CN102560155A - Method for extracting vanadium from stone coal vanadium ore by using calcium compound additive - Google Patents
Method for extracting vanadium from stone coal vanadium ore by using calcium compound additive Download PDFInfo
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- CN102560155A CN102560155A CN2012100407714A CN201210040771A CN102560155A CN 102560155 A CN102560155 A CN 102560155A CN 2012100407714 A CN2012100407714 A CN 2012100407714A CN 201210040771 A CN201210040771 A CN 201210040771A CN 102560155 A CN102560155 A CN 102560155A
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Abstract
The invention relates to a method for extracting vanadium from a stone coal vanadium ore by using a calcium compound additive. The method comprises the following steps of: uniformly mixing the stone coal vanadium ore and the calcium compound additive, and grinding into raw material powder of less than 60 meshes; and roasting the raw material powder at the temperature of between 780 and 880 DEG C for 1 to 2 hours, and cooling to obtain roasted clinker for leaching. The invention has the prominent characteristics that: the roasting conversion rate is high and is over 80 percent; the roasting temperature is low and is 100-250 DEG C lower than that in a pure calcified roasting process, and the roasting time is short and is only 1 to 2 hours, so energy consumption is low; pollution is light, waste gas reaches the standard and is discharged after being subjected to simple lime water spray washing, and liquid obtained after spraying can be used for mixing; and the method is suitable for a process for extracting the vanadium from multiple kinds of refractory stone coal.
Description
Technical field
The present invention relates to a kind of method of from bone coal, extracting vanadium, particularly a kind of method of from bone coal navajoite, extracting vanadium with the calcium composite additive.
Background technology
Bone coal is the navajoite resource of a kind of uniqueness of China, and reserves are very abundant, is distributed in more than 20 province and area, and from bone coal, extracting Vanadium Pentoxide in FLAKES is the important channel that obtains vanadium.In the last few years, to the method for extracting vanadium from stone coal, the many investigators of China had carried out number of research projects, made process for extracting vanadium from stone coal obtain fast development, for condition has been created in the development and use that contain the scherbinaite coal.Because the occurrence status of each department bone coal composition and vanadium differs greatly, therefore, various process for extracting vanadium have also been formed to the bone coal of different areas.In various process for extracting vanadium, most crucial steps at first is how from bone coal, effectively to leach vanadium.Technology from bone coal leaching vanadium mainly can be divided into two big types at present: one type is direct acid leaching process, and another kind of is roasting---extract technology.Directly acid leaching process has the sulfuric acid normal pressure to leach and two kinds of technologies of high pressure leaching.Normal pressure leaches the sulfuric acid that generally need add bone coal mineral amount 15～30%, and in 80～90 ℃ of leachings 18～48 hours, the leaching yield of vanadium was generally 60～70%; Normal pressure leaches that sour consumption is big, and the activity duration is long, and tooling cost is high and investment is big, and only is fit to the bone coal ore deposit that is easier to leach, and limitation is bigger.Adopt the high pressure extract technology, also be with sulfuric acid as leaching agent, aerating oxygen or air boiled 4～8 hours in 150～180 ℃ of pressures simultaneously, its sour consumption and normal pressure leaching are roughly the same, the leaching yield of vanadium can bring up to 70～80%; Though the high pressure extract technology has reduced extraction time, has improved leaching yield, high pressure leaches strict to equipment and technological operation, and its economy also is still waiting further commerical test and accounts, and this technology only is in laboratory stage at present.Developed the roasting of use at present---extract technology then can be subdivided into several kinds of sodium roasting-water logging, blank roasting-acidleach, calcification baking-acid (alkali) soaking technologies etc.Sodium roasting-water logging is a kind of process for extracting vanadium of classics, vanadium total yield 40～50%, and cost is at 4～50,000 yuan/t.V
2O
5, producing toxic and harmfuls such as a large amount of hydrogenchloride, chlorine because of production process, environmental pollution is serious, and is superseded basically at present; Blank roasting-acid leaching process only is suitable for the minority bone coal navajoite; And calcification baking-acid leaching process has solved the exhaust emission problem, but pure calcification baking exists maturing temperature high, generally needs 900～1100 ℃, and roasting time is long, and 3～10 hours, transformation efficiency was on the low side, generally was not higher than 70%, to defectives such as the flexibility of ore are relatively poor.
