CN101323914A - Process for extracting vanadic anhydride by high calcium calcination - Google Patents
Process for extracting vanadic anhydride by high calcium calcination Download PDFInfo
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- CN101323914A CN101323914A CNA2008100456714A CN200810045671A CN101323914A CN 101323914 A CN101323914 A CN 101323914A CN A2008100456714 A CNA2008100456714 A CN A2008100456714A CN 200810045671 A CN200810045671 A CN 200810045671A CN 101323914 A CN101323914 A CN 101323914A
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Abstract
The invention relates to a process for extracting vanadium pentoxide by high calcium roasting. The process is characterized by comprising the following process steps: calcium roasting, dilute acid leaching, the purification treatment of leached liquid, extraction-counter extraction, vanadium leaching and calcining and deaminizing and is also characterized in that calcium roasting relates to high calcium roasting: roscoelite with the existence of vanadium and carbonaceous shale ores that contain vanadium and are difficult to dissolve in aluminosilicate or decarburized coal cinder of electricity plants are taken as raw materials that are added with 13 to 15 percent of bluestone and 1 to 3 percent of fluorite which are calculated by the weight percentage of the raw materials, roasted in a furnace at a roasting temperature of 800 to 900 DEG C after undergoing mixing, grinding and pelletizing. The process overcomes the problems that the current sodium roasting produces chlorine and pollutes the environment, eliminates the defects that method of high-concentration acid lixivium pollutes the environment and has large sulphuric acid consumption and high production cost, and has the advantages of high total vanadium yield, relatively low production cost, nearly no available of waste water and residues, etc.
Description
Technical field
The present invention relates to the production method of Vanadium Pentoxide in FLAKES, particularly from contain vanadium yeath ore deposit and power plant's decarburization cinder, extract the industrial process of Vanadium Pentoxide in FLAKES.
Background technology
Vanadium is a rare precious metal, has many premium propertiess.In industries such as metallurgy, chemical industry purposes is widely arranged.
The navajoite resource mainly contain with the symbiotic vanadium titano-magnetite of iron ore and with the symbiotic bone coal navajoite of carbon.China stone coal vanadium-containing ore deposit 90% is to contain navajoite cubic meter of stone formula with illite, kaolinite, roscoelite etc. to exist.
The existing operational path that extracts Vanadium Pentoxide in FLAKES from bone coal navajoite mainly contains following mode:
1, peracid high temperature leaching method
Behind the bone coal navajoite ball milling, in temperature more than 90 ℃, directly with 15～25% sulfuric acid to leach, leaching liquid is transferred alkali through ammoniacal liquor, use solvent extraction, dilute sulphuric acid is stripped, and strips and transfers alkali pH value to 2 with ammoniacal liquor, and the precipitation of heating obtains ammonium poly-vanadate product (ammonium poly-vanadate can obtain Vanadium Pentoxide in FLAKES through calcining directly).There is Shaanxi Province adret vanadium industry company in manufacturing enterprise.This technical process complexity, the sulfuric acid consumption is big, energy consumption is big, extraction yield is low, it is inapplicable that illite, kaolinite, roscoelite etc. are contained navajoite stone.
2, sodium roasting method
Be composite additive and bone coal navajoite balling-up, go into the kiln roasting with sodium-chlor and yellow soda ash.Calcining is gone into pond water normal temperature leaching, and leaching liquid is resolved with saturated nacl aqueous solution through resin absorption, and stripping liquid adds the ammonium chloride precipitation and obtains the ammonium meta-vanadate product.Beautiful allusion quotation smelting nine weighs the production technique of vanadium industry company as Henan Zhe Chuanxian.This method vanadium recovery is low, cost is higher, waste water can not recycle contaminate environment.
3, blank roasting method
Chinese patent literature CN101182596A, CN101012496A, CN101054635A, CN1978326A disclose to contain the blank roasting method that the scherbinaite coal is a raw material.This method exists transformation efficiency not high equally, sulfur dioxide pollution and contain the handling problem of ammonia, nitrogen waste water.
Wherein CN101054635A and CN1978326A are to be raw material to contain the scherbinaite coal, by roasting, dilute sulfuric acid, extracting-back extraction get, processing step such as precipitation, calcining deamination, make the Vanadium Pentoxide in FLAKES product.
