CN103614564A - Method for continuously smelting vanadium-containing ferrophosphorous - Google Patents
Method for continuously smelting vanadium-containing ferrophosphorous Download PDFInfo
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- CN103614564A CN103614564A CN201310539239.1A CN201310539239A CN103614564A CN 103614564 A CN103614564 A CN 103614564A CN 201310539239 A CN201310539239 A CN 201310539239A CN 103614564 A CN103614564 A CN 103614564A
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Abstract
The invention discloses a method for continuously smelting vanadium-containing ferrophosphorous, which comprises the following steps: heating the vanadium-containing ferrophosphorous to a red and hot state through an electric furnace or blowing by gas ignition, blowing oxygen to high temperature vanadium-containing ferrophosphorous in a heating electric furnace or a blowing furnace, melting and smelting the vanadium-containing ferrophosphorous by using reaction heat; adding calcium oxide or soda ash, blowing oxygen, smelting and generating slag, respectively requiring high-grade vanadium slag and high phosphorus nickel molten iron; removing vanadium slag and extracting vanadium; casting a part of high phosphorus nickel molten iron on an iron ingot, mixing the part of high phosphorus nickel molten iron and the vanadium-containing ferrophosphorous at a normal temperature state continuously supplemented in the furnace, repeatedly supplementing the material, discontinuously dumping the high phosphorus nickel molten iron for casting to obtain a high phosphor ferronickel ingot. The method completely solves the defect of high energy consumption in a pyrometallurgucal process, ensures the comprehensive recovery of elements such as iron, nickel and phosphor, greatly shortens the smelting period, and increases the recovery and utilization rate of vanadium and phosphor. The final recovery rate of vanadium can reach 70-95%, and the recovery rate of iron, phosphor and nickel can reach more than 60%.
Description
Technical field
The present invention relates to metallurgy and chemical technology field, particularly relate to a kind of method of continuous smelting vanadophosphoric ferric.
Background technology
The purposes of the oxide compound of vanadium metal and vanadium is very extensive, is a kind of important alloying element in metallurgy industry.China's navajoite total resources is larger, but navajoite grade is lower, and prior art all cannot be extracted for domestic quite a few low-grade navajoite.And along with the developing rapidly of China's economy, for the demand of vanadium, be increasing.Along with external vanadophosphoric ferric enters China in a large number, domestic still short to vanadophosphoric ferric search time, also have that the vanadium metal rate of recovery is low, resource is by the comprehensive problem such as recovery.
For solving above-mentioned existing problem, Chinese patent CN101550492A discloses " from vanadophosphoric ferric, extracting the method for Vanadium Pentoxide in FLAKES ", specific as follows: (1) is levigate by being mixed into ball mill after vanadophosphoric ferric and lime fragmentation, ball milling material is granulated in roasting after adding soda ash, roasting material adds water and enters wet-type ball mill wet ball mill, ball milling ore pulp leaches by mechanical stirring, leach slurry filtration, containing vanadium solution, send after the cooling clarification of storage tank, send anionite-exchange resin absorption vanadium, the vanadium of absorption obtains high-grade Vanadium Pentoxide in FLAKES product through wash-out, precipitated crystal, pyrolysis.(2) according to the 15-35% that amount of lime is vanadophosphoric ferric weight that allocates into described in 1, allocate the 30-50% that soda ash weight is vanadium ferrophosphorus weight into.(3) according to roasting material described in 1,2, need first granulate, spherolite diameter control is in the scope of 3-15mm, and 900 ℃ of Wen Du≤750 ℃, ﹤ are burnt in roasting, roasting time ﹥ 2 hours ,≤5 hours.Roasting described in (4) 1 or 2 is discharged heat material and is directly slipped into tank, is mixed into wet-type ball mill pulp ball milling (mechanical milling process reality is also leaching process), and material: water=1:1.5-5 utilizes heat material that water temperature is raised to 50-95 ℃, does not need external heat.(5) ball milling ore pulp send mechanical agitating tank, temperature 35-39 ℃, and extraction time is 0.5-1.5 hour, in the time of leaching process, can in groove, blast partial roasting flue gas, the CO in flue gas
2more favourable to the leaching of vanadium with heat.Although this Technology has been carried out effective recovery to vanadium, owing to there is a large amount of iron in production process Raw, improved the difficulty of producing.And the elements such as iron, nickel are not carried out to comprehensive recovery.