In order to solve the defective of pure sodium or pure calcification baking technique, many investigators have researched and developed various sodium or calcification composite additive sinter process.Announced that like Chinese patent CN1884597A a kind of baking composite additive with sodium for extracting vanadium is made up of the oxide compound of sodium-chlor, yellow soda ash and transition metal salt; Use this compound roasting additive, can shorten roasting time greatly, the transformation efficiency of vanadium improves 5～10% than making additive with sodium-chlor merely, and the toxic and harmful composition reduces more than 90% in the flue gas.Chinese patent CN101709389A has announced a kind of composite additive and method of use thereof that is used for extracting vanadium from stone coal, has adopted with sodium-chlor, yellow soda ash, sodium sulfate and potassium permanganate and has formed; The recovery that this invention can reduce the consumption of additive, the transformation efficiency that shortens roasting time, assurance vanadium and Vanadium Pentoxide in FLAKES is high.Some common ground of comprehensive sodium composite additive sinter process; All be to mix other oxygenant again as composite additive with sodium salt instead of part sodium-chlor such as yellow soda ash or sodium hydrogencarbonate, sodium sulfate, SODIUMNITRATE, sodium hydroxide; Though on technical indicator, raising is arranged than pure sodium roasting technology; But aspect environmental protection and fail thoroughly to solve the pollution problem of waste gas, waste water also may not have advantage because sodium salt concentration height also is difficult to recycle aspect tooling cost.Aspect calcification composite additive sinter process; Chinese patent CN1752022A has announced a kind of method of from navajoite stone, extracting Vanadium Pentoxide in FLAKES; Adopt unslaked lime to add ethyl heteropolyacid sodium sulfate as additive, 900～980 ℃ of roastings 4～6 hours, average roasting transformation efficiency was about 70%; Chinese patent CN101215648 has announced composite additive and the method for use that is used for from the vanadium extraction of scherbinaite colliery; Adopt lime or Wingdale to join fluorite and form the calcium composite additive; 870～980 ℃ of oxidizing roastings 1.5～7 hours, the roasting transformation efficiency of vanadium can improve 20%.The sinter process of comprehensive existing various calcium composite additives; Than pure calcification baking technique; Its roasting transformation efficiency has all obtained certain raising; But having subject matter still is that unresolved maturing temperature requirement is high, roasting time length causes the high defective of energy consumption, and the flexibility aspect to ore is also strong inadequately simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of method of from bone coal navajoite, extracting vanadium with the calcium composite additive; Can solve that the maturing temperature requirement is high, roasting time length causes the high defective of energy consumption; Flexibility to ore is strong simultaneously, and calcium composite additive sinter process with low cost, that pollution is little.
The process program that the present invention adopts is following: a kind ofly from bone coal navajoite, extract the method for vanadium with the calcium composite additive, comprise the steps:
A. prepare burden: bone coal navajoite is mixed with the calcium composite additive, and be ground to below 60 orders, obtain the raw material powder after mixing thoroughly;
Calcium composite additive add-on is 15～25% of a bone coal navajoite quality, and said calcium composite additive is mixed by 16～20 parts of lime muds of weight part, 1～3 part of villaumite and 1～3 part of villiaumite and gets,
B. roasting: the raw material powder in 780～880 ℃ of roastings 1～2 hour, after the cooling, is obtained the roasting grog and promptly can be used for leaching.
Said bone coal navajoite is that bone coal is through oxidized ore after the weathering or the primary bone coal ore deposit lime-ash after decarburization.
Described lime mud is meant the waste residue that caustic soda, papermaking or aluminum oxide industry produce.
Described villaumite is meant calcium chloride, sodium-chlor, magnesium chloride or Repone K.
Described villiaumite is meant fluorite, Sodium Fluoride or Potassium monofluoride.
800～850 ℃ of preferred maturing temperatures, roasting time 1.5h.
The composition of the bone coal of different areas and the occurrence status of vanadium vary; But in the bone coal of most of areas; Vanadium mainly is present in the mineral such as mica, kaolin, garnet, tourmalinite with trivalent vanadium; The purpose of roasting all is to destroy mineral structure, promotes that vanadium is oxidized to pentavalent, and vanadium is leached easily.Calcium composite additive of the present invention is main with lime mud, and it is formulated to be aided with a spot of villaumite and villiaumite.Lime mud is with CaCO
3Be main, contain minor N aCO simultaneously
3, NaOH, Ca (OH)
2Deng, we can say that lime mud itself is exactly a kind of composite additive, and then be aided with a spot of villaumite and villiaumite, form more multi-component calcium composite additive.Use this roasting additive, can destroy various mineral structures effectively, its flexibility to various bone coals ore deposit is strengthened greatly, multi-component material forms eutectic point easily simultaneously, helps to reduce maturing temperature.
