CN108246496A - A kind of ilmenite ores separation beneficiation method of titano-hematite - Google Patents

A kind of ilmenite ores separation beneficiation method of titano-hematite Download PDF

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Publication number
CN108246496A
CN108246496A CN201810039805.5A CN201810039805A CN108246496A CN 108246496 A CN108246496 A CN 108246496A CN 201810039805 A CN201810039805 A CN 201810039805A CN 108246496 A CN108246496 A CN 108246496A
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concentrate
magnetic
iron
titano
hematite
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李文博
韩跃新
李艳军
柳晓
董振海
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Northeastern University China
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Northeastern University China
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/02Magnetic separation acting directly on the substance being separated
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/005Pretreatment specially adapted for magnetic separation
    • B03C1/015Pretreatment specially adapted for magnetic separation by chemical treatment imparting magnetic properties to the material to be separated, e.g. roasting, reduction, oxidation
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1204Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
    • C22B34/1209Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag

Abstract

The present invention relates to a kind of ilmenite ores separation beneficiation methods of titano-hematite, belong to mineral manufacture field.A kind of ferrotianium separation beneficiation method of titano-hematite, the method includes following processing steps:Titano-hematite powder is subjected to high magnetic pre-selection under conditions of magnetic field intensity is 5000Gs~13000Gs, obtains ferrotianium mixed crude concentrate;Ferrotianium mixed crude concentrate under reducing atmosphere is roasted, 500~620 DEG C of calcination temperature, make the bloodstone of weak magnetic that reduction reaction occur and be changed into ferromagnetism iron mineral;Cooling, grinding;Product after grinding is subjected to low intensity magnetic separation under conditions of magnetic field intensity is 750~1600Gs, obtains low intensity magnetic separation concentrate and tailings.The advantages that the method for the invention has titanium recovery rate high, and iron recovery is high, and flowage structure is simple, and production efficiency is high, comprehensive at low cost, good economy performance, environment friendly and pollution-free, and resource can obtain efficient utilization.

