CN103526051A - Method for separating iron, vanadium and titanium from schreyerite - Google Patents
Method for separating iron, vanadium and titanium from schreyerite Download PDFInfo
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Abstract
The invention discloses a method for separating iron, vanadium and titanium from schreyerite, which comprises the following steps: mixing schreyerite, sodium sulfate, a reducer and an adhesive, pressing into mineral coal pellets, drying the mineral coal pellets, filling into a rotary hearth furnace, and roasting at 1000-1300 DEG C for 20-60 minutes to obtain metalized pellets, wherein a neutral or micro-oxygenation atmosphere is in the rotary hearth furnace; crushing the metalized pellets, leaching at 70-90 DEG C while controlling the pH value at 3-5, and filtering the leach solution to obtain a vanadium solution; slurrying the leaching leftovers by ball milling while controlling the particle size at 0.045mm, and carrying out primary magnetic separation under the magnetic field intensity of 0.3-0.5T to obtain a nonmagnetic material which is a first titanium-rich material; carrying out secondary magnetic separation on the magnetic material under the magnetic field intensity of 0.02-0.04T to obtain a magnetic material which is a first iron-rich material; and slurrying the nonmagnetic material from the secondary magnetic separation by ball milling, and reseparating to obtain a second iron-rich material and a second titanium-rich material.
Description
Technical field
The present invention relates to the method for utilizing of schreyerite, more particularly, relate to the separation method of iron, vanadium and titanium in a kind of schreyerite.
Background technology
Climb western vanadium titano-magnetite aboundresources, the high efficiency separation that how to realize ferrovanadium titanium resource is the most urgent research topic.The traditional technology that main employing Mineral separation iron and titanium, blast furnace ironmaking, vanadium extraction by converter blowing are made steel at present, technical process is long, and intermediate by-products is more, more remarkable to environmental influence, and the recovery utilization rate of available resources is lower, and the utilization ratio of titanium is 45% left and right only.For the lower feature of traditional technology resource utilization, climb steel and carried out the prereduction of schreyerite rotary hearth furnace, the molten technique of dividing separated ferrovanadium titanium of electric furnace, and built up the pilot scale line of 100,000 tons of scales, but this process energy consumption is higher, and electric furnace liner erosion is very fast, has more deficiency.
The domestic vanadium titano-magnetite comprehensive utilization of resources research work sixties in last century just carry out, the intensification of smelting process in BF of main tackling key problem vanadium titano-magnetite, by feedstock optimization, arrange in pairs or groups at present, vanadium titano-magnetite blast furnace smelting technology is ripe, but this technique titanium resource is distributed in blast furnace slag, cannot recycle titanium, even if recycle, technical difficulty is larger, and economy is poor.Also carried out the first vanadium extraction of vanadium titano-magnetite sodium pelletizing oxidizing roasting simultaneously, the research of rear prereduction metallic iron, molten minute separated ferrotitanium, technical process is longer, and equipment and technology restriction is more, does not finally realize industrialization.
2006, climb steel and carried out the technical study of vanadium titano-magnetite pit coal pelletizing rotary hearth furnace reduction, molten minute of electric furnace, desulfurizing iron vanadium extraction, got through technical process, can realize effective separation of ferrovanadium titanium, and built up the pilot scale line of year processing 100,000 tons of iron ore concentrate scales, successfully carried out many wheel tests, satisfactory for result.But this technique still exists energy consumption higher, the jejune feature of equipment.
Abroad, New Zealand and South Africa all adopt rotary kiln reduced iron concentrate, the electric furnace technique of molten minute, have only reclaimed iron and vanadium, and titanium is stayed in slag and processed for other construction applications or stacking.