Though calcium composite additive of the present invention also uses a small amount of villaumite and villiaumite; But under the situation that a large amount of calcium exist; Chlorine and the fluorin volatilization amount in the flue gas seldom, flue gas only need use simple liming spray washing to get final product qualified discharge, spray back liquid also can add the use of preparing burden in the raw material powder to; Realize the closed cycle of chlorine and fluorine, therefore whole sinter process pollutes very little.
The present invention has following outstanding advantage:
(1) adopting the industrial waste lime mud is that the master allocates other medicament commonly used into as roasting additive, and raw material is cheap and easy to get, not only helps the method for reducing production costs, and has also digested the waste residue of other industry simultaneously;
(2) the roasting transformation efficiency is high, can reach more than 80%, adopts low acidleach to go out to obtain high leaching yield;
(3) maturing temperature is low, and than low 100～250 ℃ of pure calcification baking technique, and roasting time is short, only need 1～2 hour, so energy consumption is low;
(4) pollution is little, and waste gas gets final product qualified discharge through simple liming spray washing, and spray back liquid can be used for batching.
(5) flexibility is strong, is used for various unmanageable bone coals and all can obtains the good technical index.
Embodiment
Below through specific embodiment technical scheme of the present invention is done further explain.
Embodiment 1
Get the bone coal oxidized ore 1kg in somewhere, Guangxi, add 150g, be ground to below 60 orders, obtain the raw material powder after mixing thoroughly by 20 parts of lime muds, 1 part of calcium chloride, 2 parts of calcium composite additives that fluorite is formulated.Be incubated 120min after placing stoving oven to be warmed up to 780 ℃ the raw material powder, take out after the cooling the roasting grog.The use mass concentration is 4% dilution heat of sulfuric acid, is 2:1 by liquid-solid ratio, and 60 ℃ of following agitation leach grog 20min analyze leach liquor, get V
2O
5Leaching yield 78.74%.
Embodiment 2
Get the bone coal oxidized ore 1kg in somewhere, Guangxi, add 190g, be ground to below 60 orders, obtain the raw material powder after mixing thoroughly by 16 parts of lime muds, 2 parts of calcium chloride, 2 parts of calcium composite additives that fluorite is formulated.Be incubated 70min after placing stoving oven to be warmed up to 800 ℃ the raw material powder, take out after the cooling the roasting grog.The use mass concentration is 4% dilution heat of sulfuric acid, is 2:1 by liquid-solid ratio, and 60 ℃ of following agitation leach grog 20min analyze leach liquor, get V
2O
5Leaching yield 80.92%.
Embodiment 3
Get the bone coal oxidized ore 1kg in somewhere, Guangxi, add 210g, be ground to below 60 orders, obtain the raw material powder after mixing thoroughly by 18 parts of lime muds, 3 parts of calcium chloride, 1 part of calcium composite additive that Sodium Fluoride is formulated.Be incubated 90min after placing stoving oven to be warmed up to 820 ℃ the raw material powder, take out after the cooling the roasting grog.The use mass concentration is 4% dilution heat of sulfuric acid, is 2.5:1 by liquid-solid ratio, and the 60 ℃ of said roasting grog of following agitation leach 20min analyze leach liquor, get V
2O
5Leaching yield 82.33%.
Embodiment 4
Get the lime-ash 1kg of somewhere, Guangxi bone coal primary ore after decarburization, add 200g, be ground to below 60 orders, obtain the raw material powder after mixing thoroughly by 16 parts of lime muds, 2 parts of calcium chloride, 3 parts of calcium composite additives that fluorite is formulated.Be incubated 60min after placing stoving oven to be warmed up to 850 ℃ the raw material powder, take out after the cooling the roasting grog.The use mass concentration is 4% dilution heat of sulfuric acid, is 2.5:1 by liquid-solid ratio, and 60 ℃ of following agitation leach grog 20min analyze leach liquor, get V
2O
5Leaching yield 80.23%.
Embodiment 5
Get the lime-ash 1kg of bone coal primary ore after decarburization in somewhere, Guangxi, add 220g, be ground to below 60 orders, obtain the raw material powder after mixing thoroughly by 18 parts of lime muds, 3 parts of calcium chloride, 2 parts of calcium composite additives that Sodium Fluoride is formulated.Be incubated 90min after placing stoving oven to be warmed up to 820 ℃ the raw material powder, take out after the cooling the roasting grog.The use mass concentration is 4% dilution heat of sulfuric acid, is 2.5:1 by liquid-solid ratio, and 60 ℃ of following agitation leach grog 20min analyze leach liquor, get V
2O
5Leaching yield 80.86%.