4, calcification baking method
The calcification baking method is the more common method of industrial use.Chinese patent literature CN101066778A, CN1899971A, CN1724387A, CN17052022A, CN1184162A have disclosed to contain the calcification baking method that the scherbinaite coal is a raw material, and corresponding adding calcium oxide, white lime or calcium salt etc. carry out calcification baking in calcining process.
Wherein, the typical process of CN101066778A is: to contain the scherbinaite coal is raw material, through calcification baking, acidleach, from industry and traffic change, precipitation, calcining deamination five big operations make the Vanadium Pentoxide in FLAKES product.
Contained vanadium yeath mineral structure complexity because our company has, and analyzed through scientific research institutions, vanadium is mainly composed and is stored in roscoelite and the indissoluble silico-aluminate; Simultaneously, our company extracts the coal ash that the Vanadium Pentoxide in FLAKES raw material also has the fuel-burning power plant (is coal ash behind raw material, the burning de-carbon to contain the scherbinaite coal).And existing this class raw material of process for extracting vanadium intractable, all exist the extraction yield of vanadium low, even put forward to come out the problem of (as the sodium roasting method) at all, simultaneously, produce chlorine and hydrogen chloride gas (as sodium roasting time add sodium-chlor) during existing process for extracting vanadium roasting and cause environmental pollution; Adopt high density acidleach (being peracid high temperature leaching liquid) to exist industrial sulphuric acid consumption big, the disadvantage that production cost is high.In general, above-mentioned existing technology all exists waste water to be difficult to recycle, the common fault of waste water, waste sludge discharge contaminate environment.
Summary of the invention
The purpose of this invention is to provide and a kind ofly contain vanadium yeath mineral or power plant to contain the vanadium coal ash be raw material, adopt the high calcium calcination mode to produce the technology of the extracting vanadic anhydride by high calcium calcination of Vanadium Pentoxide in FLAKES with specific.
The object of the present invention is achieved like this: a kind of technology of extracting vanadic anhydride by high calcium calcination, it is characterized in that: comprise following processing step: calcification baking, dilute sulfuric acid, purification of leaching liquor is handled, extracting-back extraction is got, precipitation and calcining deamination, it is characterized in that: described calcification baking is a high calcium calcination: with vanadium compose be stored in roscoelite and indissoluble silico-aluminate contain vanadium yeath ore deposit or power plant's decarburization cinder is a raw material, interpolation is in the green stone of raw material weight 13～15% and 1～3% fluorite, through mixing, pulverize, after the granulation, go into the stove roasting, 800～900 ℃ of maturing temperatures.
The invention has the beneficial effects as follows:
1, extracts the Vanadium Pentoxide in FLAKES traditional technology from yeath and generally adopt sodium roasting, so-called sodium roasting technology refers to that mineral mix the back high-temperature roasting with sodium-chlor, make vanadium and sodium be combined into vanadic acid sodium and water-soluble, produce chlorine and hydrogen chloride gas when this technology shortcoming is roasting and contaminate environment is serious.There is part producer to adopt high density acid leaching extraction Vanadium Pentoxide in FLAKES in the recent period, the high concentrated acid soaking technology refers to that mineral are without roasting but through the direct sulfuric acid to leach with high density in levigate back, this processes expend sulfuric acid is big, waste water is difficult to recycle, the production cost height, and most of factory and office are in end-of-life state.These processing methodes are adapted to handled thing and simply contain vanadium yeath (vanadium mainly is present in the clay mineral) mutually, contained vanadium yeath mineral facies complex structure and my company has, analyzing vanadium through scientific research institutions mainly composes and is stored in roscoelite and the indissoluble silico-aluminate, carry to come out with the vanadium extraction of above-mentioned traditional technology method, and my processing method of company's original creation just is adapted to this unmanageable mineral at all.
