CN101624658A - Ferrotitanium concentrated ore direct reduction-magnetic separation deferrization technology - Google Patents
Ferrotitanium concentrated ore direct reduction-magnetic separation deferrization technology Download PDFInfo
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- CN101624658A CN101624658A CN200810045512A CN200810045512A CN101624658A CN 101624658 A CN101624658 A CN 101624658A CN 200810045512 A CN200810045512 A CN 200810045512A CN 200810045512 A CN200810045512 A CN 200810045512A CN 101624658 A CN101624658 A CN 101624658A
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Abstract
The invention provides a novel chemical ore dressing method which is ferrotitanium concentrated ore direct reduction-magnetic separation deferrization technology. The method comprises the following steps that: ferric oxide of ferrotitanium concentrated ore powder is directly reduced by hydrogen gas, natural gas, manufactured coal gas, coke and coal powder, fuel oil, oil residue or other reducers at a temperature of between 950 and 1,200 DEG C so as to deoxidize the ferric oxide into solid iron; 2, the reduced concentrated ore is heated to the temperature of between 1,200 and 1,300 DEG C and subjected to strong stirring to agglomerate iron microparticles into iron sand and iron beans; and the iron sand and iron beans come out of a furnace and enter water and is quenched; 3, the cooled concentrated ore enters a ball mill to separate Fe-TiO2 residue; 4, the concentrated ore is subjected to ball milling and enters a magnetic separator to separate iron sand and titanium residue out; and 5, the titanium residue is obtained; and the residual iron is washed by FeCl3 to obtain high-titanium slag with TiO2 more than or equal to between 85 and 95 percent.
Description
(1) technical field
The invention provides a kind of chemical mineral processing technology, it is a ferrotitanium concentrated ore direct reduction-magnetic separation deferrization technology.
(2) background technology
Southwest Flos Bombacis Malabarici municipalization especially big vanadium titano-magnetite in river contains TiO
2Geologic reserve 8.98 hundred million t account for national titanium resource 〉=93%, account for global titanium resource 〉=59%.Go through the tackling of key scientific and technical problems of half a lifetime discipline, now raw ore can have been contained magnetite, vanadium iron ore deposit, ilmenite three big components and reclaim through the ore dressing high efficiency separation.To magnet, the refining of vanadium iron mining and metallurgy, comprehensive utilization all obtains high level, forms, and is forming huge economic benefit.Only select the deferrization of concentrated ilmenite powder, in order to the processing titanium dioxide, metal titanium and titanium compound still still do not have ideal technological breakthrough.Nearly 800,000 t of homemade titanium dioxide in 2007 have manufacturer production more than 70.Concentrated ilmenite deferrization still＞98% usefulness falls behind, pollutes big and " sulfuric acid process " the refractory reason.Though existing company, can, obtain the success of black sulfuric acid and iron powder with " sulfuric acid process " blowdown recycling.But investment is big, and is of poor benefits, the difficult popularization.
Obtain by the artificial deferrization of concentrated ilmenite and to contain TiO
2〉=85～95% work in-process are titanium slag, are rich titanium slag or artificial rutile again.Be the exhausted comprehensively golden red masonry processing system titanium dioxide of alternative resource, the desirable feedstock of metal titanium and other titanium compound.The present invention promptly is the novel method of raw material production titanium slag with the concentrated ilmenite powder.
With the concentrated ilmenite powder, be processed into titanium slag under less energy-consumption, low cost, the cleaner production, be to solve homemade ferrotianium aboundresources and contain TiO
2Grade is low, contains (CaO+MgO) impurity height, is difficult to break away from the basic way that " sulfuric acid process " pollutes refractory.Studied both at home and abroad and industrialized scheme many, salt acid system, high pressure salt acid system, ammonium chloride method or the like are arranged, but really suitable big suitability for industrialized production has only electric furnace smelting process a kind of.In recent years introduce several and produce the trial production of ten thousand t electrosmelting subtraction units per year, contain (CaO+MgO) 〉=6% because of climbing the ore deposit Ti-Fe concentrate fines, slag is strong basicity, and is extremely viscous, Fe-TiO
2Viscosity is big, and separation performance is poor, if add the shoddye agent, has increased cost, and the titanium slag grade is descended, and comprehensive process is brought difficulty.More important, electric furnace deferrization power consumption extra-high-speed, product contains TiO
2-ton, power consumption 2800～3200 degree, after the electricity consumption preferential policy, the electrosmelting deferrization has not had profit and can say except that the chemical fertilizer industry in whole nation cancellation last year, difficult development.