In prior art at home, for example, Chinese patent application CN1814813A disclose a kind of from vanadium titano-magnetite method and the Chinese patent application CN101619371A of separating and extracting Fe, vanadium and titanium a kind of method that reclaims vanadium ferrotianium from vanadium titano-magnetite is disclosed, the two all discloses vanadium titano-magnetite by the technique of the molten separated ferrovanadium titanium of division technique of the dark reduction of pit coal pelletizing → rotary hearth furnace reduction processed → molten minute stove, this technique is built up pilot scale line in Pan Ganghelong boa group, but exist energy consumption high, the features such as molten minute stove lining erosion is serious, need to improve.Chinese patent CN102061397B discloses a kind of method of recycling vanadium, chromium, titanium, iron from vanadium titano-magnetite, comprise and will after ore or concentrate fragmentation, allocate sodium salt, oxidizing roasting into, vanadium and chromium are converted into water-soluble vanadic acid sodium and Sodium chromate, water logging is in solution, and from solution, separated vanadium chromium obtains Vanadium Pentoxide in FLAKES and chromium sesquioxide product.After leaching, residue can be allocated coal dust pelletizing into, in rotary hearth furnace, reduces, and magnetic separation separation of iron and titanium, obtain the raw material that magnetic powder can be used as powder metallurgy or steel-making, and containing TiO
2be greater than 50% non-magnetic product as the raw material of carrying titanium.This technique is traditional northern flow process, and roasting repeatedly makes long flow path, and energy consumption is high.
Summary of the invention
The object of the present invention is to provide iron in a kind of schreyerite, vanadium and the titanium method of separation and Extraction simultaneously, with simplification of flowsheet and reduce energy consumption and cost.
To achieve these goals, the invention provides the separation method of iron, vanadium and titanium in a kind of schreyerite, described separation method comprises the following steps: 80～100 parts of schreyerite, 5～30 parts of sodium sulfate, 15～30 parts of reductive agents and 1～8 part of binding agent are mixed and be pressed into pit coal pelletizing, after described pit coal pelletizing is dry, pack roasting in rotary hearth furnace and at 1000～1300 ℃ into and within 20～60 minutes, obtain metallized pellet, wherein, in described rotary hearth furnace, be neutrality or micro-oxygenation atmosphere; To after the metallized pellet fragmentation of gained, leach, extraction temperature is 70～90 ℃, and it is 3～5 that pH value is controlled, and then leach liquor is filtered to clarification and obtains vanadium liquid; To leach residuum by ball milling slurrying and control granularity below 0.045mm, and carrying out a magnetic separation separation under the condition that is then 0.3～0.5T in magneticstrength, the non-magnetic material obtaining is the first rich titanium material; Under the condition that is 0.02～0.04T by the magnetic material of gained in magneticstrength again, carry out secondary magnetic separation separated, the magnetic material obtaining is the first rich iron charge; Finally the separating obtained non-magnetic material of secondary magnetic separation is obtained to the second rich iron charge and the second rich titanium material by ball milling slurrying and Gravity separation.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, described schreyerite is v-ti magnetite concentrate or ilmenite concentrate, the granularity < 0.1mm of described schreyerite.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, described reductive agent is coke powder, pulverized anthracite or brown coal powder, the granularity < 0.1mm of described reductive agent.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, described sodium sulfate is that purity is 90～99% industrial sulphuric acid sodium, the granularity < 0.1mm of described industrial sulphuric acid sodium.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, described binding agent is polyose binding agent, polyalcohols binding agent, Walocel MT 20.000PV or basic metal water glass.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, described pit coal pelletizing is that particle diameter is the circular or oval pelletizing of 10～30mm.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, a described magnetic separation is separated to be carried out with the separated employing of secondary magnetic separation rotary drum magnetic separator, and described Gravity separation adopts shaking table or spiral chute to carry out.
According to an embodiment of the separation method of iron, vanadium and titanium in schreyerite of the present invention, the concentrated rear ammonium salt that adopts of described vanadium liquid is carried out to precipitation, the flue gas that rotary hearth furnace is produced is prepared sulfuric acid.