Embodiment 6
Get the lime-ash 1kg of bone coal primary ore after decarburization in somewhere, Guangxi, add 250g, be ground to below 60 orders, obtain the raw material powder after mixing thoroughly by 17 parts of lime muds, 3 parts of magnesium chlorides, 2 parts of calcium composite additives that Sodium Fluoride is formulated.Be incubated 60min after placing stoving oven to be warmed up to 880 ℃ the raw material powder, take out after the cooling the roasting grog.The use mass concentration is 4% dilution heat of sulfuric acid, is 2.5:1 by liquid-solid ratio, and 60 ℃ of following agitation leach grog 20min analyze leach liquor, get V
2O
5Leaching yield 79.45%.
Claims (6)
1. one kind is extracted the method for vanadium with the calcium composite additive from bone coal navajoite, it is characterized in that, this method comprises the steps,
A. prepare burden: bone coal navajoite is mixed with the calcium composite additive, and be ground to below 60 orders, obtain the raw material powder after mixing thoroughly;
Calcium composite additive add-on is 15～25% of a bone coal navajoite quality, and said calcium composite additive is mixed by 16～20 parts of lime muds of weight part, 1～3 part of villaumite and 1～3 part of villiaumite and gets,
B. roasting: the raw material powder in 780～880 ℃ of roastings 1～2 hour, after the cooling, is obtained the roasting grog and promptly can be used for leaching.
2. according to from bone coal navajoite, extracting the method for vanadium with the calcium composite additive described in the claim 1, it is characterized in that said maturing temperature is 800～850 ℃, roasting time 1.5h.
3. according to from bone coal navajoite, extracting the method for vanadium with the calcium composite additive described in the claim 1, it is characterized in that said bone coal navajoite is that bone coal is through oxidized ore after the weathering or the primary bone coal ore deposit lime-ash after decarburization.
4. according to from bone coal navajoite, extracting the method for vanadium with the calcium composite additive described in the claim 1, it is characterized in that described lime mud is meant the waste residue that caustic soda, papermaking and aluminum oxide industry produce.
5. according to from bone coal navajoite, extracting the method for vanadium with the calcium composite additive described in the claim 1, it is characterized in that described villaumite is meant calcium chloride, sodium-chlor, magnesium chloride or Repone K.
6. according to from bone coal navajoite, extracting the method for vanadium with the calcium composite additive described in the claim 1, it is characterized in that described villiaumite is meant fluorite, Sodium Fluoride or Potassium monofluoride.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531989A (en) * | 2014-12-22 | 2015-04-22 | 核工业北京化工冶金研究院 | Method for reducing leaching acid consumption and impurity dissolution rate of high-acid-consumption vanadium ore |
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| CN101215648A (en) * | 2008-01-18 | 2008-07-09 | 贵州义信矿业有限公司 | Composite additive used for extracting vanadium from vanadium stone coal ore and using method thereof |
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| CN101857915A (en) * | 2010-06-03 | 2010-10-13 | 浙江大学 | Pelletizing and calcination method for vanadium-containing stone coal ash |
| CN102296192A (en) * | 2011-09-20 | 2011-12-28 | 武汉工程大学 | Composite roasting additive for extracting vanadium pentoxide from vanadium-containing stone coal and application of composite roasting additive |
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- 2012-02-22 CN CN2012100407714A patent/CN102560155A/en active Pending
Patent Citations (8)
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| CN1782108A (en) * | 2004-11-30 | 2006-06-07 | 戴许斌 | Method for producing vanadium by stone coal compound calcifying baking-low acid leaching-special ion exchanging |
| CN1752022A (en) * | 2005-08-12 | 2006-03-29 | 岳阳市中湘实业有限公司 | Method of extracting vanadium pentoxide from vanadium ore |
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| CN101215648A (en) * | 2008-01-18 | 2008-07-09 | 贵州义信矿业有限公司 | Composite additive used for extracting vanadium from vanadium stone coal ore and using method thereof |
| CN101323914A (en) * | 2008-07-29 | 2008-12-17 | 旺苍县振华矿业有限公司 | Process for extracting vanadic anhydride by high calcium calcination |
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| CN101857915A (en) * | 2010-06-03 | 2010-10-13 | 浙江大学 | Pelletizing and calcination method for vanadium-containing stone coal ash |
| CN102296192A (en) * | 2011-09-20 | 2011-12-28 | 武汉工程大学 | Composite roasting additive for extracting vanadium pentoxide from vanadium-containing stone coal and application of composite roasting additive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531989A (en) * | 2014-12-22 | 2015-04-22 | 核工业北京化工冶金研究院 | Method for reducing leaching acid consumption and impurity dissolution rate of high-acid-consumption vanadium ore |
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Application publication date: 20120711 |