CN104894365A - Method for recleaning of vanadium-titanium magnetite concentrate through calcination, oxidation alkaline leaching, acid pickling and reselection - Google Patents

Method for recleaning of vanadium-titanium magnetite concentrate through calcination, oxidation alkaline leaching, acid pickling and reselection Download PDF

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CN104894365A
CN104894365A CN201510320436.3A CN201510320436A CN104894365A CN 104894365 A CN104894365 A CN 104894365A CN 201510320436 A CN201510320436 A CN 201510320436A CN 104894365 A CN104894365 A CN 104894365A
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content
concentrate
pickling
alkali
gravity treatment
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刘晓明
朱大鹏
陈巍
郭客
王珂
李肃
王忠红
宋仁峰
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Angang Group Mining Co Ltd
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Angang Group Mining Co Ltd
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Abstract

The invention relates to a method for recleaning of vanadium-titanium magnetite concentrate through calcination, oxidation alkaline leaching, acid pickling and reselection. The method includes the following steps: adding vanadium-titanium magnetite concentrate to CaO as per the weight ratio of 1: 0.1-0.2, calcining at the temperature of 800 DEG C to 1400 DEG C, placing the calcining product A in an aqueous alkali with the mass concentration of 5% to 52%, and adding an oxidizing agent; then performing alkaline leaching for 0.5-2.0 h at the temperature of 220 DEG C to 330 DEG C to obtain a filtrate and an alkaline leaching filter cake B; then performing acid pickling and reselection on the filter cake B. The method has the following advantages: the introduction of O2 or H2O2 in oxidation alkaline leaching oxidizes S-containing compounds, thereby accelerating the reaction, reducing the reaction temperature and shortening the reaction time; iron ore concentrate with the content of TFe being 66%-69% and titanium concentrate with the content of TiO2 being 60%-80% are sorted out, so that impurities including TiO2, S, Si, Al and the like entering a blast furnace are reduced, the capacity factor of the blast furnace is improved, and the comprehensive utilization rate of titanium resources is improved at the same time.

Description

Utilize the method for calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate
Technical field
The present invention relates to a kind of ore-dressing technique of v-ti magnetite concentrate, particularly relate to a kind of method utilizing calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate.
Background technology
Vanadium titano-magnetite is a kind of complex ore of multiple metallic element, is based on the magnetite of the symbiosis of iron content, vanadium, titanium.And one of v-ti magnetite concentrate product that to be vanadium titano-magnetite obtain through ore dressing, wherein vanadium is composed with isomorph and is stored in titanomagnetite, displacement ferric ion.Titanomagnetite is oikocryst mineral (Fe 3o 4) and chadacryst ore deposit [ulvite 2FeOTiO 2, ilmenite FeOTiO 2, aluminum-spinel (Mg, Fe) (Al, Fe) 2o 4] complex body that formed.Such as, Chinese Panzhihua Region Midi Concentrator v-ti magnetite green ore and the chemistry of the v-ti magnetite concentrate after selecting iron multielement analysis the results are shown in Table 1, and v-ti magnetite green ore and vanadium titano-magnetite concentrate material phase analysis result are respectively in table 2 and table 3.
Table 1 Chinese Panzhihua Region Midi Concentrator raw ore and v-ti magnetite concentrate chemistry multielement analysis result
Element TFe FeO mFe S Fe 2O 3 TiO 2 V 2O 5
Raw ore 29.53 21.36 20.20 0.631 17.70 10.54 0.27 8
Concentrate 54.01 32.42 51.16 0.574 40.97 12.67 0.61
Element SiO 2 Al 2O 3 CaO MgO Co P As
Raw ore 22.80 7.65 6.36 7.23 0.02 0.015 <0.01
Concentrate 3.21 3.30 0.98 2.90 0.02 0.008 <0.010
Table 2 Chinese Panzhihua Region Midi Concentrator v-ti magnetite green ore titanium, iron chemical phase analysis result
Table 3 Chinese Panzhihua Region Midi Concentrator vanadium titano-magnetite concentrate titanium, iron chemical phase analysis result
Vanadium titano-magnetite aboundresources in the world, whole world reserves reach more than 40,000,000,000 tons, and reserves in China reaches 98.3 hundred million tons.In v-ti magnetite ore, iron is mainly composed and is stored in titanomagnetite, the TiO in ore 2main tax is stored in granular ilmenite and titanomagnetite.Generally, the titanium of about 57% is composed and is stored in titanomagnetite (mFeTiO 3nFe 3o 4) in, the titanium of about 40% is composed and is stored in ilmenite (FeTiO 3) in, because vanadium titano-magnetite ore composition is complicated, character is special, and thus the comprehensive utilization of this kind of ore is the international a great problem always thoroughly do not solved.This occurrence characteristics of vanadium titano-magnetite mineral determines the effective separation adopting physical concentration method cannot realize titanium, iron from the source of ore, cause v-ti magnetite ore after physical concentration, iron concentrate grade low (TFe<55%), the titanium in iron ore concentrate enters blast furnace slag (TiO completely at iron manufacturing process 2content reaches more than 22%) form vitreum, TiO 2lose activity and cannot economic recovery, meanwhile, titanium recovery rate is low only has 18%.Therefore sort titanium iron ore by the beneficiation method of physics and greatly reduce the value that titanium and iron utilizes separately.