The present invention compares with existing techniques such as current existing cooled agglomerated pellet direct-reduction technique, sodium pelletizing oxidizing roasting techniques, has the following advantages:
1. only by a step reduction, the iron in mineral can be converted into metallic iron, vanadium is converted into soluble sodium salt, then by leaching vanadium extraction and magnetic separation gravity treatment combination separation of iron and titanium, realizes the high efficiency separation of three kinds of elements, avoid molten minute stove high temperature reduction and molten dividing, reduced energy consumption.Titaniferous material is without pyroprocessing simultaneously, and solubility in acid is better, can adopt traditional sulfuric acid process to carry titanium.
2. rich iron charge can return as iron-making and steel-making ferriferous raw material, also further deep processing iron powder product.
3. the by product that industrial sulphuric acid sodium is supporting process for extracting vanadium, generation is huge, for this technique provides raw material cheap and easy to get.
Accompanying drawing explanation
Fig. 1 is the flow process figure of the separation method of iron, vanadium and titanium in schreyerite of the present invention.
Embodiment
Below, with reference to accompanying drawing, describe the separation method of iron, vanadium and titanium in schreyerite of the present invention in detail.
Fig. 1 is the flow process figure of the separation method of iron, vanadium and titanium in schreyerite of the present invention.As shown in Figure 1, according to the separation method of iron, vanadium and titanium in schreyerite of the present invention, comprise the following steps:
First prepare burden, 80～100 parts of schreyerite, 5～30 parts of sodium sulfate, 15～30 parts of reductive agents and 1～8 part of binding agent are mixed and be pressed into pit coal pelletizing.Wherein, schreyerite can be v-ti magnetite concentrate, ilmenite concentrate or other schreyerite, the granularity < 0.1mm of schreyerite.Reductive agent can be coke powder, pulverized anthracite or brown coal powder etc., the granularity < 0.1mm of reductive agent, and the effect of reductive agent is that the iron reduction in schreyerite is become to metallic iron.Sodium sulfate can be the purity industrial sulphuric acid sodium that is 90～99%, the granularity < 0.1mm of industrial sulphuric acid sodium, and adopting industrial sulphuric acid sodium is that generation is large and cheap and easy to get because it is the by product of supporting process for extracting vanadium.Binding agent can be polyose binding agent, polyalcohols binding agent, Walocel MT 20.000PV or basic metal water glass etc., adopt organic binder bond and mineral binder bond all can, as long as can make the moulding of pit coal pelletizing.Because the less raw material of granularity is conducive to the subsequent processing steps such as mixing, roasting of material, therefore the granularity of each raw material is advisable to be less than 0.1mm.Preferably, pit coal pelletizing is that particle diameter is the circular or oval pelletizing of 10～30mm, is convenient to processing.
Wherein, the effect of sodium sulfate is the catalytic reaction solution estranged by vanadium in iron ore etc. produce oxysulfide at high temperature, makes reaction atmosphere become micro-oxidizing atmosphere, is convenient to reduction and the conversion of vanadium, form vanadic acid sodium solvend, even if the vanadium in schreyerite is converted into soluble vanadium.In general, the content of sodium salt is higher, more be conducive to the conversion of vanadium, according to climbing concentrate content of vanadium, while allocating the sodium sulfate of 5 parts into, by the control of oxidizing atmosphere, the transformation efficiency of vanadium is higher, if under micro-reducing atmosphere, the amount of allocating into of sodium salt needs higher, allocate 30 parts of conversions that are enough to guarantee vanadium into, can form the sodium salt of titanium etc. simultaneously.