2, the process for extracting vanadium of my company is the high calcium calcination extraction vanadium extraction technology, the reaction mechanism of this technology is: most of vanadium is mainly composed with trivalent V-arrangement formula and is stored in roscoelite and the aluminosilicate structure in the bone coal, this roscoelite and aluminosilicate structure are comparatively stable, be difficult to by water, acid or alkali dissolution, green stone that is added during roasting and fluorite can destroy the structure of this vanadium, vanadium is discharged, trivalent V is oxidized to pentavalent V, generate the vanadic acid calcium that dissolves in dilute sulphuric acid with the calcium reaction then, vanadium exists with the pentavalent vanadium in solution, can be extracted by the tertiary amine extraction agent, the vanadium that is extracted the agent extraction is arrived aqueous phase by solvent stripping again, at this moment the vanadium of the aqueous phase purification that obtained height with concentrate, Vanadium Pentoxide in FLAKES concentration reaches 150g/l can be used for precipitating into ammonium meta-vanadate, ammonium meta-vanadate is through calcination, piece of Vanadium is cast in fusing.Relevant reaction formula is as follows:
V
2O
3+0.5O
2→V
2O
4
V
2O
4+0.5O
2→V
2O
5
V
2O
5+CaO→Ca(VO
3)
2
V
2O
5+2H
+→2VO
2 ++H
2O
Ca(VO
3)
2+2H
+→2VO
2 ++H
2O+Ca
2+
2NH
4VO
3→V
2O
5+2NH
3↑
3, my company's post processing adopts advanced extraction vanadium extraction technology, selects for use tertiary amine-type N235 to make extraction agent, has percentage extraction height (percentage extraction and stripping rate all can reach more than 99%), good separating effect, and the Vanadium Pentoxide in FLAKES purity of extraction can reach more than 99%.
4, general traditional technology trade effluent discharges, and our technology trade effluent, part waste residue can recycle.The reuse of waste water, waste residue embodiment part is in the back further described and is illustrated.
The relevant yield of this processing method is as follows:
Roasting transformation efficiency 75%; Leaching yield 95%; Percentage extraction 99%; Precipitation rate 98%; Total yield 68%.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Accompanying drawing illustrates, and technical process of the present invention is as follows:
A), high calcium calcination
To contain vanadium yeath ore deposit (vanadium is composed and is stored in roscoelite and the indissoluble silico-aluminate) or power plant's decarburization cinder is raw material, with green stone and fluorite (is the fluorine ore deposit, main component CaF2, proportion 3.18, hardness 4, isometric system) be additive, the addition of green stone and fluorite is respectively in 13～15% and 1～3% of raw material weight.
Raw material and green stone, fluorite are broken to fineness 120 orders 〉=80% through powder mix, granulating, (particle diameter is 8～12mm again, right fed to boiler roasting (is fuel with coal gas), 850～1100 ℃ of maturing temperatures, roasting time 60 minutes～90 minutes, the optimum addition of above-mentioned additive is: the addition of green stone is 14%, and the addition of fluorite is 2%.
The main component of green stone is a lime carbonate, and lime carbonate is decomposed into calcium oxide when high-temperature roasting, and calcium oxide is very active when high temperature, can replace vanadium and enter mica and silico-aluminate thing mutually in, vanadium is discharged generates vanadic acid calcium.Fluorite mainly rises and reduces thing phase fusing point and katalysis.
B), rarely get leaching
Roasting material carries out wet ball mill earlier, and with the dilute sulphuric acid leaching, leaching concentration is pH value 2.5 then; Add soda ash in the leach liquor after the solid-liquid separation and carry out purifying treatment;
C), extracting-back extraction is got
Scavenging solution after the b step handles is after solid-liquid separation, add extraction agent tertiary amine-type N235 (N235 in its liquid phase, Chinese is trioctylamine, commercial product code 7301, be a kind of of tertiary amines, be mainly used in the extraction of noble metal) under certain PH, extract, add strippant (sodium carbonate solution) again and strip, the liquid phase of strip liquor after purifying solid-liquid separation is deposition vanadium mother liquid;
D), precipitation
In deposition vanadium mother liquid, add ammonium chloride, obtain precipitating ammonium meta-vanadate;
E), calcining deamination
To precipitate the ammonium meta-vanadate calcining, remove the ammonia in the molecule, make the Vanadium Pentoxide in FLAKES product.
