 74 μm, obtains bone coal powder.
Step 2: hydrochloric acid activation
Hydrochloric acid solution and the bone coal powder mixs by liquid-solid ratio for 1.4~1.7L/kg, activation 38 under room temperature~
60min, ore pulp after being activated.
The volumetric concentration of the hydrochloric acid solution is 4~8%.
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, leached
Preceding ore pulp.Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.13~0.15)；
The mass ratio of sulfate ion and the bone coal powder is (0.039 ~ 0.058) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is in the calcium base carrier（0.017~0.022）∶1.
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, in the condition of 150~160 DEG C and partial pressure of oxygen for 0.9~1.5MPa
1.7~3.0h of lower leaching obtains acidleach slurry.
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue.
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；
V2O5Grade is 0.8~1.2wt%.
The exciting agent is zinc sulfate.
The calcium base carrier is dead plaster.
After measured, V leaching rate is 92.10~95.45% for pickle liquor obtained by the present embodiment.
Present embodiment generated advantageous effect compared with existing acidleach method is：
1st, under room temperature bone coal raw ore is enhanced in advance using calcite and pyrite in hydrochloric acid solution removing bone coal raw ore
The surface texture defect of grain, is conducive to the dissolving of muscovite particle, vanadium is made to be easier to be leached, extraction time foreshortens to 1~3h.
2nd, external excitation agent and calcium base carrier under the high temperature conditions, improve the solution degree of supersaturation of calcium sulfate, realize
Nucleation and growth of the calcium sulphate crystal in bone coal grain structure fault location, especially in crack or nook, produce stress with
Strain makes bone coal particle that local deformation occur, and promotes the cracking of bone coal particle, increases the reaction interface of mica and acid, realize V
(III) efficient release.After measured, V leaching rate is 84.27~95.45%, significantly improves the leaching of vanadium for obtained pickle liquor
Extracting rate.
3rd, the exciting agent selected by present embodiment and calcium base carrier, are routinely easy to get, environmental-friendly, and leaching process is not
Generate pollution gas.
4th, calcium content is high in the acid leaching residue obtained by present embodiment, is conducive to the comprehensive utilization of tailings.
Therefore, present embodiment has the characteristics that efficient, environmental-friendly and V leaching rate is high.
Claims (2)
1. a kind of leaching method for extracting vanadium from stone coal, it is characterised in that the leaching method comprises the concrete steps that：
Step 1: ore grinding
Bone coal ore fine grinding to granularity is accounted for into 75~90wt% less than 74 μm, obtains bone coal powder；
Step 2: hydrochloric acid activation
Hydrochloric acid solution with the bone coal powder by liquid-solid ratio for 1.2~1.7L/kg is mixed, 30~60min is activated under room temperature, is obtained
Ore pulp after to activation；
The volumetric concentration of the hydrochloric acid solution is 4~8%；
Step 3: it sizes mixing
Ore pulp after the activation is added in the concentrated sulfuric acid, is uniformly mixed, is added exciting agent and calcium base carrier, obtain leaching preceding ore deposit
Slurry；Wherein：
The ratio between ore pulp and the volume of the concentrated sulfuric acid are 1 after the activation: (0.09~0.15)；
The mass ratio of sulfate ion and the bone coal powder is (0.019~0.058) in the exciting agent: 1；
The mass ratio of calcium ion and the bone coal powder is (0.005~0.022) in the calcium base carrier: 1；
Step 4: pressure leaching
Ore pulp before the leaching is fed in autoclave, is soaked under conditions of 130~160 DEG C and partial pressure of oxygen is 0.5~1.5MPa
Go out 1~3h, obtain acidleach slurry；
Step 5: separation of solid and liquid
The acidleach is starched and carries out separation of solid and liquid, obtains pickle liquor and acid leaching residue；
The bone coal raw ore for vanadium by lower valency and it is isomorphous in the form of Rock coal containing alum of the preservation in mica mineral；V2O5
Grade is 0.6~1.2wt%；
The exciting agent is one kind in potassium sulfate, sodium sulphate, magnesium sulfate, copper sulphate and zinc sulfate.
2. the leaching method according to claim 1 for extracting vanadium from stone coal, it is characterised in that the calcium base carrier is chlorination
One or more of calcium and dead plaster.
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| CN101935755A (en) * | 2010-09-15 | 2011-01-05 | 长沙达华矿业技术开发有限公司 | Two-stage leaching method for vanadium in vanadium-containing ore |
| CN102828025A (en) * | 2012-09-20 | 2012-12-19 | 长沙矿冶研究院有限责任公司 | Method for extracting V2O5 from stone coal navajoite |
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