Then, packing roasting in rotary hearth furnace and at 1000～1300 ℃ into and obtain metallized pellet in 20～60 minutes after pit coal pelletizing is dried, wherein, is neutrality or micro-oxygenation atmosphere in rotary hearth furnace.Thus, can in rotary hearth furnace, realize simultaneously by the iron in schreyerite be reduced to metallic iron, vanadium is converted into soluble vanadium.During dry pit coal pelletizing, can directly utilize the waste heat of rotary hearth furnace flue gas to carry out, its temperature can arrive 100～300 ℃, has both been enough to carry out the dry of material, is also conducive to save energy and reduces energy consumption.Making in rotary hearth furnace is the conversion that neutrality or micro-oxygenation atmosphere are conducive to vanadium, also can guarantee that the metallic iron in metallized pellet is not oxidized simultaneously, is conducive to improve the rate of recovery of iron, vanadium and titanium.The whole atmosphere of rotary hearth furnace bottom is neutrality or micro-oxygenation atmosphere, and for example furnace atmosphere comprises CO
27～15%, O
24～5%, CO1～3% etc., but the invention is not restricted to this.
Afterwards, will after the metallized pellet fragmentation of gained, leach, extraction temperature is 70～90 ℃, and it is 3～5 that pH value is controlled, and then leach liquor is filtered to clarification and obtains vanadium liquid.Preferably, the concentrated rear employing ammonium salt of vanadium liquid is carried out to precipitation and can realize the recovery to vanadium.In addition, the flue gas that rotary hearth furnace can also be produced be prepared sulfuric acid, for example, adopt organic amine absorption cycle desulfurization sulfuric acid processed, to reduce, pollutes and reclaims sulphur.Metallized pellet can directly leach under hot, also can cooling rear crushing and grinding and then adopt the hot water leaching of 70～90 ℃.In a word, must guarantee that higher extraction temperature is to guarantee leaching yield.
To leach residuum by ball milling slurrying again and control granularity below 0.045mm, and carrying out a magnetic separation separation under the condition that is then 0.3～0.5T in magneticstrength, the non-magnetic material obtaining is the first rich titanium material; Under the condition that is 0.02～0.04T by the magnetic material of gained in magneticstrength again, carry out secondary magnetic separation separated, the magnetic material obtaining is the first rich iron charge; Finally the separating obtained non-magnetic material of secondary magnetic separation is obtained to the second rich iron charge and the second rich titanium material by ball milling slurrying and Gravity separation, realized thus separated to vanadium, iron and titanium in schreyerite.Wherein, a magnetic separation is separated separated with secondary magnetic separation can adopt rotary drum magnetic separator to carry out, and Gravity separation can adopt shaking table or spiral chute to carry out.In order to guarantee the separated of iron and titanium, the material of magnetic separation need to guarantee thinner granularity, according to the present invention, the granularity that leaches residuum is controlled as below 0.045mm.
The present invention is that directly schreyerite first to be carried out to sodium reducing roasting and control furnace atmosphere be neutrality or micro-oxygenation atmosphere, can make thus that iron is converted into metallic iron, vanadium is converted into solvable vanadium simultaneously, then by leaching separated vanadium, by mode separation of iron and the titanium of high intensity magnetic separation, low intensity magnetic separation, gravity treatment combination, there is certain novelty again.
Below in conjunction with concrete example, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described example ranges.And unless otherwise noted, the per-cent relating in this specification sheets is all weight percentage.
example 1:
Schreyerite (is contained to TFe54.2%, V<sub TranNum="112">2</sub>o<sub TranNum="113">5</sub>0.62%, TiO<sub TranNum="114">2</sub>13.7%, granularity<0.1mm), reductive agent (pulverized anthracite, containing volatile matter 17.6%, ash content 7.9%, fixed carbon 74.6%, granularity<0.1mm), industrial sulphuric acid sodium (purity 92%, granularity<0.1mm), binding agent (sodium silicate) mixes and is pressed into pit coal pelletizing by the proportioning of 100 parts of schreyerite, 25 parts of reductive agents, 25 parts, sodium sulfate, 8 parts of binding agents, pack rotary hearth furnace into after dry at 150 ℃ and at 1100 ℃ roasting 40min, obtaining degree of metalization is more than 81% metallized pellet.Then after the metallized pellet of gained being broken into the particle below 2mm, adopt hot water leaching, extraction temperature is 90 ℃, and pH value is 5, filters and obtains vanadium liquid.To leach residuum by ball milling slurrying and control below granularity 0.045mm, and by rotary drum magnetic separator, with the magneticstrength of 0.4T, carrying out a magnetic separation separation, (the first rich titanium material, wherein contains TiO to obtain non-magnetic material<sub TranNum="115">2</sub>48.6%), the magnetic material of gained is carried out to secondary magnetic separation by rotary drum magnetic separator with the magneticstrength of 0.03T more separated, obtain magnetic material (i.e. the first rich iron charge, wherein containing TFe91.5%), by the non-magnetic material of gained, again by adopting table concentration after ball milling slurrying, separation obtains the second rich titanium material (wherein containing TiO<sub TranNum="116">2</sub>42.1%) and the second rich iron charge (wherein containing TFe55.7%).