China is first country comprehensively extracting iron, vanadium, titanium with technical scale from complicated vanadium titano-magnetite in the world, but due to general physical method fundamentally can not change iron, the tax of the fine and close symbiosis of titanium deposits characteristic, therefore, adopt the physical concentration methods such as common gravity separation method, magnetic method, flotation process to carry out titanium, iron is separated, efficiency is low, is difficult to select of high grade and the ilmenite concentrate that impurity is few or iron ore concentrate; Meanwhile, TiO 2organic efficiency is not high, v-ti magnetite green ore after Mineral separation, the TiO of about 54% 2enter iron ore concentrate, these TiO 2after blast-furnace smelting, almost all enter slag phase, form TiO 2the blast furnace slag of content 20 ~ 24%; In addition, because the foreign matter contents such as S, Si, the Al in iron ore concentrate are also too high, above-mentioned reason not only causes that steelmaking furnace utilization coefficient is low, energy consumption is large, titanium resource waste, and amount of slag is large, environmental pollution is serious.
CN2011100879566 discloses " a kind of beneficiation method of ilmenite ", is the magnetic separation after ore grinding, alkaline pretreatment, filtration, again ore grinding of v-ti magnetite green ore is obtained the method for ilmenite concentrate and iron ore concentrate.The method is by iron content 32.16% with containing TiO 2the v-ti magnetite green ore of 12.11%, by magnetic separation process after ore grinding, alkaline pretreatment, filtration, again ore grinding, defines iron content 59.30% iron ore concentrate and contains TiO 2the ilmenite concentrate of 20.15%.Because the method is for ilmenite raw ore, raw ore SiO 2, Al 2o 3, the gangue mineral content such as CaO, MgO is high, the process of alkali leaching preferentially will occur in SiO 2, Al 2o 3with it mineral, define the alkali leaching rear compound similar to titanium in the dipped journey of alkali, the NaOH alkali number of alkali leaching ferrotianium raw ore consumption is 469Kg/t raw ore, and cost is high; And the titanium compound formed after the leaching of ferrotianium raw ore alkali, the compound of the silicon formed after soaking with the gangue mineral alkali such as quartz, it is very difficult for wanting to realize effectively being separated in follow-up magnetic separation, and this also constrains the raising of the rear iron concentrate grade of ferrotianium raw ore alkali leaching and ilmenite concentrate grade.Meanwhile, the method adopts twice grinding process to change mineral surface physicochemical property, adds complexity and the process cost of the method.In a word, by this kind of procedure complexity, and in treating processes, quantity of alkali consumption is large, cost is high; Meanwhile, more high-grade iron ore concentrate and ilmenite concentrate cannot be obtained.
CN201310183580.8 discloses " a kind of wet processing sefstromite concentrate prepares the method for titanium liquid ", proposes the method with salt pickling separating titanium iron.This invention is the method that wet processing v-ti magnetite concentrate prepares titanium liquid, comprise v-ti magnetite concentrate hydrochloric acid leaching, molten salt react ion, again pickling, sulfuric acid solution, filtration etc. and obtain the processes such as titanium liquid, the method is mainly for extraction ilmenite concentrate, its complex technical process, need in hydrochloric acid leaching process to react with hydrochloric acid and iron and vanadium to dissolve in filtrate, consume a large amount of hydrochloric acid, cost is high; Meanwhile, NaOH and titanium and pasc reaction is used to consume alkali in fused salt process.In addition, owing to employing hydrochloric acid in the method leaching process, in hydrochloric acid, chlorion is large to equipment corrosion, not easily suitability for industrialized production.The method is mainly applicable to the recycling of titanium in the low poor v-ti magnetite concentrate of high vanadium low iron content.
During Chinese patent 201210137458.2 discloses " reclaiming the method for vanadium in vanadium titano-magnetite ", adopt calcification baking-carbonating to leach the vanadium reclaimed in vanadium titano-magnetite, the agglomerates of sintered pellets of the calcic Iron-ore Slag obtained can directly apply to blast-furnace smelting; Thus efficiently solve the recovery of vanadium in vanadium titano-magnetite, can't follow-up blast-furnace smelting be impacted; The recyclable chromium of crystalline mother solution obtained after reclaiming vanadium, thus more effectively realize the comprehensive utilization of vanadium titano-magnetite.Although the method applies the method for calcification baking, alkali-free leaching, magnetic separation process, pickling is weakly acidic carbonating, obviously different from the mechanism of action of sulfuric acid strong acid.