China's concentrated ilmenite deferrization must be innovated the road in addition!
This invention people once learned steel-making, and " modern times of sponge iron are smelted method " joint is arranged on nineteen fifty-nine version " steelmaking theory " textbook, emphasized low-temperature reduction between 950～1200 ℃, made the ferric oxide deoxidation become solid-state spongy pure iron, can not inhale carbon.Can avoid 〉=iron becomes Fe because of inhaling carbon 1200 ℃ the time
3C and pure iron on every side constitute the pig iron of 1140 ℃ of minimum fusing points.Before coming out of the stove, stir down between reheat to 1200～1300 ℃, to impel the irony particulate to reunite and grow up into crude iron sand, water quick cooling is gone in the back of coming out of the stove, and makes iron and TiO at once
2Slag produces the crack because of the coefficient of expansion differs greatly, and after ball milling, makes to be dissociated into monomer, crosses magnetic separation and tells abrasive grit and TiO
2Slag.This article particularly points out: also might utilize this method to smelt for the iron ore that contains a large amount of chromium or titanium.---it has pointed out direction for the present invention.Once read in World War II when " mass movement to make iron and steel ", the Japanese is at the report of crossing spongy abrasive grit towards the scale operation of using fresh herb direct-reduction process.In the nineteen eighty-three version, The former Russian scholar ME. ripple is appointed etc. under 439 pages in work " inorganic salt technology " volume two the 40th chapter " product of the high temperature oxidation of ore " chapter in " method of ilmenite deferrization " chapter, just speak of direct reducing iron oxides and become pure iron, remove TiO with magnetic separation method
2The description of the iron in the slag.But only mention principle, valuable industry report is not found in the general introduction of several crosses so far as yet, and not seeing has the relevant patent disclosure consistent with this law.
(3) summary of the invention
Content of the present invention is:
1, concentrated ilmenite powder usefulness hydrogen or Sweet natural gas, manufactured gas, also available coke powder, conny, fuel oil, the dregs of fat are made reductive agent, go into stove (fluidizing furnace, rotary kiln or other stove all can), controlled temperature directly is reduced into solid-state sponge iron and TiO between 950～1200 ℃
2Slag.
2, the reduction honest material is heated to before coming out of the stove between 1200～1300 ℃, makes iron granules and TiO under the strong mixing
2Slag is come out of the stove into water quick cooling after reunion is grown up respectively.
3, pull the water-cooled material out and make abrasive grit and TiO through abundant ball milling
2Slag is divided into monomer.
4, the ball milling honest material is crossed magnetic separator, tells iron sand and TiO
2Slag is to iron-TiO
2The material that is difficult for branch returns reheat in 1200～1300 ℃ of stoves, stir process.
5, obtain TiO
2Slag is to contain FeCl
3Behind the oxide compounds such as the residual iron of aqueous solution eccysis and dissolving Mg, Ca, Al, it is moisture that water rinse dries, and warm air drying obtains the titanium slag product, contains TiO
2〉=85～95% is major product.The wash water oxidation regeneration is not given unnecessary details.
(4) technology implementation
Technology implementation:
1, according to west, river actual conditions, select Sweet natural gas to make reductive agent the best.Because of easily precisely control of furnace temperature, reaction is fast, efficient is high, cost is low with double-deck fluidizing furnace for reduction furnace, energy-conservation, after the blow-on with breeze (very thin-200 purposes, mostly can-350 orders) by the furnace roof input, be preheating to 750 ± 50 ℃ at top layer, crystal grain is beneficial to reduction reaction transition simultaneously, approximately the top layer preheating is 40 minutes, fluidized bed on earth under the preheating material, the boiling reduction is 80～90 minutes under 1050 ± 50 ℃ of optimum tempss, furnace temperature＜1000 ℃, react too slow, the easily sticking furnace wall in furnace temperature 〉=1100 ℃, breeze, all bad; The reduction honest material goes out fluidizing furnace and goes into 1200-1300 ℃ of following strong mixing 2h of short type rotary kiln heating, the entry of coming out of the stove.
2, by picking up furnace charge in the water, go into ball mill, ball milling 40～60 minutes is observed Fe-TiO
2Fundamental solution from, but blowing is gone into magnetic separator, isolates iron sand and TiO
2Slag is to Fe-TiO
2Separate bad " raw material " and return short rotary kiln heated and stirred processing.