example 2:
Schreyerite (is contained to TFe30.5%, TiO<sub TranNum="120">2</sub>47.2%, granularity<0.1mm), (pulverized anthracite, containing volatile matter 16.2% for reductive agent.Ash content 7.6%, fixed carbon 77.6%, granularity < 0.1mm), industrial sulphuric acid sodium (purity 95%, granularity < 0.1mm), binding agent (sodium cellulose glycolate) mixes and is pressed into pit coal pelletizing by the proportioning of 100 parts of schreyerite, 15 parts of reductive agents, 8 parts, sodium sulfate, 2 parts of binding agents, after dry at 200 ℃, pack rotary hearth furnace into and at 1200 ℃ roasting 50min, obtaining degree of metalization is more than 65% metallized pellet.Then after the metallized pellet of gained being broken into the particle below 3mm, adopt hot water leaching, extraction temperature is 90 ℃, and pH value is 4, filters and obtains vanadium liquid.To leach residuum by ball milling slurrying and control below granularity 0.045mm, and by rotary drum magnetic separator, with the magneticstrength of 0.5T, carrying out a magnetic separation separation, (the first rich titanium material, wherein contains TiO to obtain non-magnetic material<sub TranNum="121">2</sub>75.2%), the magnetic material of gained is carried out to secondary magnetic separation by rotary drum magnetic separator with the magneticstrength of 0.02T more separated, obtain magnetic material (i.e. the first rich iron charge, wherein containing TFe87.5%), by the non-magnetic material of gained, again by adopting table concentration after ball milling slurrying, separation obtains the second rich titanium material (wherein containing TiO<sub TranNum="122">2</sub>57.5%) and the second rich iron charge (wherein containing TFe51.8%).
embodiment 3
Schreyerite (is contained to TFe53.1%, V<sub TranNum="126">2</sub>o<sub TranNum="127">5</sub>0.57%, TiO<sub TranNum="128">2</sub>12.8%, granularity<0.1mm), reductive agent (brown coal, containing volatile matter 5.6%, ash content 28.2%, fixed carbon 64.6%, granularity<0.1mm), industrial sulphuric acid sodium (purity 98%, granularity<0.1mm), binding agent (polyose binding agent, because of complicated components, specifically do not exemplify) by the proportioning of 100 parts of schreyerite, 30 parts of reductive agents, 30 parts, sodium sulfate, 3 parts of binding agents, mix and be pressed into pit coal pelletizing, pack rotary hearth furnace into after dry at 100 ℃ and at 1250 ℃ roasting 60min, obtaining degree of metalization is more than 84% metallized pellet.Then after the metallized pellet of gained being broken into the particle below 2mm, adopt hot water leaching, extraction temperature is 85 ℃, and pH value is 3, filters and obtains vanadium liquid.To leach residuum by ball milling slurrying and control below granularity 0.045mm, and by rotary drum magnetic separator, with the magneticstrength of 0.6T, carrying out a magnetic separation separation, (the first rich titanium material, wherein contains TiO to obtain non-magnetic material<sub TranNum="129">2</sub>52.0%), the magnetic material of gained is carried out to secondary magnetic separation by rotary drum magnetic separator with the magneticstrength of 0.025T more separated, obtain magnetic material (i.e. the first rich iron charge, wherein containing TFe90.2%), by the non-magnetic material of gained, again by adopting table concentration after ball milling slurrying, separation obtains the second rich titanium material (wherein containing TiO<sub TranNum="130">2</sub>43.7%) and the second rich iron charge (wherein containing TFe57.2%).