CN201410164297.5 discloses one and " utilizes calcining, alkali leaching, pickling and gravity treatment to select the method for v-ti magnetite concentrate again ", the ratio of v-ti magnetite concentrate 1:0.1 ~ 0.2 is by weight added CaO by this invention, then at the temperature of 800 DEG C ~ 1400 DEG C, calcining 20 ~ 60 minutes is carried out, again calcination product is placed in the leaching of alkaline solution alkali, then by the alkali leaching cake after filtration in H 2sO 4pickling in solution, then acidleach filter cake is carried out gravity treatment, obtain the iron ore concentrate that TFe content is 65% ~ 68% respectively, TiO 2content is the ilmenite concentrate of 60% ~ 80%.The method achieve and efficiently sort v-ti magnetite concentrate, but adopt alkali leaching due to simple in reaction, react 0.5 ~ 5 hour at 300 ~ 370 DEG C of temperature, chemical reaction temperature is higher, and the time is longer, and SiO after reaction 2and TiO 2content is up to 3%, and foreign matter content is higher, causes the capacity factor of a blast furnace to reduce, adds ironmaking cost; Meanwhile, in this inventive method, alkaline consumption is higher, sodium titanate or the lower titanium resource utilization ratio that causes of potassium titanate productive rate not high.
Summary of the invention
In order to overcome the deficiency of above-mentioned beneficiation method, technical problem to be solved by this invention is on the basis that physics and chemistry beneficiation method effectively combines, a kind of method that cost is low, reclaim quality and the high and utilization calcining of good operability of efficiency, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate is provided, achieve and high efficiency separation is carried out to titanium, iron in v-ti magnetite concentrate, improve into stokehold Iron grade, reduce and enter blast furnace TiO 2, the impurity such as S, Si, Al content, improve the capacity factor of a blast furnace, reduce the quantity discharged of blast furnace slag, reduce ironmaking cost, improve TiO 2comprehensive resource utilization rate, reduces NaOH or KOH consumption simultaneously, decreases environmental pollution.
In order to realize object of the present invention, technical scheme of the present invention is achieved in that
A kind of method utilizing calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate of the present invention, is characterized in that comprising the steps:
1) calcine
Be 50% ~ 55%, TiO by TFe content range 2content range is 10% ~ 15%, SiO 2content is 3% ~ 6%, Al 2o 3content is 3% ~ 6%, the ratio of the v-ti magnetite concentrate of S content >0.5% 1:0.1 ~ 0.2 by weight adds CaO, at the temperature of 800 DEG C ~ 1400 DEG C, carry out calcining 20 ~ 60 minutes, forms calcination product A;
2) alkali oxide leaching
Calcination product A in step 1) is placed in the alkaline solution that mass concentration is 5% ~ 52%, adds oxygenant, then at the temperature of 220 DEG C ~ 330 DEG C, alkali soaks reaction 0.5 ~ 2.0 hour, and obtain filtrate and alkali leaching cake B, described filtrate feeds recovery and processing system;
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:1 ~ 10, then be placed in the H that mass concentration is 1% ~ 10% 2sO 4in solution, under 50 DEG C ~ 90 DEG C conditions, pickling 5 ~ 60 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system;
4) gravity treatment
The ore pulp making mass concentration 35% ~ 40% that added water by acidleach filter cake C in step 3) carries out gravity treatment, obtain gravity concentrate D, gravity tailings E and gravity treatment chats F respectively, described gravity concentrate D to be TFe content range be 66% ~ 69% iron ore concentrate, described gravity treatment chats F is TiO 2content range is the ilmenite concentrate of 60% ~ 80%, and described gravity tailings E is SiO 2content range is the true tailings of 55% ~ 60%.
Described alkaline solution is any one in the NaOH aqueous solution, the KOH aqueous solution or NaOH and KOH mixed aqueous solution.
Described oxygenant is O 2or H 2o 2, O 2add-on is 20 ~ 120psi, H 2o 2add-on is 50 ~ 200kg/t to ore deposit.
Described gravity treatment adopts the spiral chute of ￠ 0.6 ~ ￠ 1.2 meters to carry out gravity treatment.
Advantage of the present invention is:
Calcination utilizes CaO part to replace alkali lye consumption in the dipped journey of alkali, decreases the consumption 20% ~ 30% of NaOH or KOH in follow-up alkali leaching operation; Because CaO price is NaOH price 1/5 ~ 1/6, be 1/20 of KOH price, therefore greatly can reduce production cost.
