CN109666805A - A kind of ilmenite low-temperature reduction technique - Google Patents

A kind of ilmenite low-temperature reduction technique Download PDF

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Publication number
CN109666805A
CN109666805A CN201811589287.0A CN201811589287A CN109666805A CN 109666805 A CN109666805 A CN 109666805A CN 201811589287 A CN201811589287 A CN 201811589287A CN 109666805 A CN109666805 A CN 109666805A
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CN
China
Prior art keywords
ilmenite
magnetic separation
low
reduction technique
coal dust
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811589287.0A
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Chinese (zh)
Inventor
钟金根
董文
阎镇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hainan Haituo Mining Co Ltd
Hainan Wensheng New Material Science & Technology Co Ltd
Original Assignee
Hainan Haituo Mining Co Ltd
Hainan Wensheng New Material Science & Technology Co Ltd
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Publication date
Application filed by Hainan Haituo Mining Co Ltd, Hainan Wensheng New Material Science & Technology Co Ltd filed Critical Hainan Haituo Mining Co Ltd
Priority to CN201811589287.0A priority Critical patent/CN109666805A/en
Publication of CN109666805A publication Critical patent/CN109666805A/en
Pending legal-status Critical Current

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    • 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
    • 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
    • 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

Abstract

The present invention provides a kind of ilmenite low-temperature reduction technique, comprising the following steps: under normal temperature conditions, ilmenite and coal dust 5:1 in mass ratio~1.2 are mixed;Material is sent into rotary kiln or tunnel oven after mixing, firing coal-dust, is heated to 600 DEG C~700 DEG C 0.5~1h of reaction;After being cooled to room temperature after reaction, material after cooling is handled through gas flow sizing machine, and carries out magnetic separation twice, is carried out first time magnetic separation prior to 1000-2000Gs, is obtained titanium-containing magnet mine and tailing, and tailing is carried out second of magnetic separation then at 5000-8000Gs, obtains ilmenite concentrate.The present invention makees reducing agent under middle cryogenic conditions, using coal dust, using rotary kiln or tunnel oven, significantly improves the solubility of ilmenite, while improving TiO2Main content obtains titanium-containing magnet mine and high-quality ilmenite concentrate, reduces the production cost of titanium dioxide, improve the quality of titanium dioxide.