Description

A kind of ilmenite ores separation beneficiation method of titano-hematite
Technical field
The present invention relates to a kind of ilmenite ores separation beneficiation methods of titano-hematite, belong to mineral manufacture field.
Background technology
Titanium and its alloy because with density is low, intensity is high, high temperature resistant and it is anticorrosive when characteristics due in space flight, aviation and national defence The fields of grade are used widely, but because its renewable is weaker, so with increasing of the titanium article industry to ilmenite concentrate demand It is long, carry out titanium resource recycling and research on utilization has important practical significance.Primary ore is substantially mineral intergrowth, have ilmenite, The different types such as titanomagnetite and haplotypite.At present, the raw material of Ti industry is mainly ilmenite, accounts for about World Titanium total resources 80% (press TiO2It calculates).At present, the research of the domestic bloodstone for titaniferous is less, not only due to China's titanium resource 95% For preservation in primary vanadium titano-magnetite ore, titano-hematite resource is less;Also as bloodstone density, specific susceptibility and Electric conductivity is closer to ilmenite, therefore, ilmenite is enriched with from iron selection tailings using gravity treatment, high intensity magnetic separation or electric separation technique When, bloodstone will also enter in titanium rougher concentration, this will can not only obtain efficiently separating for ferrotianium, also increase subsequent purification The difficulty of ilmenite.Even if in addition, in the mineral deposit of vanadium titano-magnetite type, also containing a small amount of bloodstone, it is being enriched with ferrotianium During ore deposit, this part bloodstone will also enter in ilmenite concentrate, reduce ilmenite concentrate grade.
Mining industry is resources industry, and is conventional industries, be now in reform and to Modern Mineral stride forward new history when Phase.There are still but will establish Mining Development new concept and could promote the sustainable development of mining industry for its Industry Foundation status.Certain The development of mineral resources technique of preparing can promote this mineral resources to generate larger economic benefit, push and itself sent out with related industry Exhibition and variation.This motive force is mainly technology and economy.The development of mining industry is in total economic development, main influence factor It is production cost, and technology is to influence the key factor of cost.It relies on scientific and technological advances in creative solution mineral processing industries Restrict the new issue of development, it becomes even more important.
Invention content
The present invention starts new approaches, selects to obtain titanium and iron together by ilmenite and bloodstone using high magnetic pre-selection technique Mixed crude concentrate, then mixed crude concentrate is subjected to reduction roasting in reduction roasting device, bloodstone therein is restored and is generated Ferromagnetism iron mineral obtains iron ore concentrate using low intensity magnetic separation, and low intensity magnetic separation tailing is ilmenite concentrate, it is achieved thereby that titanium mineral and iron Mineral efficiently separate, and realize the comprehensive utilization of resource, also reduce beneficiation cost, and environment friendly and pollution-free, are brought to society Certain economic benefit and environment protection significance.
The present invention provides a kind of bloodstone of titaniferous and sorts-iron mineral object inversion of phases-low intensity magnetic separation separation ilmenite ores in advance Beneficiation method, i.e., ilmenite and bloodstone are preferentially selected using high magnetic pre-selection technique, obtain the mixed of titanium mineral and iron mineral Rough concentrate is closed, reduction roasting then is carried out to pre-selection rough concentrate using calciner so that bloodstone therein is in reducing atmosphere Under, reduction reaction occurs and generates ferromagnetic magnetic iron ore or maghemite (γ-Fe2O3), then roasted product is subjected to low intensity magnetic separation, Magnetic separation of iron ore concentrate is obtained, and magnetic tailing is the ilmenite concentrate of weak magnetic.
A kind of ilmenite ores separation beneficiation method of titano-hematite, the method includes following processing steps:
Titano-hematite powder is subjected to high magnetic pre-selection under conditions of magnetic field intensity is 5000Gs~13000Gs, is obtained Ferrotianium mixed crude concentrate;Ferrotianium mixed crude concentrate is roasted under reducing atmosphere, 500~620 DEG C of calcination temperature makes weak Magnetic bloodstone occurs reduction reaction and is changed into ferromagnetism iron mineral;Cooling, grinding;By the product after grinding in magnetic field intensity To carry out low intensity magnetic separation under conditions of 750~1600Gs, weak magnetic separation iron concentrate and tailings are obtained.
It is 55%~65% to obtain weak magnetic separation iron concentrate Iron grade using the above method;Low intensity magnetic separation tailing as ilmenite concentrate, Its TiO2Grade is 39%~47%.The TiO2The rate of recovery >=55%, the rate of recovery >=80% of iron.