It is specific as follows that Chinese patent CN1970803A discloses " utilizing the technique of extracting vanadium from vanadium-containing ferrophosphor smelting ferrovanadium ": (1) is first that 1.5 times amounts put in electric furnace with sodium carbonate in containing vanadium ratio by vanadophosphoric ferric (containing V5%), be heated to 2000 ℃, melting was poured in hot metal ladle after 2 hours, when temperature drops to 1400 ℃, in melt, be blown into oxygen-rich air, skim the scum silica frost containing vanadium phosphorus; (2) the molten iron ingot casting of melting in hot metal ladle is cooled to finished product ingot iron; (3) step 1 is skimmed containing the scum silica frost of vanadium phosphorus through cooling, be broken into powder (fineness reaches 100 orders), with addition of sodium salt powder pelletizing group, roasting 2 hours; Roasting process temperature is controlled at 900 ℃; (4) by water logging ball, solvend in pelletizing is dissolved in water and obtains vanadic acid sodium and sodium phosphate mixing solutions, in this solution, add CaO, go through 24 hours precipitations, through press filtration, phosphorus slag filter cake is again through light industry slaking, and smelted furnace cinder proportioning is mixed and made into phosphate fertilizer; (5) in the filtrate producing in step 4, add sulfuric acid, obtain Vanadium Pentoxide in FLAKES solid sediment; Through press filtration, be melt into sheet vanadium, then deliver to electrosmelting and be produced into vanadium iron finished product.
First this Technology is oxidized de-iron in conjunction with traditional smelting iron ore technology and makes vanadium slag, has realized preliminary slag iron separated, is conducive to vanadium extraction in subsequent technique, and the impact that reduces iron improves the rate of recovery of vanadium, has realized to a certain extent comprehensive utilization.But smelting cycle is long during due to employing electrosmelting, cause current consumption larger, production cost increases, and also can cause the problems such as environmental pollution.
Summary of the invention
The object of the invention is for solving existing problem in existing technique, propose a kind of continuous low-energy consumption and smelt the method for vanadophosphoric ferric production higher-grade vanadium slag and high-phosphorus ferronickel byproduct, fundamentally solved the high defect of pyrometallurgical smelting energy consumption, both guaranteed the comprehensive recovery of the elements such as iron nickel, greatly shorten again smelting cycle, improved the recovery utilization rate of vanadium, phosphorus.
The object of the invention is to realize by following technical proposals.
A continuous smelting vanadophosphoric ferric method, the method comprises the steps:
Step 1 heats vanadophosphoric ferric in electric furnace or the winding-up of some coal gas is heated to red heat state or molten state;
Step 2 is poured in converting furnace and is carried out oxygen blast in process furnace or by the vanadophosphoric ferric of high temperature, utilizes chemical reaction heat to flux and burns the vanadophosphoric ferric of red heat state or molten state;
Step 3, after treating that vanadophosphoric ferric melts completely, adds basic cpd according to mass ratio when temperature is higher, continues oxygen blast smelting 10-50min and slags tap, and obtains respectively vanadium slag and high-phosphorus ferronickel water that vanadiumcontent is higher;
Step 4, vanadium slag skims, and utilizes the method for traditional sodium roasting to carry out vanadium extraction to vanadium slag; Pouring out 30-60% high-phosphorus ferronickel water waters and casts iron ingot;
Step 5, residue high-phosphorus ferronickel water mixes with the 40-150% normal-temperature vanadophosphoric ferric that continues to fill into the interior melt quality of (can add) stove in batches, and repeating step two is to step 4; Discontinuity is poured out molten iron casting and is obtained high-phosphorus ferronickel ingot, realizes and smelts continuously vanadophosphoric ferric.The ult rec of vanadium can reach 70-95%, and the rate of recovery of iron, phosphorus and nickel can reach more than 60%.
The method further comprises:
In described step 2, oxygen blast in process furnace, produces gaseous state P in the part vanadium in iron liquid and phosphorus oxidation process
2o
5and V
2o
5flue gas is recovered to fume recovery system; Recovery system absorbs flue gas through alkaline solution hydration, obtain phosphorous and aqueous solution vanadium, the aqueous solution of phosphorous and vanadium through extract separated after, finally obtain vanadium and phosphorus product.
Described alkaline solution is sodium hydroxide or aqua calcis.
The basic cpd that the described acidic oxide that interpolation is used for and oxygen blast produces in process furnace is made vanadium slag is calcium oxide, sodium carbonate or calcium carbonate.
The described basic cpd addition that adds is vanadophosphoric ferric: basic cpd=10:0.9-10:1.3 according to mass ratio.