In sum, the raw materials such as the vanadium titano-magnetite that in schreyerite of the present invention, the separation method of iron, vanadium and titanium adopts, industrial sulphuric acid sodium, coal dust are all cheap and easy to get, and can effectively the iron in schreyerite, vanadium and titanium resource be extracted by the method, technical process is simple, technical maturity is high, energy consumption is low, the comprehensive recovery of ferrovanadium titanium resource is high, degree of metalization can reach more than 80%, the rate of recovery of iron reaches more than 85%, the rate of recovery of vanadium reaches more than 75%, and the rate of recovery of titanium reaches more than 90%.
Claims (8)
1. a separation method for iron, vanadium and titanium in schreyerite, is characterized in that, described separation method comprises the following steps:
80～100 parts of schreyerite, 5～30 parts of sodium sulfate, 15～30 parts of reductive agents and 1～8 part of binding agent are mixed and be pressed into pit coal pelletizing, after described pit coal pelletizing is dry, pack roasting in rotary hearth furnace and at 1000～1300 ℃ into and within 20～60 minutes, obtain metallized pellet, wherein, in described rotary hearth furnace, be neutrality or micro-oxygenation atmosphere;
To after the metallized pellet fragmentation of gained, leach, extraction temperature is 70～90 ℃, and it is 3～5 that pH value is controlled, and then leach liquor is filtered to clarification and obtains vanadium liquid;
To leach residuum by ball milling slurrying and control granularity below 0.045mm, and carrying out a magnetic separation separation under the condition that is then 0.3～0.5T in magneticstrength, the non-magnetic material obtaining is the first rich titanium material; Under the condition that is 0.02～0.04T by the magnetic material of gained in magneticstrength again, carry out secondary magnetic separation separated, the magnetic material obtaining is the first rich iron charge; Finally the separating obtained non-magnetic material of secondary magnetic separation is obtained to the second rich iron charge and the second rich titanium material by ball milling slurrying and Gravity separation.
2. the separation method of iron, vanadium and titanium in schreyerite according to claim 1, is characterized in that, described schreyerite is v-ti magnetite concentrate or ilmenite concentrate, the granularity < 0.1mm of described schreyerite.
3. the separation method of iron, vanadium and titanium in schreyerite according to claim 1, is characterized in that, described reductive agent is coke powder, pulverized anthracite or brown coal powder, the granularity < 0.1mm of described reductive agent.
4. the separation method of iron, vanadium and titanium in schreyerite according to claim 1, is characterized in that, described sodium sulfate is that purity is 90～99% industrial sulphuric acid sodium, the granularity < 0.1mm of described industrial sulphuric acid sodium.
5. the separation method of ferrovanadium titanium in schreyerite according to claim 1, is characterized in that, described binding agent is polyose binding agent, polyalcohols binding agent, Walocel MT 20.000PV or basic metal water glass.
6. the separation method of iron, vanadium and titanium in schreyerite according to claim 1, is characterized in that, described pit coal pelletizing is that particle diameter is the circular or oval pelletizing of 10～30mm.
7. the separation method of iron, vanadium and titanium in schreyerite according to claim 1, is characterized in that, a described magnetic separation is separated to be carried out with the separated employing of secondary magnetic separation rotary drum magnetic separator, and described Gravity separation adopts shaking table or spiral chute to carry out.
8. the separation method of iron, vanadium and titanium in schreyerite according to claim 1, is characterized in that, the concentrated rear ammonium salt that adopts of described vanadium liquid is carried out to precipitation, and the flue gas that rotary hearth furnace is produced is prepared sulfuric acid.
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