3, get TiO
2Slag is again with 1～1.5mol/lFeCl
3The residual iron of aqueous solution flush away, the oxide compound of Ca, Mg, Al etc. is also dissolved simultaneously, cleans deferrization TiO
2Slag dries, and warm air drying is for containing TiO
2〉=85～95% titanium slag product, iron sand are by-product.FeCl
3More recyclable Fe (OH) is handled in wash water, air blast
3, solution circulated usefulness, salt accumulation such as Mg, Ca, Al should be extracted the part Separation and Recovery in the circulation, and old technology is not given unnecessary details.
4, climb Ti-Fe concentrate fines ore deposit, ore deposit, belong to the primitive rock ore deposit, granularity-200 ,-350 order persons occupy the majority average T iO
247%, FeO33.5%, Fe
2O
38.2%, (CaO+MgO) 〉=6% and SiO
2, Al
2O
3Deng,
Reduction main reaction: 3FeO+CH
4=3Fe+2H
2O+CO-67 kilocalorie/mole
Fe
2O
3+ CH
4=2Fe+2H
2O+CO-72.9 kilocalorie/mole
TiO in the ore deposit
2, SiO
2, Al
2O
3, CaO, MgO can be reduced can be considered zero, then every t only has in the ore deposit～6.2 kilomol O atoms need reduction, then the reduction of 1t ore deposit is with Sweet natural gas 54Nm in theory
3(Sweet natural gas contains CH with regard to much of that
490%) reduction reaction heat absorption＜140,000 kilocalories/t, 20Nm
3Sweet natural gas is much of that, but furnace gas, furnace charge take away heat, furnace wall heat radiation or the like actual heat dissipation be reaction theory need heat 3-4 doubly more than, the few point of big, the advanced real heat dissipation of stove, on the contrary just high.Modern with the double-deck boiling of 3.5t/h production capacity furnace gauge, Sweet natural gas 220-240Nm need be consumed in ore deposit per ton
3, wherein participating in reduction reaction must be about 1/4, and burning person 30%, and the Sweet natural gas of making to strengthen reductibility that do not burn accounts for 45%, combustible gas composition: CO in the furnace exhaust gas
2〉=2: 1, just enough reducing atmospheres can be arranged, above-mentioned ore deposit consumption air 600Nm per ton
3This stove produces tail gas, after the dedusting, feeds the boiler reignition, but producing steam, and scale is big, can be for generating, recyclable half many combustion gas heat energy.
5, climb the ore deposit concentrated ilmenite and include TiO
2With (FeO+Fe
2O
3) and Al, Mg, Ca oxide compound, be molecular level concretion, especially TiO
2With ferriferous oxide, mol ratio is almost 1, and high dispersing after the reduction, only is heated to 1200-1300 ℃, in fast molten again strong mixing when tip-off is long, bumps repeatedly and pounds, and little Fe grain is assembled grown up TiO
2Also concentrated relatively, after the Quench, temperature great change, Fe-TiO
2The difference of the coefficient of expansion enlarges, produce the crack, the crack is enlarged, be divided into monomer through ball milling, just but magnetic separates, so boiling upper strata preheating, crystal formation change (placer need not crystal conversion), the solid state reduction Cheng Tie of lower floor, go out fluidizing furnace and go into rotary kiln 1200-1300 ℃ of following strong mixing and make Fe-TiO
2Reunite relatively respectively and grow up, arrive water Quench, ball milling, magnetic separation, reasonable step by step, a step can not be lacked, and is the classical work of the present invention, characteristic.
6, make reductive agent with hydrogen, Sweet natural gas, do not bring impurity into, than with burnt, coal is guaranteed qualitatively, and is more expensive on the price, the one, regain when heat energy can be gone into the boiler reignition mostly, go into the stove air with the tail gas sensible heat through the interchanger preheating in addition, can reduce energy consumption 10～15%.Because of having lacked coal ash than coal tar to the quality of titanium slag, the negative impact of iron sand quality, titanium slag, iron sand thereby can oversold money count carefully and, with per hour 3.5t ilmenite this law deferrization, can attached product 1t iron sand, and product 1.6～1.7t contains TiO
2≈ 90% titanium slag is sold the recoverable Sweet natural gas of 1t iron sand, electricity consumption, is torn expenses such as old, artificial open, and a surplus is still arranged, and 90% sells titanium slag at market price, the profit tax near half, electricity consumption is electric furnace process about 1/14 only, advantage is the difficult ratio of each method in the past, and is significant.