Described be heated to red heat state be by vanadophosphoric ferric in electric furnace or some coal gas winding-up be heated to 800-1500 ℃.
Described vanadophosphoric ferric is poured in converting furnace and is carried out oxygen blast for blowing pure oxygen, oxygen-rich air or air.
Described temperature adds calcium oxide, calcium carbonate or soda ash when higher, continue oxygen blast and guarantee that homo(io)thermism is within the scope of 1100-1500 ℃.
Advantage of the present invention is: in whole smelting process, energy consumption is few, under the prerequisite of less energy-consumption, realized the first element such as Separation and Recovery iron nickel, got rid of the interference of follow-up process for extracting vanadium, be conducive to improve the rate of recovery of vanadium, and processed well the problems such as the vanadium phosphor resource waste that pyrometallurgical smelting is taken away by flue gas, contaminate environment, with respect to existing technique, there is novelty and break through.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing and principle, the present invention is described in further detail.
Shown in Figure 1, the present invention smelts vanadophosphoric ferric method continuously, comprises the steps:
1) adopt heating by electric cooker or some coal gas winding-up flame to make vanadophosphoric ferric be warming up to 800-1500 degree Celsius, be heated to red heat state or molten state;
2) in electric furnace or pour out in blowing equipment and to make it to occur oxidizing reaction and produce reaction heat and flux burning carry out oxygen blast gas, oxygen-rich air or the air of the vanadophosphoric ferric material of red heat state or molten state;
3) treat that vanadophosphoric ferric melts completely, owing to advertising the larger time reaction of amount of oxygen or Rich Oxygen Amount comparatively violent, emit a large amount of heat and may cause in stove temperature higher, therefore can advertise a certain amount of air, reduce temperature; Oxygen blast gas or oxygen-rich air when temperature is lower, when temperature is higher according to quality than vanadophosphoric ferric: basic cpd=10:0.9-10:1.3 ratio adds basic cpd calcium oxide, sodium carbonate or calcium carbonate, 10-50min is smelted in oxygen blast, guarantee that homo(io)thermism is within certain smelting scope, while preventing extremes of temperature, the working of a furnace is unstable, affect metallurgical effect, be conducive to carrying out smoothly of selective oxidation vanadium extraction;
4) when the quantity of slag is larger, pour out vanadium slag, obtain respectively higher-grade vanadium slag and high-phosphorus ferronickel water; And can reduce the erosion of slag blanket to refractory materials, the oxidation that also helps vanadium is proceeded;
Skim respectively vanadium slag, utilize the method for traditional sodium roasting vanadium slag to be carried out to vanadium extraction and pour out 30-60% high-phosphorus ferronickel water being cast into high-phosphorus ferronickel ingot, realize slag iron separated;
5) after converting furnace slag iron, the 40-150% normal-temperature vanadophosphoric ferric that add stove in melt quality suitable according to furnace temperature, then continues oxygen blast and fluxes, constantly repeating step 2)-4) realize smelting continuously and produce high-phosphorus ferronickel and higher-grade vanadium slag.Whole step 2)-4) in continuous flow procedure, do not expend other energy, rely on reaction heat completely, self-sufficient realization is smelted.
In above-mentioned oxygen blast or air event, because the content of phosphorus and vanadium is higher, in the part vanadium in iron liquid and phosphorus oxidation process, can produce gaseous state P
2o
5and V
2o
5along with flue gas is taken out of in a large number.Utilize fume recovery system that flue gas is absorbed through solution hydrations such as sodium solution or sodium hydroxide and calcium hydroxides, obtain phosphorous and aqueous solution vanadium, the aqueous solution phosphorous and vanadium finally obtains vanadium and phosphorus product through extracting after separating.
Below by specific embodiment, the present invention is described in further details.
Embodiment 1
The vanadophosphoric ferric major ingredient of smelting is specific as follows: P22.6%, V9%, Ni1%, Fe61%, Gr4%, in process furnace, add the winding-up of 100kg vanadophosphoric ferric point coal gas and carry out heat temperature raising, temperature stops coal gas while rising to 800 ℃, in process furnace, pour out, in blowing equipment, carry out oxygen blast gas and flux and make it to melt completely.Until melt completely, when temperature is higher in stove, can the sodium carbonate of 9kg be divided 3 times and add in smelting furnace, with air, replace oxygen to be blown in stove, continue oxidizing reaction and control temperature to be unlikely to too high; Can oxygen blast gas when temperature is lower or oxygen-rich air suitably heat up, make smelting temperature constant within the scope of 1100-1500 ℃.Whole air blowing process is about 50 minutes and is blown into oxygen and is about 11m
3(being blown into air capacity converts by oxygen).