Raffinate water behind the dilute sulfuric acid after the washing lotion of solid-liquid separation, the extraction all is back in the wet ball mill step, participates in wet ball mill; The residue of solid-liquid separation all returned and participates in roasting in the stove after the residue of solid-liquid separation and strip liquor purified behind the purification of leaching liquor; The upper strata liquid and the wash water of solid-liquid separation turns back to granulation after the precipitation.
Be used in the wet ball mill operation before washing lotion in the technological process, raffinate water etc. all return, some returns roasting once more in the calcining process residue in the technological process, and the residue of dishing out is a good raw material (containing aluminium, silicon height in the residue) of doing lagging material.On the one hand, do not have wastewater disposition in the whole production substantially, alleviated pollution, on the other hand, improved the total recovery of vanadium environment.
This technology is used, and to contain the culmiferous analyzing test data of vanadium as follows:
1, primary sample vanadium material phase analysis:
| Vanadium thing phase | Ferric oxide and clay | Mica mineral | The indissoluble silico-aluminate | Total vanadium |
| Occupation rate (%) | 0.064 | 0.549 | 0.387 | 1.00 |
| Partition ratio (%) | 6.40 | 54.90 | 38.70 | 100 |
2, primary sample vanadium occurrence status is analyzed:
| Vanadium thing phase | V3+ | V4+ | V5+ | Total vanadium |
| Occupation rate (%) | 0.292 | 0.105 | 0.163 | 0.560 |
| Partition ratio (%) | 52.14 | 18.75 | 29.11 | 100 |
Can draw as drawing a conclusion by above test data:
1, the vanadium of half in the raw ore is composed to be stored in the mica mineral with adsorbed state and (is contained vanadium partition ratio 54.90%);
2, replace Fe3+ with class matter in-phase version on a small quantity and enter oxide minerals (containing vanadium partition ratio 6.40%) such as ferric oxide and clay pit;
3, replace Al3+ with class matter in-phase version greatly and enter indissoluble silicoaluminate salt face (containing vanadium partition ratio 38.70%);
4, mainly there be (partition ratio is 52.14%) in vanadium with the V3+ form in raw ore;
5, secondly be V5+ (partition ratio is 29.11%);
6, secondly be V4+ (partition ratio is 18.75%) again
Claims (5)
1, a kind of technology of extracting vanadic anhydride by high calcium calcination, it is characterized in that: comprise following processing step: calcification baking, dilute sulfuric acid, purification of leaching liquor are handled, extracting-back extraction is got, precipitation and calcining deamination, it is characterized in that: described calcification baking is a high calcium calcination: with vanadium compose be stored in roscoelite and indissoluble silico-aluminate contain vanadium yeath ore deposit or power plant's decarburization cinder is a raw material, interpolation is in the Wingdale of raw material weight 13～15% and 1～3% fluorite, after mixing, pulverize, granulating, go into the stove roasting, 850～1000 ℃ of maturing temperatures.
2, according to the technology of the described extracting vanadic anhydride by high calcium calcination of claim 1, it is characterized in that: in the described high calcium calcination step, the addition of Wingdale is 14%, and the addition of fluorite is 2%.
3, according to the technology of the described extracting vanadic anhydride by high calcium calcination of claim 2, it is characterized in that: the extraction agent of described extraction step is tertiary amine-type N235.
4, according to the technology of the described extracting vanadic anhydride by high calcium calcination of claim 3, it is characterized in that: it is 120 orders 〉=80% that described raw material mixes the granularity of pulverizing the back; It is 8～12% that granulation requires diameter; Carry out wet ball mill processing after the raw material roasting again, adopt dilute sulphuric acid to leach then, leaching acidity PH2.5; Add soda ash in the leach liquor and carry out purifying treatment.