The process of alkali oxide leaching has carried out chemical reaction to elements such as Ti, S, Si, Al in v-ti magnetite concentrate, defines corresponding salt, makes the iron in v-ti magnetite concentrate change the form of ferric oxide into.With v-ti magnetite concentrate unlike, SiO in ilmenite raw ore 2and Al 2o 3content far away higher than SiO in v-ti magnetite concentrate 2and Al 2o 3content, wherein SiO in ilmenite raw ore 2>20%, Al 2o 3>7%, SiO in v-ti magnetite concentrate 2<6%, Al 2o 3<6%.In alkali leaching ilmenite raw ore process, because the process of alkali leaching preferentially will occur in SiO 2, Al 2o 3deng on mineral, alkali is made to soak v-ti magnetite concentrate more less than alkali leaching ilmenite raw ore alkali consumption, simultaneously O 2introducing make containing S compound oxidation, oxidized FeTiO 3, accelerate reaction, reduce temperature of reaction, shorten the reaction times, better effects if, greatly reduce energy consumption and facility investment.Such as, after calcining, when soaking with NaOH alkali oxide, the alkali number that the present invention consumes is less than 50kg/t concentrate, reduces more than 9 times, than not passing into O than the alkali number 469kg/t raw ore of alkali leaching raw ore consumption 2alkali leaching consume alkali number reduce 10kg/t concentrate; Meanwhile, O 2introducing alkali is soaked temperature of reaction is minimum is down to 220 DEG C, the reaction times is less than 2 hours.
Acid cleaning process has dissolved oxysalt and the sulfide such as Ti, Si, Al after alkali leaching effectively, makes it to dissociate with iron ore concentrate.In addition because the present invention adopts sulfuric acid to carry out pickling, reaction conditions is gentle, and little to equipment corrosion, cost is low, is more conducive to suitability for industrialized production.
Add gravity treatment, make iron concentrate grade bring up to 66% ~ 69% by 50% ~ 55%, in isolated iron ore concentrate, S content significantly reduces simultaneously, is down to is less than 0.10%, SiO by more than 0.50% 2content is down to less than 1%, Al by 3% ~ 6% 2o 3content is down to less than 1.8%, TiO by 3% ~ 6% 2content is down to less than 6% by more than 12%; Meanwhile, TiO can also be obtained 2content is the ilmenite concentrate of 60% ~ 80%.
The method of this invention integrated use calcining, alkali oxide leaching, pickling and gravity treatment selects v-ti magnetite concentrate again, achieves titanium in v-ti magnetite concentrate, iron high efficiency separation, reduces and enter blast furnace TiO 2, the impurity such as S, Si, Al content, improve the capacity factor of a blast furnace, reduce the quantity discharged of blast furnace slag, reduce ironmaking cost, for subsequent smelting creates better condition, improve the comprehensive utilization ratio of titanium resource simultaneously.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Fig. 2 is that the present invention adopts two sections of gravity separation technology schemas.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further:
As shown in Figure 1.
Embodiment 1
1) calcine
Be 50.5%, TiO by TFe content 2content is 14.2%, SiO 2content is 3.63%, Al 2o 3content is 4.42%, the v-ti magnetite concentrate of S content 0.59%, and the ratio of 1:0.1 adds CaO by weight, at the temperature of 800 DEG C, carry out calcining 60 minutes, and form calcination product A, its chemical equation is:
CaO+ TiO 2 CaTiO 3
2) alkali oxide leaching
Calcination product A in step 1) is placed in the NaOH alkaline solution that mass concentration is 30%, passes into the O of 26psi 2, then at the temperature of 220 DEG C, alkali soaks reaction 2.0 hours, and filtered by reactant, obtain filtrate and alkali leaching cake B, NaOH consumption 49 kg/t is to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is:
4mFeTiO 3+8NaOH +mO 2 2mFe 2O 3↓+4Na 2O·(TiO 2) m↓+4H 2O m≥1
pFe 3O 4·q（FeO·TiO 2) +2rNaOH pFe 3O 4↓+qFeO↓+ (Na 2O) r·(TiO 2) q↓+rH 2O
Al 2O 3+2NaOH 2NaAlO 2+ H 2O
tSiO 2+2NaOH Na 2O·(SiO 2) t↓+ H 2O
3FeS 2+6NaOH 3FeS↓+Na 2SO 3+2Na 2S+3H 2O
4FeS 2+ 11O 2 2Fe 2O 3 + 8SO 2
4FeO+O 2 2Fe 2O 3
2SO 2+O 2+4NaOH 2Na 2SO 4+ 2H 2O
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:9.5, then be placed in the H that mass concentration is 7% 2sO 4in solution, under the condition of 65 DEG C, pickling 60 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is:
Na 2O·(TiO 2) x +H + (H 2O)·（TiO 2) x↓+Na +
Na 2O·（SiO 2） t+H + (H 2O)·（SiO 2) t↓+Na +
NaAlO 2+4H + Al 3++Na ++2H 2O
4) gravity treatment
The spiral chute of the ore pulp ￠ 1.2 meters making mass concentration 40% of being added water by acidleach filter cake C in step 3) carries out gravity treatment, respectively gravity concentrate D, gravity tailings E and gravity treatment chats F, gravity concentrate D to be TFe content be 66.5% final iron ore concentrate, wherein SiO 2content is 0.38%, Al 2o 3content is 1.18%, S content is 0.02%; Described gravity tailings E is SiO 2content is the true tailings of 59.1%, and gravity treatment chats F is TiO 2content is the final ilmenite concentrate of 60.4%.