In smelting process, in blowing, in the time of 25 minutes, skim vanadium slag once, after blowing 50 minutes, skim whole vanadium slags, finally emit the molten iron of stove interior 30% and make high-phosphorus ferronickel ingot.Then (according to furnace temperature, can divide 2 batches) and add 40% normal-temperature vanadophosphoric ferric of melt quality in stove, in stove, remaining high-phosphorus ferronickel heat transfer water is to vanadophosphoric ferric, and then oxygen blast is fluxed-smelted, constantly repeats to realize continuous smelting production high-phosphorus ferronickel and higher-grade vanadium slag.During follow-up continuous production, rely on reaction heat completely, self-sufficient realization is smelted continuously.
In above-mentioned oxygen blast or air event due to molten iron in the content of phosphorus and vanadium higher, in the part vanadium in iron liquid and phosphorus oxidation process, can produce gaseous state P
2o
5and V
2o
5along with flue gas is taken out of in a large number.Utilize fume recovery system to collect flue gas.Flue gas is recovered through solution hydrations such as sodium hydroxide and calcium hydroxides and absorbs, and obtains phosphorous and aqueous solution vanadium, extracts after separating and finally obtains vanadium and phosphorus product.
Embodiment 2
The vanadophosphoric ferric major ingredient of smelting is specific as follows: P30%, V4.5%, Ni1%, Fe59%, Gr3.6%.Heating by electric cooker 100kg vanadophosphoric ferric stops energising while being warming up to 1500 ℃, pour out the vanadophosphoric ferric material of molten state in smelting furnace, is blown into oxygen-rich air or air 10min smelts in blowing equipment, is blown into air capacity according to oxygen blast tolerance 0.1m
3/ kg conversion can add sodium carbonate 13kg when temperature is higher in converting furnace, advertises a certain amount of air and reduces temperature; When temperature is lower, oxygen blast gas or oxygen-rich air guarantee that homo(io)thermism is within 1100-1500 ℃ of scope, and while preventing extremes of temperature, the working of a furnace is unstable, affects metallurgical effect.
Oxygen blast skims whole vanadium slags after smelting and finishing, and then pours out 60% molten iron casting high-phosphorus ferronickel ingot.Afterwards according to furnace temperature height, suitable add in stove in batches 150% normal-temperature vanadophosphoric ferric of melt quality continue oxygen blast Zhu Rong ?smelt (reinforced principle: the one, can not feed in raw material too quickly, so that cause the too low impact blowing of furnace temperature; The 2nd, guarantee suitable heat size ratio, while avoiding blowing, there is the excessive slag of splash).Constantly repeat, realize smelting continuously and produce high-phosphorus ferronickel and higher-grade vanadium slag.In whole continuous flow procedure, consumed energy is less, relies on reaction heat during follow-up continuous production completely, and self-sufficient realization is smelted.
In above-mentioned oxygen blast or air event due to molten iron in the content of phosphorus and vanadium higher, in the part vanadium in iron liquid and phosphorus oxidation process, can produce gaseous state P
2o
5and V
2o
5along with flue gas is taken out of in a large number.Utilize fume recovery system to collect flue gas.Flue gas is recovered through solution hydrations such as sodium hydroxide or calcium hydroxides and absorbs, and obtains phosphorous and aqueous solution vanadium, extracts after separating and finally obtains vanadium and phosphorus product.
Above content is in conjunction with concrete preferred implementation further description made for the present invention; can not assert that the specific embodiment of the present invention only limits to this; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by submitted to claims.
Claims (8)
1. smelt continuously a vanadophosphoric ferric method, it is characterized in that, the method comprises the steps:
Step 1 heats vanadophosphoric ferric in electric furnace or the winding-up of some coal gas is heated to red heat state or molten state;
Step 2 is poured in converting furnace and is carried out oxygen blast within adding electrothermal stove or by the vanadophosphoric ferric of high temperature, utilizes chemical reaction heat to flux and burns the vanadophosphoric ferric of red heat state or molten state;
Step 3, after treating that vanadophosphoric ferric melts completely, adds basic cpd according to mass ratio when temperature is higher, continues oxygen blast, smelts 10-50min and slags tap, and obtains respectively vanadium slag and high-phosphorus ferronickel water that vanadiumcontent is higher;
Step 4, vanadium slag skims, and utilizes the method for traditional sodium roasting to carry out vanadium extraction to vanadium slag; The high-phosphorus ferronickel water of pouring out 30-60% waters casts iron ingot;
Step 5, residue high-phosphorus ferronickel water mixes with the 40-150% normal-temperature vanadophosphoric ferric that again fills into the interior melt quality of stove, and repeating step two, to step 4, constantly obtains vanadium slag and high-phosphorus ferronickel ingot that vanadiumcontent is higher, realizes and smelts continuously vanadophosphoric ferric.