Claims (6)
1, select Sweet natural gas to make reductive agent.Because of easily precisely control of furnace temperature, reaction is fast, efficient is high, cost is low with double-deck fluidizing furnace for reduction furnace, energy-conservation, after the blow-on with breeze (very thin-200 purposes, mostly can-350 orders) by the furnace roof input, be preheating to 750 ± 50 ℃ at top layer, crystal grain is beneficial to reduction reaction transition simultaneously, approximately the top layer preheating is 40 minutes, fluidized bed on earth under the preheating material, the boiling reduction is 80～90 minutes under 1050 ± 50 ℃ of optimum tempss, furnace temperature＜1000 ℃, react too slow, the easily sticking furnace wall in furnace temperature 〉=1100 ℃, breeze, all bad; The reduction honest material goes out fluidizing furnace and goes into 1200-1300 ℃ of following strong mixing 2h of short type rotary kiln heating, the entry of coming out of the stove.
2, by picking up furnace charge in the water, go into ball mill, ball milling 40～60 minutes is observed Fe-TiO
2Fundamental solution from, but blowing is gone into magnetic separator, isolates iron sand and TiO
2Slag is to Fe-TiO
2Separate bad " raw material " and return short rotary kiln heated and stirred processing.
3, get TiO
2Slag is again with 1～1.5mol/1FeCl
3The residual iron of aqueous solution flush away, the oxide compound of Ca, Mg, Al etc. is also dissolved simultaneously, cleans deferrization TiO
2Slag dries, and warm air drying is for containing TiO
2〉=85～95% titanium slag product, iron sand are by-product.FeCl
3More recyclable Fe (OH) is handled in wash water, air blast
3, solution circulated usefulness, salt accumulation such as Mg, Ca, Al should be extracted the part Separation and Recovery in the circulation, and old technology is not given unnecessary details.
4, climb Ti-Fe concentrate fines ore deposit, ore deposit, belong to the primitive rock ore deposit, granularity-200 ,-350 order persons occupy the majority average T iO
247%, FeO33.5%, Fe
2O
38.2%, (CaO+MgO) 〉=6% and SiO
2, Al
2O
3Deng,
Reduction main reaction: 3FeO+CH
4=3Fe+2H
2O+CO-67 kilocalorie/mole
Fe
2O
3+ CH
4=2Fe+2H
2O+CO-72.9 kilocalorie/mole
TiO in the ore deposit
2, SiO
2, Al
2O
3, CaO, MgO can be reduced can be considered zero, then every t only has in the ore deposit～6.2 kilomol O atoms need reduction, then the reduction of 1t ore deposit is with Sweet natural gas 54Nm in theory
3(Sweet natural gas contains CH with regard to much of that
490%) reduction reaction heat absorption＜140,000 kilocalories/t, 20Nm
3Sweet natural gas is much of that, but furnace gas, furnace charge take away heat, furnace wall heat radiation or the like actual heat dissipation be reaction theory need heat 3-4 doubly more than, the few point of big, the advanced real heat dissipation of stove, on the contrary just high.Modern with the double-deck boiling of 3.5t/h production capacity furnace gauge, Sweet natural gas 220-240Nm need be consumed in ore deposit per ton
3, wherein participating in reduction reaction must be about 1/4, and burning person 30%, and the Sweet natural gas of making to strengthen reductibility that do not burn accounts for 45%, combustible gas composition: CO in the furnace exhaust gas
2〉=2: 1, just enough reducing atmospheres can be arranged, above-mentioned ore deposit consumption air 600Nm per ton
3This stove produces tail gas, after the dedusting, feeds the boiler reignition, but producing steam, and scale is big, can be for generating, recyclable half many combustion gas heat energy.
5, climb the ore deposit concentrated ilmenite and include TiO
2With (FeO+Fe
2O
3) and Al, Mg, Ca oxide compound, be molecular level concretion, especially TiO
2With ferriferous oxide, mol ratio is almost 1, and high dispersing after the reduction, only is heated to 1200-1300 ℃, in fast molten again strong mixing when tip-off is long, bumps repeatedly and pounds, and little Fe grain is assembled grown up TiO
2Also concentrated relatively, after the Quench, temperature great change, Fe-TiO
2The difference of the coefficient of expansion enlarges, produce the crack, the crack is enlarged, be divided into monomer through ball milling, just but magnetic separates, so boiling upper strata preheating, crystal formation change (placer need not crystal conversion), the solid state reduction Cheng Tie of lower floor, go out fluidizing furnace and go into rotary kiln 1200-1300 ℃ of following strong mixing and make Fe-TiO
2Reunite relatively respectively and grow up, arrive water Quench, ball milling, magnetic separation, reasonable step by step, a step can not be lacked.