Embodiment 2
1) calcine
Be 54.8%, TiO by TFe content 2content is 10.5%, SiO 2content is 3.55%, Al 2o 3content is 5.45%, the v-ti magnetite concentrate of S content 0.76%, and the ratio of 1:0.1 adds CaO by weight, at the temperature of 900 DEG C, carry out calcining 50 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in the NaOH alkaline solution that mass concentration is 24%, passes into the O of 50psi 2, then at the temperature of 310 DEG C, alkali soaks reaction 1.0 hours, and filtered by reactant, obtain filtrate and alkali leaching cake B, NaOH consumption 38 kg/t is to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1;
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:7, then be placed in the H that mass concentration is 10% 2sO 4in solution, under the condition of 50 DEG C, pickling 20 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1;
4) gravity treatment
The spiral chute of the ore pulp ￠ 0.9 meter making mass concentration 36% of being added water by acidleach filter cake C in step 3) carries out gravity treatment, respectively gravity concentrate D, gravity tailings E and gravity treatment chats F, gravity concentrate D to be TFe content be 67.3% final iron ore concentrate, wherein SiO 2content is 0.60%, Al 2o 3content is 1.18%, S content is 0.02%; Described gravity tailings E is SiO 2content is the true tailings of 58.1%, and gravity treatment chats F is TiO 2content is the final ilmenite concentrate of 77.3%.
Embodiment 3
1) calcine
Be 53.4%, TiO by TFe content 2content is 13.1%, SiO 2content is 3.72%, Al 2o 3content is 5.49%, the v-ti magnetite concentrate of S content 0.86%, and the ratio of 1:0.1 adds CaO by weight, at the temperature of 1000 DEG C, carry out calcining 40 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in the NaOH alkaline solution that mass concentration is 18%, adds 83kg/t to ore deposith 2o 2, then at the temperature of 270 DEG C, alkali soaks reaction 45 minutes, and filtered by reactant, obtain filtrate and alkali leaching cake B, NaOH consumption 40 kg/t is to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is:
2mFeTiO 3+4NaOH+mH 2O 2 mFe 2O 3↓+2Na 2O·(TiO 2) m↓+(m+2)H 2O m≥1
pFe 3O 4·q（FeO·TiO 2) +2rNaOH pFe 3O 4↓+qFeO↓+ (Na 2O) r·(TiO 2) q↓+rH 2O
Al 2O 3+2NaOH 2NaAlO 2+ H 2O
tSiO 2+2NaOH Na 2O·(SiO 2) t↓+ H 2O
3FeS 2+6NaOH 3FeS↓+Na 2SO 3+2Na 2S+3H 2O
2FeS 2+ 11H 2O 2 Fe 2O 3 +4SO 2+ 11H 2O
2FeO+H 2O 2 Fe 2O 3+ H 2O
SO 2+H 2O 2+2NaOH Na 2SO 4+ 2H 2O
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:5, then be placed in the H that mass concentration is 6% 2sO 4in solution, under the condition of 60 DEG C, pickling 6 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1;
4) gravity treatment
The spiral chute of the ore pulp ￠ 1.2 meters making mass concentration 40% of being added water by acidleach filter cake C in step 3) carries out gravity treatment, respectively gravity concentrate D, gravity tailings E and gravity treatment chats F, gravity concentrate D to be TFe content be 67.0% final iron ore concentrate, wherein SiO 2content is 0.40%, Al 2o 3content is 1.27%, S content is 0.02%; Described gravity tailings E is SiO 2content is the true tailings of 57.6%, and gravity treatment chats F is TiO 2content is the final ilmenite concentrate of 73.1%.
Embodiment 4
1) calcine
Be 51.2%, TiO by TFe content 2content is 13.9%, SiO 2content is 3.93%, Al 2o 3content is 5.58%, the v-ti magnetite concentrate of S content 0.60%, and the ratio of 1:0.15 adds CaO by weight, at the temperature of 1100 DEG C, carry out calcining 35 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in the NaOH alkaline solution that mass concentration is 12%, passes into the O of 120psi 2, then at the temperature of 330 DEG C, alkali soaks reaction 0.5 hour, and filtered by reactant, obtain filtrate and alkali leaching cake B, NaOH consumption 36 kg/t is to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1;
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:1.5, then be placed in the H that mass concentration is 4% 2sO 4in solution, under the condition of 65 DEG C, pickling 40 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1;
4) gravity treatment
The spiral chute of the ore pulp ￠ 0.9 meter making mass concentration 40% of being added water by acidleach filter cake C in step 3) carries out gravity treatment, respectively gravity concentrate D, gravity tailings E and gravity treatment chats F, gravity concentrate D to be TFe content be 68.5% final iron ore concentrate, wherein SiO 2content is 0.44%, Al 2o 3content is 1.38%, S content is 0.02%; Described gravity tailings E is SiO 2content is the true tailings of 56.2%, and gravity treatment chats F is TiO 2content is the final ilmenite concentrate of 74.5%.