2. continuous smelting vanadophosphoric ferric method according to claim 1, is characterized in that, the method further comprises:
In described step 2, oxygen blast in process furnace, produces gaseous state P in the part vanadium in iron liquid and phosphorus oxidation process
2o
5and V
2o
5flue gas is recovered to fume recovery system; Recovery system absorbs flue gas through alkaline solution hydration, obtain phosphorous and aqueous solution vanadium, the aqueous solution of phosphorous and vanadium through extract separated after, finally obtain vanadium and phosphorus product.
3. continuous smelting vanadophosphoric ferric method according to claim 2, is characterized in that, described alkaline solution is sodium hydroxide or aqua calcis.
4. continuous smelting vanadophosphoric ferric method according to claim 1, is characterized in that, the basic cpd that the described acidic oxide that interpolation is used for and oxygen blast produces in process furnace is made vanadium slag is calcium oxide, sodium carbonate or calcium carbonate.
5. the method for continuous smelting vanadophosphoric ferric according to claim 4, is characterized in that: described in to add basic cpd addition be vanadophosphoric ferric: basic cpd=10:0.9-10:1.3 according to mass ratio.
6. the method for continuous smelting vanadophosphoric ferric according to claim 1, is characterized in that: described in be heated to red heat state or molten state be by vanadophosphoric ferric in electric furnace or the winding-up of some coal gas be heated to 800-1500 ℃.
7. according to the continuous smelting vanadophosphoric ferric method described in claim 1-6, it is characterized in that, described vanadophosphoric ferric is poured in converting furnace and is carried out oxygen blast for blowing pure oxygen, oxygen-rich air or air.
8. continuous smelting vanadophosphoric ferric method according to claim 7, is characterized in that, described temperature adds basic cpd when higher, continues oxygen blast and guarantees that homo(io)thermism is within the scope of 1100-1500 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111304408A (en) * | 2020-03-25 | 2020-06-19 | 中国科学院过程工程研究所 | Method for refining ferrophosphorus |
| CN117512362A (en) * | 2023-11-29 | 2024-02-06 | 马鞍山中科冶金材料科技有限公司 | Method for extracting vanadium and dephosphorizing vanadium-containing molten iron |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696321A (en) * | 2005-04-15 | 2005-11-16 | 李春德 | Method for jpreparing high ferrotitanium in use for smelting steel |
| CN1970803A (en) * | 2006-10-24 | 2007-05-30 | 郴州市金龙铁合金有限公司 | Process for smelting ferrovanadium by extraction of vanadium from vanadium-containing errophosphorus |
| CN101705367A (en) * | 2009-11-23 | 2010-05-12 | 长沙有色冶金设计研究院 | Copper nickel smelting process with oxygen-enriched side-blowing bath smelting method |
-
2013
- 2013-11-01 CN CN201310539239.1A patent/CN103614564B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696321A (en) * | 2005-04-15 | 2005-11-16 | 李春德 | Method for jpreparing high ferrotitanium in use for smelting steel |
| CN1970803A (en) * | 2006-10-24 | 2007-05-30 | 郴州市金龙铁合金有限公司 | Process for smelting ferrovanadium by extraction of vanadium from vanadium-containing errophosphorus |
| CN101705367A (en) * | 2009-11-23 | 2010-05-12 | 长沙有色冶金设计研究院 | Copper nickel smelting process with oxygen-enriched side-blowing bath smelting method |
Non-Patent Citations (1)
| Title |
|---|
| 向秋林等: "从含钒磷铁中提取钒", 《湿法冶金》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111304408A (en) * | 2020-03-25 | 2020-06-19 | 中国科学院过程工程研究所 | Method for refining ferrophosphorus |
| CN117512362A (en) * | 2023-11-29 | 2024-02-06 | 马鞍山中科冶金材料科技有限公司 | Method for extracting vanadium and dephosphorizing vanadium-containing molten iron |
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