CN102732736A - Method for extracting vanadium from burning slag of stone coal vanadium mine fluidized bed - Google Patents
Method for extracting vanadium from burning slag of stone coal vanadium mine fluidized bed Download PDFInfo
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- CN102732736A CN102732736A CN2012102561001A CN201210256100A CN102732736A CN 102732736 A CN102732736 A CN 102732736A CN 2012102561001 A CN2012102561001 A CN 2012102561001A CN 201210256100 A CN201210256100 A CN 201210256100A CN 102732736 A CN102732736 A CN 102732736A
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- vanadium
- roasting
- sulphuric acid
- ammonium sulfate
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Abstract
The invention relates to a method for extracting vanadium from burning slag of a stone coal vanadium mine fluidized bed. The method comprises the following process flows of: grinding the burning slag of the stone coal vanadium mine fluidized bed together with ammonium sulfate, and roasting an obtained ground material at a low temperature; leaching an obtained roasting product by adopting dilute sulphuric acid, and sequentially preparing V2O5 and aluminum compounds from an obtained leaching solution by adopting a conventional method; preparing ammonium sulfate from the solution after aluminum extraction; and returning the obtained aluminum extraction to the grinding procedure for recycling. The invention provides the method for extracting the vanadium by roasting the burning slag of the stone coal vanadium mine fluidized bed at the low temperature and then leaching by using the dilute sulphuric acid, wherein the roasting temperature of the method is only 300-500 DEG C, and compared with the traditional sodication, calcification and low sodium roasting, the roasting temperature of the method is reduced by a half, so the energy consumption is obviously reduced, and the method is easy to implement in industrial production and solves the problem that proper roasting equipment is short of large production lines for extracting the vanadium from stone coal. Due to the method, the vanadium and the aluminum are more easily extracted from the leaching solution by using the traditional technology, and the leaching rates of vanadium and aluminum are respectively more than 88% and 91% which are both higher than those in the traditional method; and the ammonium sulfate is recovered from waste water where the vanadium and the aluminum are extracted and then returned to be used as an ingredient, so the method has the advantages of less consumption auxiliary materials, low processing cost and environmental protection.
Description
Technical field:
Relate to a kind of method that adopts the ammonium sulfate roasting method from bone coal navajoite fluidized-bed combustion lime-ash, to extract vanadium, belong to the chemical industry metallurgical field.
Background technology:
Vanadium is the important strategic goods and materials, and it has many good physicochemical properties and mechanical propertys such as HMP and easy deformation processing, thereby is widely used in the fields such as iron and steel, national defence sophisticated technology, chemical industry and light and textile industries in the The modern industry technology.
China's vanadium resource is mainly composed and is existed in the bone coal, and vanadium extraction is the important development direction that China's vanadium resource utilizes from bone coal.Bone coal also is a kind of low calorie fuels, the about 4000kJ/kg ~ 6000kJ/kg of its thermal value.A few days ago, the technology of bone coal comprehensive utilization is generally: adopt circular fluid bed to produce steam-electric power, from boiler ash, extract Vanadium Pentoxide in FLAKES, tailings in vanadium extraction produces material of construction.From bone coal navajoite fluidized-bed combustion lime-ash, extract Vanadium Pentoxide in FLAKES two class methods are arranged: first kind method is direct acidleach (comprises self-heating mix sour slaking), adopts the high temperature more than 85 ℃, and about 20% sulfuric acid leaches, about 20h of time.From leach liquor, reclaim vanadium with SX or ion exchange process then, the total yield of vanadium is up to 74%.Second class methods are that stone coal ash is carried out re-baking (like sodium roasting, calcification baking, low sodium roasting etc.), and water, acid or alkali leach the roasting material then, from leach liquor, reclaim vanadium with SX or ion exchange process again, V
2O
5Total yield reach 70.7%.Directly acid leaching process acid consumption is high, and energy consumption is high, and production cost is high, and equipment anticorrosion requires high.This technology only is adapted to vanadium and mainly is present in kaolinite, illitic bone coal navajoite with adsorbed state.All between 800 ℃ ~ 950 ℃, roasting time is all more than 2h, on industrial production for the maturing temperature of re-baking; Have only flat kiln can satisfy the requirement of sinter process basically, but flat kiln floor space is big, labor condition is poor; Fluctuation of service; The roasting transformation efficiency is low, and metal recovery rate is low, can't realize large-scale commercial prodn.
Existing in front process for extracting vanadium from stone coal is the recovery of the vanadium 50-74% that only has an appointment not only, the temperature of roasting process up to 800 ℃ ~ 950 ℃, roasting time is longer, can't find and satisfy the large-scale roasting apparatus that processing condition require.