Embodiment 5
As shown in Figure 2.
1) calcine
Be 52.9%, TiO by TFe content 2content is 12.1%, SiO 2content is 3.92%, Al 2o 3content is 4.66%, the v-ti magnetite concentrate of S content 0.55%, and the ratio of 1:0.15 adds CaO by weight, at the temperature of 1200 DEG C, carry out calcining 30 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in the KOH alkaline solution that mass concentration is 38%, passes into the O of 86psi 2, then at the temperature of 255 DEG C, alkali soaks reaction 1.5 hours, and filtered by reactant, obtain filtrate and alkali leaching cake B, KOH consumption 30 kg/t is to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is:
4mFeTiO 3+8KOH+mO 2 2mFe 2O 3↓+4K 2O·(TiO 2) m↓+4H 2O m≥1
pFe 3O 4·q（FeO·TiO 2) +2rKOH pFe 3O 4↓+qFeO↓+ (K 2O) r·(TiO 2) q↓+rH 2O
Al 2O 3+2KOH 2KAlO 2+ H 2O
tSiO 2+2KOH K 2O·（SiO 2） t↓+ H 2O
3FeS 2+6KOH 3FeS↓+K 2SO 3+2K 2S+3H 2O
4FeS 2+ 11O 2 2Fe 2O 3 + 8SO 2
4FeO+O 2 2Fe 2O 3
2SO 2+O 2+4KOH 2K 2SO 4+ 2H 2O
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:3.5, then be placed in the H that mass concentration is 9% 2sO 4in solution, under the condition of 70 DEG C of pickling 15 minutes, filtered by pickling reactant, obtain filtrate and acidleach filter cake C, described filtrate fed recovery and processing system, and its chemical equation is:
K 2O·(TiO 2) x+H + (H 2O)·（TiO 2) x↓+ K +
K 2O·（SiO 2） t+H + (H 2O)·（SiO 2) t↓+ K +
KAlO 2+4H + Al 3++K ++2H 2O
4) gravity treatment
The spiral chute that the ore pulp of making mass concentration 36% of being added water by acidleach filter cake C in step 3) feeds ￠ 0.6 meter carries out one section and roughly selects, obtain one section of rougher concentration D1, an one section of rougher tailings E1 and section respectively and roughly select chats F, the spiral chute that the ore pulp of making mass concentration 41% of being added water by one section of rougher concentration D1 feeds ￠ 0.6 meter carry out two sections selected, obtain two sections of selected concentrate D2 and two section cleaner tailings E2 respectively, two sections of cleaner tailings E2 return one section of spiral chute roughly selected, two sections of selected concentrate D2 to be TFe content be 67.7% final iron ore concentrate, wherein SiO 2content is 0.46%, Al 2o 3content is 1.35%, S content is 0.02%; One section of described rougher tailings E1 is SiO 2content is the true tailings of 59.4%, and one section is roughly selected chats F is TiO 2content is the final ilmenite concentrate of 71.5%.
Embodiment 6
1) calcine
Be 54.0%, TiO by TFe content 2content is 11.5%, SiO 2content is 3.92%, Al 2o 3content is 4.74%, the v-ti magnetite concentrate of S content 0.53%, and the ratio of 1:0.2 adds CaO by weight, at the temperature of 1300 DEG C, carry out calcining 25 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in the KOH alkaline solution that mass concentration is 49%, adds 51kg/t to ore deposith 2o 2, then at the temperature of 290 DEG C, alkali soaks reaction 75 minutes, and filtered by reactant, obtain filtrate and alkali leaching cake B, KOH consumption 46 kg/t is to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is:
2mFeTiO 3+4KOH+mH 2O 2 mFe 2O 3↓+2K 2O·(TiO 2) m↓+(m+2)H 2O m≥1
pFe 3O 4·q（FeO·TiO 2) +2rKOH pFe 3O 4↓+qFeO↓+ (K 2O) r·(TiO 2) q↓+rH 2O
Al 2O 3+2KOH 2KAlO 2+ H 2O
tSiO 2+2KOH K 2O·(SiO 2) t↓+ H 2O
3FeS 2+6KOH 3FeS↓+K 2SO 3+2K 2S+3H 2O
2FeS 2+ 11H 2O 2 Fe 2O 3 +4SO 2+ 11H 2O
2FeO+H 2O 2 Fe 2O 3+ H 2O
SO 2+H 2O 2+2KOH K 2SO 4+ 2H 2O
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:3, then be placed in the H that mass concentration is 1% 2sO 4in solution, under the condition of 90 DEG C, pickling 50 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 5;
4) gravity treatment
The spiral chute that the ore pulp of making mass concentration 37% of being added water by acidleach filter cake C in step 3) feeds ￠ 0.9 meter carries out one section and roughly selects, obtain one section of rougher concentration D1, an one section of rougher tailings E1 and section respectively and roughly select chats F, the spiral chute that the ore pulp of making mass concentration 40% of being added water by one section of rougher concentration D1 feeds ￠ 0.6 meter carry out two sections selected, obtain two sections of selected concentrate D2 and two section cleaner tailings E2 respectively, two sections of cleaner tailings E2 return one section of spiral chute roughly selected, two sections of selected concentrate D2 to be TFe content be 68.0% final iron ore concentrate, wherein SiO 2content is 0.48%, Al 2o 3content is 1.60%, S content is 0.02%; One section of described rougher tailings E1 is SiO 2content is the true tailings of 57.8%, and one section is roughly selected chats F is TiO 2content is the final ilmenite concentrate of 72.4%.