Heretofore described ferromagnetism iron mineral is Fe3O4Or γ-Fe2O3, or both mixing.
In the present invention, in reducing roasting process, mineral are under reducing agent atmosphere, bloodstone (Fe2O3) and reproducibility gas Body (such as CO) occurs reduction reaction and generates magnetic iron ore (Fe3O4) or maghemite (γ-Fe2O3).Therefore subsequent low intensity magnetic separation Operation can will be detached by the ferromagnetic iron mineral of bloodstone transformation generation and the titanium mineral of weak magnetic.Weak magnetic concentrate selection is iron essence Ore deposit, low intensity magnetic separation tailing are ilmenite concentrate.The method for separating of the present invention finally effectively realizes ilmenite ores separation.
The ilmenite ores separation beneficiation method of titano-hematite of the present invention, preferably described reducing atmosphere is by restoring Property gas and the gaseous mixture of inert gas provide, wherein, the volume ratio of reducing gas and inert gas is 1:9~1:1, total gas Flow is 0.01m3/ h~5m3/ h, the reducing gas are CO, H2Or both arbitrary proportion mixing.
Further, the inert gas is preferably nitrogen or argon gas, most preferably nitrogen.
The ilmenite ores separation beneficiation method of titano-hematite of the present invention, wherein, high magnetic pre-selection obtains ferrotianium and mixes Close rough concentrate TiO2Grade is that 11%~21%, TFe grades are 44%~56%.
The preferred technical solution of ilmenite ores separation beneficiation method one of titano-hematite of the present invention is, including under State processing step:
(1) titano-hematite is crushed, the particle that ore grinding to granularity is -0.074mm account for the 60wt.% of whole materials~ 90wt.%;
(2) levigate material is subjected to high magnetic pre-selection in intensity magnetic separator, magnetic field intensity is 5000Gs~13000Gs, obtains titanium Iron mixed crude concentrate;
(3) ferrotianium mixed crude concentrate is roasted in reduction roasting device, temperature is 500~620 DEG C, gaseous mixture total flow For 0.01m3/ h~5m3/ h makes the bloodstone of weak magnetic that reduction reaction occur and is changed into ferromagnetism iron mineral, and gaseous mixture is by restoring Property gas and inert gas by volume 1:9~1:1 composition;
(4) product of roasting is cooled down, the particle that ore grinding to granularity is -0.043mm account for the 62wt.% of whole materials~ 95wt.%;
(5) the ore grinding product after roasting is subjected to low intensity magnetic separation under conditions of magnetic field intensity is 750~1600Gs, obtained weak Magnetic concentrate and tailing, wherein weak magnetic concentrate selection Iron grade are 55%~65%;And low intensity magnetic separation tailing is as its TiO of ilmenite concentrate2 Grade is 39%~47%.
In above-mentioned technical proposal, in the step (3), calciner used in reduction roasting for tube furnace or it is industrial also Former roaster, using the recovery time of tube furnace for 5~25min, using the recovery time of industrial reduction roaster for 10~ 90s。
In above-mentioned technical proposal, in the step (3), first sample to be restored is put into calciner heat up it is pre- Heat after in-furnace temperature reaches desired temperature, is passed through inert gas replacement furnace air, continues to keep being somebody's turn to do after gas displacement Temperature is simultaneously passed through gaseous mixture in preset ratio.
Compared with prior art, the features of the present invention:The method of the present invention is then fired and also by high intensity magnetic separation preenrichment Former (low intensity magnetic separation bloodstone is converted into ferromagnetism iron mineral in reduction process), then carries out low intensity magnetic separation, sorts out iron ore concentrate, and weak Magnetic tailing is then ilmenite concentrate.It, not only can be effectively compared with traditional magnetic for titano-hematite floats dressing method again Realize ilmenite ores separation, and more high-grade ilmenite concentrate and iron ore concentrate can be obtained that there is titanium recovery rate height, iron recovery Height, flowage structure is simple, and production efficiency is high, and comprehensive at low cost, good economy performance, environment friendly and pollution-free, resource can obtain efficient utilization The advantages that.
Specific embodiment
Following non-limiting examples can make those of ordinary skill in the art be more fully understood the present invention, but not with Any mode limits the present invention.
Test method described in following embodiments is conventional method unless otherwise specified;The reagent and material, such as Without specified otherwise, commercially obtain.
Reduction roasting device employed in the embodiment of the present invention is two kinds, and one kind is laboratory tube roaster, separately One kind is industrial reduction roaster.
It is 5~25min the recovery times to be when in the embodiment of the present invention using laboratory tube furnace, is roasted using industrial reduction The recovery time is 10~90s when burning stove;