Summary of the invention:
The objective of the invention is in order to overcome the deficiency of above-mentioned prior art; Provide a kind of environmentally friendly; Low simple and practical of energy consumption extracts the method for vanadium from bone coal navajoite fluidized-bed combustion lime-ash, and it is low that this method has a maturing temperature, in industrial production, realizes easily; The recovery is high, and the characteristics of the auxiliary material reusable edible that adds.
Technical scheme of the present invention: with bone coal navajoite fluidized-bed combustion lime-ash and ammonium sulfate combined grinding; The powder that obtains is after 300 ℃ ~ 500 ℃ following roastings; In roasting material, add dilute sulphuric acid and leach, the leach liquor that contains vanadium, aluminium that obtains is liquid after obtaining vanadium extraction liquid and vanadium extraction behind the extraction separation vanadium; By separate in the liquid after the vanadium extraction obtain aluminum compound after, obtain carrying aluminium waste water, by carrying reclaim(ed) sulfuric acid ammonium in the aluminium waste water, the ammonium sulfate recycling of recovery.
The present invention's preferred bone coal navajoite fluidized combustion lime-ash and ammonium sulfate are that the mixed of 1:0.4 ~ 1.5 is carried out grinding by mass ratio, and the granularity of 60 ~ 90% mix grinding material is advisable less than 0.043mm.
Powder roasting time behind the described grinding is 1h ~ 5h.
Roasting material is added mass percent concentration≤10% dilute sulphuric acid agitation leach down at 40 ℃ ~ 80 ℃.The mass percent concentration of preferred dilute sulphuric acid is 4～10%.
Adopting the time of dilute sulphuric acid agitation leach is 0.5h ~ 3h, and the dilute sulphuric acid quality is 1 ~ 2 times of roasting material.
The described leach liquor that contains vanadium, aluminium is ion exchange method or solvent extration extraction by routine through the extraction separation vanadium.
Said aluminum compound is tschermigite, white lake or aluminum oxide.
Produce flue gas in the said roasting process and then join in the step of extraction separation aluminum compound, further recycle.
Technological process of the present invention comprises following step:
1) bone coal navajoite fluidized-bed combustion lime-ash and ammonium sulfate are pressed grinding in mass ratio 1:0.4 ~ 1.5 batching back entering milling equipments;
2) place roasting apparatus through 300 ~ 500 ℃ of following roasting 1h-5h the powder behind the grinding;
3) roasting material is put into reactor drum, add dilute sulphuric acid, heating, stirring 0.5 ~ 3h after-filtration obtain leach liquor;
4) from leach liquor, extract V with common process
2O
5
5) after vanadium extraction, press common process the liquid and extract aluminum compound;
6) the present invention also utilizes baking flue gas as carrying the aluminium auxiliary material, reaches the purpose of further recycle.
7) reclaim(ed) sulfuric acid ammonium from carry aluminium waste water;
8) ammonium sulfate that reclaims returns the powder-grinding process batching again.
The concrete technological process that the present invention implements is:
Bone coal navajoite fluidized-bed combustion lime-ash and ammonium sulfate are pressed batching back, 1:0.4 ~ 1.5 (wt) get into grinding in the milling equipments (like ball mill), 60 ~ 90% granularity is arranged in the control grinding material less than 0.043mm.Powder behind the grinding is put into stoving oven (like external-heating rotary kiln) at 300 ~ 500 ℃ of following roasting 1h-5h postcooling; Adding weight is 1 ~ 2 times dilute sulphuric acid (its mass percent concentration≤10%) in roasting material; Be heated to 40 ~ 80 ℃ of following agitation leach 0.5 ~ 3h; Filter, obtain containing the leach liquor of vanadium, aluminium; (adopting ordinary method such as ion exchange method or solvent extration) extracted vanadium from leach liquor, finally obtain V
2O
5Again after the vanadium extraction after the leach liquor vanadium extraction the liquid (pressing common process) extract aluminum compound; Waste water behind the aluminium concentrates with carrying, crystallisation by cooling, obtains ammonium sulfate; The ammonium sulfate that recovery obtains returns the powder-grinding process batching again, recycles.