Embodiment 7:
1) calcine
Be 52.1%, TiO by TFe content 2content is 11.3%, SiO 2content is 4.20%, Al 2o 3content is 4.52%, the v-ti magnetite concentrate of S content 0.71%, and the ratio of 1:0.2 adds CaO by weight, at the temperature of 1400 DEG C, carry out calcining 20 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in NaOH mass concentration be 22% and KOH mass concentration be the mixed ammonium/alkali solutions of 6%, pass into the O of 98psi 2, then at the temperature of 240 DEG C, alkali soaks reaction 100 minutes, is filtered by reactant, obtain filtrate and alkali leaching cake B, NaOH consumption 18kg/t is to ore deposit, KOH consumption 10 kg/t to ore deposit, and described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1 and embodiment 5;
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:2, then be placed in the H that mass concentration is 2.5% 2sO 4in solution, 80 DEG C of pickling 35 minutes, filtered by pickling reactant, obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1 and embodiment 5;
4) gravity treatment
One section of spiral chute that the ore pulp of making mass concentration 37% of being added water by acidleach filter cake C in step 3) feeds ￠ 0.9 meter carries out one section and roughly selects, obtain one section of rougher concentration D1, an one section of rougher tailings E1 and section respectively and roughly select chats F, the spiral chute that the ore pulp of making mass concentration 40% of being added water by one section of rougher concentration D1 feeds ￠ 0.6 meter carry out two sections selected, obtain two sections of selected concentrate D2 and two section cleaner tailings E2 respectively, two sections of cleaner tailings E2 return one section of spiral chute, two sections of selected concentrate D2 to be TFe content be 68.9% final iron ore concentrate, wherein SiO 2content is 0.31%, Al 2o 3content is 1.23%, S content is 0.01%; One section of described rougher tailings E1 is SiO 2content is the true tailings of 55.5%, and one section is roughly selected chats F is TiO 2content is the final ilmenite concentrate of 79.5%.
Embodiment 8:
1) calcine
Be 52.8%, TiO by TFe content 2content is 11.4%, SiO 2content is 3.80%, Al 2o 3content is 4.35%, the v-ti magnetite concentrate of S content 0.72%, and the ratio of 1:0.2 adds CaO by weight, at the temperature of 1300 DEG C, carry out calcining 30 minutes, and form calcination product A, its chemical equation is with embodiment 1;
2) alkali oxide leaching
Step 1) calcination product A is placed in NaOH mass concentration be 25% and KOH mass concentration be the mixed ammonium/alkali solutions of 5%, add 196kg/t to ore deposith 2o 2, then at the temperature of 250 DEG C, alkali soaks reaction 1.5 hours, is filtered by reactant, filtrate and alkali leaching cake B, NaOH consumption 18.5kg/t to ore deposit, KOH consumption 12.8 kg/t is to ore deposit, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 3 and embodiment 6;
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:3, then be placed in the H that mass concentration is 3% 2sO 4in solution, 70 DEG C of pickling 40 minutes, filtered by pickling reactant, obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system, and its chemical equation is with embodiment 1 and embodiment 5;
4) gravity treatment
One section of spiral chute that the ore pulp of making mass concentration 38% of being added water by acidleach filter cake C in step 3) feeds ￠ 0.9 meter carries out one section and roughly selects, obtain one section of rougher concentration D1, an one section of rougher tailings E1 and section respectively and roughly select chats F, the spiral chute that the ore pulp of making mass concentration 40% of being added water by one section of rougher concentration D1 feeds ￠ 0.6 meter carry out two sections selected, obtain two sections of selected concentrate D2 and two section cleaner tailings E2 respectively, two sections of cleaner tailings E2 return one section of spiral chute, two sections of selected concentrate D2 to be TFe content be 68.2% final iron ore concentrate, wherein SiO 2content is 0.31%, Al 2o 3content is 1.23%, S content is 0.01%; One section of described rougher tailings E1 is SiO 2content is the true tailings of 56.2%, and one section is roughly selected chats F is TiO 2content is the final ilmenite concentrate of 78.9%.