Reduction roasting uses carbon monoxide and nitrogen as industrial products purchased in market in the embodiment of the present invention.
Φ 180mm × 200mm tube ball mill ore grindings are used in the embodiment of the present invention.
It is sorted in the embodiment of the present invention using the magnetic separation after Φ 50mm magnetic separation tubes are roasted.
The background magnetic field intensity of magnetic separation tube is 750~1600Oe in the embodiment of the present invention.
Embodiment 1
The titano-hematite sample ore of use, TiO2Content is that 15.26%, TFe contents are 45.85%.
Method carries out according to the following steps:
(1) titano-hematite sample ore is crushed to granularity -2.0mm, and it is total that ore grinding to granularity is that the part of -0.074mm accounts for material The 80% of weight;
(2) material after ore grinding is taken, magnetic separation is carried out by the intensity magnetic separator under 8500Gs magnetic field intensities, obtains high magnetic pre-selection Rough concentrate;
(3) using laboratory tube roaster, high magnetic pre-selection rough concentrate is subjected to reduction roasting, calcination temperature is 560 DEG C, Gaseous mixture is by CO and nitrogen by volume 3:The gaseous mixture of 7 compositions, the total tolerance of gaseous mixture are 0.015m3/ h, during reduction roasting Between for 10min, make the bloodstone of weak magnetic that reduction reaction occur and be changed into ferromagnetism iron mineral;
(4) the levigate part to granularity for -0.043mm of product of roasting is accounted for the 85% of material total weight;
(5) by the ore grinding product after roasting under conditions of magnetic field intensity is 1070Gs, low intensity magnetic separation is carried out by magnetic separation tube, Low intensity magnetic separation concentrate and tailings are obtained, wherein weak magnetic concentrate selection Iron grade is 60.11%, iron recovery 85.20%;And low intensity magnetic separation Tailing is as its TiO of ilmenite concentrate2Grade is 45.83%, TiO2The rate of recovery is 57.34%.
Embodiment 2
The titano-hematite sample ore of use, TiO2Content is that 16.53%, TFe contents are 42.25%, the multielement of raw material Analysis result refers to table 1.
Table 1
Element Fe TiO2 SiO2 CaO MgO Al2O3 S P
Content/wt% 42.25 16.53 8.98 0.04 0.47 8.03 0.03 <0.01
Method carries out according to the following steps:
(1) titano-hematite is crushed to granularity -2.0mm, and ore grinding to granularity is that the part of -0.074mm accounts for material total weight 70%;
(2) material after ore grinding is taken, magnetic separation is carried out by the intensity magnetic separator under 7500Gs magnetic field intensities, obtains high magnetic pre-selection Rough concentrate;
(3) using suspension roaster, high magnetic pre-selection rough concentrate is subjected to reduction roasting, calcination temperature is 540 DEG C, gaseous mixture For by CO and nitrogen by volume 3.5:The gaseous mixture of 6.5 compositions, the total tolerance of gaseous mixture are 4m3/ h, reduction roasting time is 50s makes the bloodstone of weak magnetic that reduction reaction occur and is changed into ferromagnetism iron mineral;
(4) the levigate content to granularity for -0.043mm parts of product of roasting is accounted for the 75% of material total weight;
(5) by the ore grinding product after roasting under conditions of magnetic field intensity is 1320Gs, low intensity magnetic separation is carried out by magnetic separation tube, Low intensity magnetic separation concentrate and tailings are obtained, wherein weak magnetic concentrate selection Iron grade is 58.74%, iron recovery 88.23%;And low intensity magnetic separation Tailing is as its TiO of ilmenite concentrate2Grade is 45.13%, TiO2The rate of recovery is 63.04%.
Embodiment 3
The bloodstone sample ore of the titaniferous of use, wherein TiO2Content is that 13.11%, TFe contents are 48.82%.Method is pressed Following steps carry out:
(1) the bloodstone sample ore of titaniferous is crushed to granularity -2.0mm, and it is total that ore grinding to granularity for -0.074mm contents accounts for material The 75% of weight;
(2) material after ore grinding is taken, magnetic separation is carried out by the intensity magnetic separator under 8000Gs magnetic field intensities, obtains high magnetic pre-selection Rough concentrate;
(3) using laboratory tube roaster, high magnetic pre-selection rough concentrate is subjected to reduction roasting, calcination temperature is 580 DEG C, Gaseous mixture is by CO and nitrogen by volume 4:The gaseous mixture of 6 compositions, the total tolerance of gaseous mixture are 0.03m3/ h, reduction roasting time For 20min, make the bloodstone of weak magnetic that reduction reaction occur and be changed into ferromagnetism iron mineral;
(4) the 80% of material total weight is accounted for for -0.043mm contents to granularity by product of roasting is levigate;
(5) by the ore grinding product after roasting under conditions of magnetic field intensity is 770Gs, low intensity magnetic separation is carried out by magnetic separation tube, Low intensity magnetic separation concentrate and tailings are obtained, wherein weak magnetic concentrate selection Iron grade is 64.16%, iron recovery 84.75%;And low intensity magnetic separation Tailing is as its TiO of ilmenite concentrate2Grade is 44.21%, TiO2The rate of recovery is 58.98%.