6, make reductive agent with hydrogen, Sweet natural gas, do not bring impurity into, than with burnt, coal is guaranteed qualitatively, and is more expensive on the price, the one, regain when heat energy can be gone into the boiler reignition mostly, go into the stove air with the tail gas sensible heat through the interchanger preheating in addition, can reduce energy consumption 10～15%.Because of having lacked coal ash than coal tar to the quality of titanium slag, the negative impact of iron sand quality, titanium slag, iron sand thereby can oversold money count carefully and, and per hour 3.5t ilmenite this law deferrization can attached product 1t iron sand, and product 1.6～1.7t contains TiO
2≈ 90% titanium slag is sold the recoverable Sweet natural gas of 1t iron sand, electricity consumption, is torn expenses such as old, artificial open, and a surplus is still arranged, and 90% sells titanium slag at market price, the profit tax near half, electricity consumption is electric furnace process about 1/14 only.
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|---|---|---|---|
| CN200810045512A CN101624658A (en) | 2008-07-10 | 2008-07-10 | Ferrotitanium concentrated ore direct reduction-magnetic separation deferrization technology |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430472A (en) * | 2011-12-26 | 2012-05-02 | 东北大学 | Direct reduction-magnetic separation method of vanadium titanomagnetite |
| CN102531048A (en) * | 2012-02-22 | 2012-07-04 | 山东东佳集团股份有限公司 | Method for preparing acid-soluble titanium slag by reduction at low temperature |
| CN102676796A (en) * | 2012-05-23 | 2012-09-19 | 北京矿冶研究总院 | Method for processing vanadium titano-magnetite |
| CN104694810A (en) * | 2015-02-06 | 2015-06-10 | 铜陵百荣新型材料铸件有限公司 | Method for preparing ferrotitanium alloy from ilmenite |
| CN107999255A (en) * | 2017-12-05 | 2018-05-08 | 连云港隆和矿产有限公司 | A kind of efficiently water process garnet filtrate production technology |
| CN108212509A (en) * | 2018-01-16 | 2018-06-29 | 东北大学 | Titanium vanadium mineral separation beneficiation method in a kind of hematite-limonite of titaniferous vanadium |
| CN112548312A (en) * | 2020-12-01 | 2021-03-26 | 昆山万洲特种焊接有限公司 | Method for removing residual welded material on surface of welding tool by using temperature difference |
| CN113355118A (en) * | 2021-06-04 | 2021-09-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of iron coke for titanium slag smelting and iron coke |
-
2008
- 2008-07-10 CN CN200810045512A patent/CN101624658A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430472A (en) * | 2011-12-26 | 2012-05-02 | 东北大学 | Direct reduction-magnetic separation method of vanadium titanomagnetite |
| CN102531048A (en) * | 2012-02-22 | 2012-07-04 | 山东东佳集团股份有限公司 | Method for preparing acid-soluble titanium slag by reduction at low temperature |
| CN102676796A (en) * | 2012-05-23 | 2012-09-19 | 北京矿冶研究总院 | Method for processing vanadium titano-magnetite |
| CN102676796B (en) * | 2012-05-23 | 2014-11-12 | 北京矿冶研究总院 | Method for processing vanadium titano-magnetite |
| CN104694810A (en) * | 2015-02-06 | 2015-06-10 | 铜陵百荣新型材料铸件有限公司 | Method for preparing ferrotitanium alloy from ilmenite |
| CN104694810B (en) * | 2015-02-06 | 2017-01-25 | 铜陵百荣新型材料铸件有限公司 | Method for preparing ferrotitanium alloy from ilmenite |
| CN107999255A (en) * | 2017-12-05 | 2018-05-08 | 连云港隆和矿产有限公司 | A kind of efficiently water process garnet filtrate production technology |
| CN108212509A (en) * | 2018-01-16 | 2018-06-29 | 东北大学 | Titanium vanadium mineral separation beneficiation method in a kind of hematite-limonite of titaniferous vanadium |
| CN112548312A (en) * | 2020-12-01 | 2021-03-26 | 昆山万洲特种焊接有限公司 | Method for removing residual welded material on surface of welding tool by using temperature difference |
| CN113355118A (en) * | 2021-06-04 | 2021-09-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of iron coke for titanium slag smelting and iron coke |
| CN113355118B (en) * | 2021-06-04 | 2022-06-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of iron coke for titanium slag smelting and iron coke |
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Open date: 20100113 |