Claims (4)

1. utilize a method for calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate, it is characterized in that comprising the steps:
1) calcine
Be 50% ~ 55%, TiO by TFe content range 2content range is 10% ~ 15%, SiO 2content is 3% ~ 6%, Al 2o 3content is 3% ~ 6%, the ratio of the v-ti magnetite concentrate of S content >0.5% 1:0.1 ~ 0.2 by weight adds CaO, at the temperature of 800 DEG C ~ 1400 DEG C, carry out calcining 20 ~ 60 minutes, forms calcination product A;
2) alkali oxide leaching
Calcination product A in step 1) is placed in the alkaline solution that mass concentration is 5% ~ 52%, adds oxygenant, then at the temperature of 220 DEG C ~ 330 DEG C, alkali soaks reaction 0.5 ~ 2.0 hour, and obtain filtrate and alkali leaching cake B, described filtrate feeds recovery and processing system;
3) pickling
By step 2) in alkali leaching cake B add water and make the ore pulp that solid-liquid mass ratio is 1:1 ~ 10, then be placed in the H that mass concentration is 1% ~ 10% 2sO 4in solution, under 50 DEG C ~ 90 DEG C conditions, pickling 5 ~ 60 minutes, filters pickling reactant, and obtain filtrate and acidleach filter cake C, described filtrate feeds recovery and processing system;
4) gravity treatment
The ore pulp making mass concentration 35% ~ 40% that added water by acidleach filter cake C in step 3) carries out gravity treatment, obtain gravity concentrate D, gravity tailings E and gravity treatment chats F respectively, described gravity concentrate D to be TFe content range be 66% ~ 69% iron ore concentrate, described gravity treatment chats F is TiO 2content range is the ilmenite concentrate of 60% ~ 80%, and described gravity tailings E is SiO 2content range is the true tailings of 55% ~ 60%.
2. the method utilizing calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate according to claim 1, is characterized in that described alkaline solution is any one in the NaOH aqueous solution, the KOH aqueous solution or NaOH and KOH mixed aqueous solution.
3. the method utilizing calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate according to claim 1, is characterized in that described oxygenant is O 2or H 2o 2, described O 2add-on is 20 ~ 120psi, H 2o 2add-on is 50 ~ 200kg/t to ore deposit.
4. the method utilizing calcining, alkali oxide leaching, pickling and gravity treatment v-ti magnetite concentrate according to claim 1, is characterized in that described gravity treatment adopts the spiral chute of ￠ 0.6 ~ ￠ 1.2 meters to carry out gravity treatment.
CN201510320436.3A 2015-06-12 2015-06-12 Method for recleaning of vanadium-titanium magnetite concentrate through calcination, oxidation alkaline leaching, acid pickling and reselection Pending CN104894365A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010051120A1 (en) * 1997-10-17 2001-12-13 Marcelo De Matos Process for the production titanium concentrate having a chemical composition similar to ilmenite from highly impure anatase ores
CN102181626A (en) * 2011-04-08 2011-09-14 北京矿冶研究总院 Beneficiation method of ilmenite
CN102787194A (en) * 2012-08-27 2012-11-21 攀枝花学院 Method for preparing titanium-rich material by directly reducing molten slag from vanadium-titanium-ferrum concentrate
CN103526051A (en) * 2013-09-26 2014-01-22 攀钢集团攀枝花钢铁研究院有限公司 Method for separating iron, vanadium and titanium from schreyerite
CN103966422A (en) * 2014-04-23 2014-08-06 鞍钢集团矿业公司 Method for re-concentrating vanadium-titanium magnetite concentrate through calcination, alkaline leaching, acid pickling and re-selection

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010051120A1 (en) * 1997-10-17 2001-12-13 Marcelo De Matos Process for the production titanium concentrate having a chemical composition similar to ilmenite from highly impure anatase ores
CN102181626A (en) * 2011-04-08 2011-09-14 北京矿冶研究总院 Beneficiation method of ilmenite
CN102787194A (en) * 2012-08-27 2012-11-21 攀枝花学院 Method for preparing titanium-rich material by directly reducing molten slag from vanadium-titanium-ferrum concentrate
CN103526051A (en) * 2013-09-26 2014-01-22 攀钢集团攀枝花钢铁研究院有限公司 Method for separating iron, vanadium and titanium from schreyerite
CN103966422A (en) * 2014-04-23 2014-08-06 鞍钢集团矿业公司 Method for re-concentrating vanadium-titanium magnetite concentrate through calcination, alkaline leaching, acid pickling and re-selection

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