Claims (8)

1. a kind of ilmenite ores separation beneficiation method of titano-hematite, it is characterised in that:The method includes following techniques steps Suddenly:
Titano-hematite powder is subjected to high magnetic pre-selection under conditions of magnetic field intensity is 5000Gs~13000Gs, obtains ferrotianium Mixed crude concentrate;Ferrotianium mixed crude concentrate is roasted under reducing atmosphere, 500~620 DEG C of calcination temperature makes weak magnetic Bloodstone occur reduction reaction be changed into ferromagnetism iron mineral;Cooling, grinding;It is in magnetic field intensity by the product after grinding Low intensity magnetic separation is carried out under conditions of 750~1600Gs, obtains weak magnetic separation iron concentrate and tailings.
2. according to the method described in claim 1, it is characterized in that:The weak magnetic separation iron concentrate Iron grade is 55%~65%; Low intensity magnetic separation tailing is as ilmenite concentrate, TiO2Grade is 39%~47%.
3. according to the method described in claim 1, it is characterized in that:The reducing atmosphere is by reducibility gas and indifferent gas The gaseous mixture of body provides, wherein, the volume ratio of reducing gas and inert gas is 1:9~1:1, total gas couette 0.01m3/h ~5m3/ h, the reducing gas are CO, H2Or both arbitrary proportion mixing.
4. according to the method described in claim 1, it is characterized in that:High magnetic pre-selection obtains ferrotianium mixed crude concentrate TiO2Grade It is 44%~56% for 11%~21%, TFe grades.
5. according to the method described in claim 1, it is characterized in that:Including following processing steps:
(1) titano-hematite is crushed, the particle that ore grinding to granularity is -0.074mm account for the 60wt.% of whole materials~ 90wt.%;
(2) levigate material is subjected to high magnetic pre-selection in intensity magnetic separator, magnetic field intensity is 5000Gs~13000Gs, obtains ferrotianium and mixes Close rough concentrate;
(3) ferrotianium mixed crude concentrate is roasted in reduction roasting device, temperature is 500~620 DEG C, and gaseous mixture total flow is 0.01m3/ h~5m3/ h makes the bloodstone of weak magnetic that reduction reaction occur and is changed into ferromagnetism iron mineral, and gaseous mixture is by reproducibility Gas and inert gas by volume 1:9~1:1 composition;
(4) product of roasting is cooled down, ore grinding to granularity is that the particle of -0.043mm accounts for 62wt.%~95wt.% of whole materials;
(5) the ore grinding product after roasting is subjected to low intensity magnetic separation under conditions of magnetic field intensity is 750~1600Gs, obtains low intensity magnetic separation Concentrate and tailings, wherein weak magnetic concentrate selection Iron grade are 55%~65%;And low intensity magnetic separation tailing is as its TiO of ilmenite concentrate2Grade It is 39%~47%.
6. according to the method described in claim 5, it is characterized in that:In the step (3), calciner is used in reduction roasting Tube furnace or industrial reduction roaster are 5~25min using the recovery time of tube furnace, use industrial reduction roasting The recovery time of stove is 10~90s.
7. according to the method described in claim 5, it is characterized in that:In the step (3), sample to be restored is first put into roasting Heating preheating is carried out in device, after in-furnace temperature reaches desired temperature, is passed through inert gas replacement furnace air, gas displacement After continue to keep the temperature and be passed through gaseous mixture in preset ratio.
8. according to the method described in claim 1, it is characterized in that:The TiO2The rate of recovery >=55%, the rate of recovery of iron >= 80%.
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CN109821650A (en) * 2019-02-15 2019-05-31 河北钢铁集团矿业有限公司 A kind of high silicon bloodstone tailing treatment technology
CN109967229A (en) * 2019-04-26 2019-07-05 广东省资源综合利用研究所 A kind of method that weathering type haplotypite containing vanadium selects smelting recycling vanadium ferrotianium
CN110292989A (en) * 2019-07-04 2019-10-01 广东省资源综合利用研究所 A kind of method of beach sand titanium rough concentrate ferrotianium separation upgrading
CN110935562A (en) * 2019-10-25 2020-03-31 中国地质科学院矿产综合利用研究所 Beneficiation method for separating iron and titanium of oxidized iron-titanium mixed ore
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CN109821650A (en) * 2019-02-15 2019-05-31 河北钢铁集团矿业有限公司 A kind of high silicon bloodstone tailing treatment technology
CN109967229A (en) * 2019-04-26 2019-07-05 广东省资源综合利用研究所 A kind of method that weathering type haplotypite containing vanadium selects smelting recycling vanadium ferrotianium
CN109967229B (en) * 2019-04-26 2020-08-25 广东省资源综合利用研究所 Method for recovering vanadium, titanium and iron from weathered vanadium, titanium and hematite
CN110292989A (en) * 2019-07-04 2019-10-01 广东省资源综合利用研究所 A kind of method of beach sand titanium rough concentrate ferrotianium separation upgrading
CN110935562A (en) * 2019-10-25 2020-03-31 中国地质科学院矿产综合利用研究所 Beneficiation method for separating iron and titanium of oxidized iron-titanium mixed ore
CN110935562B (en) * 2019-10-25 2022-07-05 中国地质科学院矿产综合利用研究所 Beneficiation method for separating iron and titanium of oxidized iron-titanium mixed ore
CN111298962A (en) * 2020-02-11 2020-06-19 广东工业大学 Method for improving magnetism of low-grade hematite
CN111286630A (en) * 2020-02-28 2020-06-16 东北大学 Method for removing impurities and purifying titanium concentrate through suspension roasting
CN111286630B (en) * 2020-02-28 2021-06-15 东北大学 Method for removing impurities and purifying titanium concentrate through suspension roasting
CN115478165A (en) * 2022-09-22 2022-12-16 郑州大学 Method for gradient resource utilization of red mud by low-temperature Bayer process
CN115478165B (en) * 2022-09-22 2023-10-03 郑州大学 Low-temperature Bayer process red mud cascade resource utilization method

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Application publication date: 20180706