Ultimate principle of the present invention:
The atomic radius of vanadium is 132pm, and the atomic radius of aluminium is 143pm, and both are very approaching.In bone coal navajoite, vanadium is present in silico-aluminate with class matter homophase---in mica group, the kaolinite.Ammonium sulfate is heated to just to begin more than 100 ℃ to decompose emits ammonia, helps the reaction of ammonium sulfate and aluminium silicate mineral, generates exsiccated ammonium alum, and exsiccated ammonium alum can resolve into Tai-Ace S 150 and ammonia more than 280 ℃.Ammonium sulfate has SO when thermolysis
3Produce SO
3Be strong oxidizer, (300 ~ 500 ℃) are oxidized to 4 valencys with 3 valency vanadium at low temperatures, and when leaching with dilute sulphuric acid, 4 valency vanadium produce VOSO with the acid effect
4Get into solution, aluminium gets into solution with the Tai-Ace S 150 form.
The present invention reduces maturing temperature, energy-saving consumption-reducing greatly through this gordian technique of low-temperature bake bone coal navajoite fluidized-bed combustion lime-ash.
The present invention compares with prior art and has the following advantages and effect:
1. can reclaim vanadium and aluminium in the bone coal navajoite simultaneously, the leaching of vanadium and aluminium reaches respectively more than 88% and 91%, and the existing technology of the recovery of vanadium is high more than 10 percentage points;
2. low-temperature bake bone coal navajoite fluidized-bed combustion lime-ash reduces maturing temperature greatly, and save energy is easy to realize large industrialized production (available external-heating rotary kiln carries out);
3. the low temperature calcining only needs dilute sulphuric acid to leach, and has reduced vitriolic consumption, has suppressed the leaching of silicon, has reduced the desiliconization burden;
4. reclaim preparation Tai-Ace S 150 with waste water that extracts vanadium, aluminium and baking flue gas, reagent obtains recycle, realizes waste water, waste gas zero release, environmental friendliness.
In sum; The maturing temperature of the inventive method has only 300 ~ 500 ℃; More existing sodium, calcification, low sodium maturing temperature reduce half the approximately; Not only energy consumption obviously reduces, and in industrial production, realizes easily, has solved the big problem that extracting vanadium from stone coal maximization production line lacks suitable roasting apparatus.Present method is more easily extracted vanadium and aluminium with prior art from leach liquor, its leaching yield is respectively 88%, more than 91%, all be higher than existing method.Reclaim(ed) sulfuric acid ammonium from the waste water that extracts vanadium, aluminium returns batching again, and subsidiary material consumption is few, and processing charges is low, environmental friendliness.
Description of drawings
Accompanying drawing is a concrete process flow sheet of the present invention.
Embodiment:
Below in conjunction with embodiment, the present invention is further described, following examples are intended to explain the present invention, rather than to further qualification of the present invention.
Embodiment 1
Mining company's fluidized-bed combustion lime-ash contains V in the Hunan, Hunan
2O
51.25% Al
2O
38.23%, with this lime-ash and ammonium sulfate by mass ratio be the granularity of 1:1.1 combined grinding to 69% less than 0.043mm after, at 380 ℃ of following roasting 2h, at 80 ℃ down with the 3%H of 2 times of roasting material weight
2SO
4Solution leaches 3h, and the leaching yield of vanadium is 90.1%, and the leaching yield of aluminium reaches 93.1%.
Embodiment 2
With the fluidized-bed combustion lime-ash of instance 1 and ammonium sulfate by mass ratio be the granularity of 1:0.9 combined grinding to 90% less than 0.043mm after, at 500 ℃ of following roasting 1h, at 90 ℃ down with the 10%H of 2 times of roasting material weight
2SO
4Solution leaches 0.5h, and the leaching yield of vanadium is 88.9%, and the leaching yield of aluminium reaches 91.8%.
Embodiment 3
Guangxi vanadium industry company fluidized-bed combustion lime-ash contains Al
2O
318.2%V
2O
51.43%; With ashes and ammonium sulfate by mass ratio be 1:1.5 mix grinding to 60% granularity less than 0.043mm after, under 400 ℃, fuse 3h, 70 ℃ down with the 5% sulphuric acid solns leaching 0.5h of 1.8 times of roasting material weight; The leaching yield of vanadium reaches 88.7%, and the leaching yield of aluminium reaches 90.9%.
Embodiment 4
Tongcheng, Hubei mining company fluidized-bed combustion lime-ash contains Al
2O
36.93% V
2O
51.12%; Is that the granularity of 1:0.4 combined grinding to 72% is less than 0.043mm with this lime-ash and ammonium sulfate by mass ratio; The grinding material is fused 5h under 360 ℃, leach 1h with 2% dilute sulphuric acid of 2 times of roasting material weight down at 60 ℃, vanadium, aluminium leaching yield are respectively 87.9%, 90.3%.