5, according to the technology of the described extracting vanadic anhydride by high calcium calcination of claim 4, it is characterized in that: the washing lotion of solid-liquid separation behind the described dilute sulfuric acid, the raffinate water after the extraction all is back in the wet ball mill step, participates in wet ball mill; Behind the purification of leaching liquor behind the residue of solid-liquid separation and the strip liquor residue of solid-liquid separation all return and participate in roasting in the stove; The upper strata liquid and the wash water of solid-liquid separation turns back to granulation after the precipitation.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519723B (en) * | 2009-02-17 | 2012-05-09 | 贵州省地质矿产中心实验室 | Clean production process for extracting vanadium from vanadium-containing carbonaceous shale by hot-pressing oxidation method |
| CN102560155A (en) * | 2012-02-22 | 2012-07-11 | 广西冶金研究院 | Method for extracting vanadium from stone coal vanadium ore by using calcium compound additive |
| CN103194611A (en) * | 2013-04-01 | 2013-07-10 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing vanadium oxide |
| CN103667710A (en) * | 2013-12-04 | 2014-03-26 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
| CN104018011A (en) * | 2014-06-23 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of vanadic oxide |
| 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 |
| CN104711430A (en) * | 2015-03-23 | 2015-06-17 | 紫阳县广润煤炭实业有限公司 | Production method for preparing vanadium product by taking stone coal as raw material |
| CN104988337A (en) * | 2015-06-09 | 2015-10-21 | 陕西五洲矿业股份有限公司 | Stone coal vanadium ore leaching process for recycling residual acid |
| CN105110373A (en) * | 2015-09-23 | 2015-12-02 | 攀钢集团西昌钢钒有限公司 | Vanadium oxide cleaner production method and recovery method of acid leaching slags in vanadium oxide cleaner production |
| CN105776333A (en) * | 2016-02-05 | 2016-07-20 | 河北钢铁股份有限公司承德分公司 | Preparation method of vanadium pentoxide |
| CN114644357A (en) * | 2022-03-11 | 2022-06-21 | 万循材料科技有限公司 | Method for preparing ammonium metavanadate by sodium modification vanadium extraction combined alkali preparation and low-cost vanadium slag utilization |
| CN115247234A (en) * | 2020-10-17 | 2022-10-28 | 刘辉 | Method for preparing ammonium metavanadate by direct sulfuric acid oxidation and acidolysis of vanadium slag |
-
2008
- 2008-07-29 CN CNA2008100456714A patent/CN101323914A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519723B (en) * | 2009-02-17 | 2012-05-09 | 贵州省地质矿产中心实验室 | Clean production process for extracting vanadium from vanadium-containing carbonaceous shale by hot-pressing oxidation method |
| CN102560155A (en) * | 2012-02-22 | 2012-07-11 | 广西冶金研究院 | Method for extracting vanadium from stone coal vanadium ore by using calcium compound additive |
| CN103194611A (en) * | 2013-04-01 | 2013-07-10 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing vanadium oxide |
| CN103667710A (en) * | 2013-12-04 | 2014-03-26 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
| CN103667710B (en) * | 2013-12-04 | 2015-06-17 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
| CN104018011B (en) * | 2014-06-23 | 2015-05-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of vanadic oxide |
| CN104018011A (en) * | 2014-06-23 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of vanadic oxide |
| 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 |
| CN104711430A (en) * | 2015-03-23 | 2015-06-17 | 紫阳县广润煤炭实业有限公司 | Production method for preparing vanadium product by taking stone coal as raw material |
| CN104988337A (en) * | 2015-06-09 | 2015-10-21 | 陕西五洲矿业股份有限公司 | Stone coal vanadium ore leaching process for recycling residual acid |
| CN105110373A (en) * | 2015-09-23 | 2015-12-02 | 攀钢集团西昌钢钒有限公司 | Vanadium oxide cleaner production method and recovery method of acid leaching slags in vanadium oxide cleaner production |
| CN105776333A (en) * | 2016-02-05 | 2016-07-20 | 河北钢铁股份有限公司承德分公司 | Preparation method of vanadium pentoxide |
| CN115247234A (en) * | 2020-10-17 | 2022-10-28 | 刘辉 | Method for preparing ammonium metavanadate by direct sulfuric acid oxidation and acidolysis of vanadium slag |
| CN114644357A (en) * | 2022-03-11 | 2022-06-21 | 万循材料科技有限公司 | Method for preparing ammonium metavanadate by sodium modification vanadium extraction combined alkali preparation and low-cost vanadium slag utilization |
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