Embodiment 5
The western Hunan, Hunan mining company fluidized-bed combustion lime-ash contains Al
2O
39.01%, V
2O
51.31%; Is that the granularity of 1:1.0 combined grinding to 80% is less than 0.043mm with this lime-ash and sulfuric acid acid ammonium by mass ratio; The grinding material is fused 3.0h under 420 ℃, 50 ℃ down with 4% dilute sulphuric acid agitation leach 1.5h of 1.5 times of roasting material weight, vanadium, aluminium leaching yield are respectively 90.3%, 92.1%.
Embodiment 6
Is that the granularity of 1:1.2 combined grinding to 90% is less than 0.043mm with the fluidized-bed combustion lime-ash of embodiment 5 and the ammonium sulfate that reclaims preparation by mass ratio; The grinding material is fused 1.0h under 500 ℃; 40 ℃ down with 10% dilute sulphuric acid agitation leach 2h of 1.2 times of roasting material weight, vanadium, aluminium leaching yield are respectively 91.1%, 92.8%.
Claims (9)
1. method of from bone coal navajoite fluidized-bed combustion lime-ash, extracting vanadium; It is characterized in that: with bone coal navajoite fluidized-bed combustion lime-ash and ammonium sulfate combined grinding; The powder that obtains is after 300 ℃ ~ 500 ℃ following roastings; In roasting material, add dilute sulphuric acid and leach, the leach liquor that contains vanadium, aluminium that obtains is liquid after obtaining vanadium extraction liquid and vanadium extraction behind the extraction separation vanadium; By in the liquid after the vanadium extraction behind the extraction separation aluminum compound, obtain carrying aluminium waste water, by carrying reclaim(ed) sulfuric acid ammonium in the aluminium waste water, the ammonium sulfate recycling of recovery.
2. method according to claim 1 is characterized in that: is that the mixed of 1:0.4 ~ 1.5 is carried out grinding with bone coal navajoite fluidized combustion lime-ash and ammonium sulfate by mass ratio, and the granularity of 60 ~ 90% mix grinding material is less than 0.043mm.
3. method according to claim 1 is characterized in that: the powder roasting time behind the described grinding is 1h ~ 5h.
4. method according to claim 1 is characterized in that: roasting material is added mass percent concentration≤10% dilute sulphuric acid agitation leach down at 40 ℃ ~ 80 ℃.
5. method according to claim 4 is characterized in that: the mass percent concentration of described dilute sulphuric acid is 4～10%.
6. method according to claim 4 is characterized in that: adopting the time of dilute sulphuric acid agitation leach is 0.5h ~ 3h, and the dilute sulphuric acid quality is 1 ~ 2 times of roasting material.
7. method according to claim 1 is characterized in that: the described leach liquor that contains vanadium, aluminium is ion exchange method or solvent extration extraction by routine through the extraction separation vanadium.
8. according to claim 1 or 6 described methods, it is characterized in that: said aluminum compound is tschermigite, white lake or aluminum oxide.
9. according to claim 1 or 6 described methods, it is characterized in that: produce flue gas in the said roasting process and then join in the step of extraction separation aluminum compound.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107983764A (en) * | 2017-12-19 | 2018-05-04 | 湖南华麒资源环境科技发展有限公司 | A kind of method that chromium-polluted soil repairs upgrading |
| CN112011692A (en) * | 2020-09-23 | 2020-12-01 | 攀钢集团研究院有限公司 | Method for extracting vanadium by composite roasting of solid waste slag |
| CN112080651A (en) * | 2020-09-23 | 2020-12-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN115505759A (en) * | 2022-09-07 | 2022-12-23 | 北京华能长江环保科技研究院有限公司 | Fluidized bed system for comprehensive utilization of stone coal for extracting selenium and vanadium and comprehensive utilization method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983764A (en) * | 2017-12-19 | 2018-05-04 | 湖南华麒资源环境科技发展有限公司 | A kind of method that chromium-polluted soil repairs upgrading |
| CN112011692A (en) * | 2020-09-23 | 2020-12-01 | 攀钢集团研究院有限公司 | Method for extracting vanadium by composite roasting of solid waste slag |
| CN112080651A (en) * | 2020-09-23 | 2020-12-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN112080651B (en) * | 2020-09-23 | 2022-07-19 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN115505759A (en) * | 2022-09-07 | 2022-12-23 | 北京华能长江环保科技研究院有限公司 | Fluidized bed system for comprehensive utilization of stone coal for extracting selenium and vanadium and comprehensive utilization method |
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