Description

A kind of ilmenite low-temperature reduction technique
Technical field
The present invention relates to ilmenite technical field, in particular to a kind of ilmenite low-temperature reduction technique.
Background technique
Ilmenite is the primary raw material for manufacturing titanium dioxide and titanium alloy, to consume ten thousand tons of 700-750 every year in China at present, Wherein most comes from beach placer.Beach placer is washed away by air and water flow for a long time, forms the big portion FeO of ilmenite molecule Divide and has been oxidized to Fe2O3, since the ilmenite after oxidation is difficult to dissolve, titanium dioxide enterprise will increase very big production cost, So there is ten thousand tons of 200-300 of ilmenite to overstock in warehouse every year.The country has a kind of facture to be called reduction titanium at present, It is carried out at 1100 DEG C of high temperature, the product of generation is easily reoxidized by air, and not only cost is very high, and produces a large amount of Metallic iron causes titanium dioxide industry not to be available.Therefore it is badly in need of a kind of ilmenite low-temperature reduction technique, solve above-mentioned technical problem.
Summary of the invention
For mirror with this, the present invention proposes a kind of ilmenite low-temperature reduction technique, solves above-mentioned technical problem.
The technical scheme of the present invention is realized as follows:
A kind of ilmenite low-temperature reduction technique, it is characterised in that: the following steps are included:
S1, mixing: under normal temperature conditions, ilmenite and coal dust 5:1 in mass ratio~1.2 are mixed;
S2, reaction: sending material into rotary kiln or tunnel oven after mixing, firing coal-dust, is heated to 600 DEG C~700 DEG C React 0.5~1h;
S3, separation: after being cooled to room temperature after reaction, material after cooling is handled through gas flow sizing machine, and carries out magnetic twice Choosing carries out first time magnetic separation prior to 1000-2000Gs, obtains titanium-containing magnet mine and tailing, and tailing is carried out then at 5000-8000Gs Second of magnetic separation, obtains ilmenite concentrate.
Preferably, the mass ratio that S1 step, ilmenite and coal dust are pressed is 5:1.
Preferably, S2 step is heated to 630 DEG C~650 DEG C.
Preferably, S3 step, the field strength of the first time magnetic separation are 1300-1500Gs;The field strength of second of magnetic separation is 6000-6500Gs。
Compared with prior art, the beneficial effects of the present invention are:
The present invention makees reducing agent under middle cryogenic conditions, using coal dust, using rotary kiln or tunnel oven, realizes in ilmenite Fe2O3It is reduced into FeO, significantly improves the solubility of ilmenite, while improving TiO2High-quality ilmenite concentrate is made in main content, reduces The production cost of titanium dioxide improves the quality of titanium dioxide.The quality that the present invention improves ilmenite under conditions of middle low temperature refers to Mark, the product for avoiding conventional high-temperature condition from handling are reoxidized and at high cost, and the ilmenite that the present invention is restored no longer is weighed New oxidation, has at low cost, stable product quality, and adaptable feature can significantly reduce the cost of downstream titanium dioxide user, mention The quality level of high entire titanium dioxide industry.
Specific embodiment
In order to be best understood from the technology of the present invention content, specific embodiment is provided below, the present invention is described further.
Experimental method used in the embodiment of the present invention is conventional method unless otherwise specified.
Material used in the embodiment of the present invention, reagent etc., are commercially available unless otherwise specified.
A kind of ilmenite low-temperature reduction technique, comprising the following steps:
S1, mixing: under normal temperature conditions, ilmenite and coal dust 5:1 in mass ratio~1.2 are mixed;
S2, reaction: equably sending material into rotary kiln or tunnel oven after mixing, in the another of rotary kiln or tunnel oven One end has one to light mouth, by lighting the coal dust of recycling, to being heated to 600 DEG C~700 DEG C in entire rotary kiln or tunnel oven 0.5~1h is reacted, material is slowly run to discharge end from feed end, and temperature also gradually rises, until at 500 DEG C or more, coal dust In part of coal and air in oxygen generate carbon monoxide, carbon monoxide immediately with the Fe in ilmenite2O3FeO is reduced into, Material is discharged after Carbon monoxide reduction from rotary kiln or tunnel oven discharge end;
S3, separation: reacting rear material is cooled to room temperature by cooling cylinder, in material after cooling containing part without The coal dust of burning is handled by gas flow sizing machine and separates coal dust, and titanium ore carries out magnetic separation twice in material, is first sent into magnetic separation Machine carries out first time magnetic separation under 1000-2000Gs magnetic field strength, obtains titanium-containing magnet mine and tailing, then by tailing in 5000- Second of magnetic separation is carried out under 8000Gs magnetic field strength, obtains high-quality ilmenite concentrate.
Embodiment 1
A kind of ilmenite low-temperature reduction technique, comprising the following steps:
S1, mixing: under normal temperature conditions, ilmenite and coal dust 5:1 in mass ratio are mixed;
S2, reaction: equably sending material into rotary kiln or tunnel oven after mixing, in the another of rotary kiln or tunnel oven One end has one to light mouth, by lighting the coal dust of recycling, to being heated to 600 DEG C~620 DEG C in entire rotary kiln or tunnel oven React 1h;
S3, separation: after reacting rear material is cooled to room temperature by cooling cylinder, in material after cooling not containing part Coal dust through burning is handled by gas flow sizing machine and separates coal dust, and titanium ore carries out magnetic separation twice in material, is first sent into magnetic It selects machine to carry out first time magnetic separation under 1000-1200Gs magnetic field strength, obtains titanium-containing magnet mine and tailing, then by tailing in 5000- Second of magnetic separation is carried out under 5500Gs magnetic field strength, obtains ilmenite concentrate.
Embodiment 2
A kind of ilmenite low-temperature reduction technique, comprising the following steps:
S1, mixing: under normal temperature conditions, ilmenite and coal dust 5:1.2 in mass ratio are mixed;
S2, reaction: equably sending material into rotary kiln or tunnel oven after mixing, in the another of rotary kiln or tunnel oven One end has one to light mouth, by lighting the coal dust of recycling, in entire rotary kiln or tunnel oven, is heated to 660 DEG C~700 DEG C React 1h;
S3, separation: after reacting rear material is cooled to room temperature by cooling cylinder, in material after cooling not containing part Coal dust through burning is handled by gas flow sizing machine and separates coal dust, and titanium ore carries out magnetic separation twice in material, is first sent into magnetic It selects machine to carry out first time magnetic separation under 1600-2000Gs magnetic field strength, obtains titanium-containing magnet mine and tailing, then by tailing in 7000- Second of magnetic separation is carried out under 8000Gs magnetic field strength, obtains ilmenite concentrate.
Embodiment 3
A kind of ilmenite low-temperature reduction technique, comprising the following steps:
S1, mixing: under normal temperature conditions, ilmenite and coal dust 5:1 in mass ratio are mixed;
S2, reaction: equably sending material into rotary kiln or tunnel oven after mixing, in the another of rotary kiln or tunnel oven One end has one to light mouth, by lighting the coal dust of recycling, in entire rotary kiln or tunnel oven, is heated to 630 DEG C~650 DEG C React 0.5h;
S3, separation: after reacting rear material is cooled to room temperature by cooling cylinder, in material after cooling not containing part Coal dust through burning is handled by gas flow sizing machine and separates coal dust, and titanium ore carries out magnetic separation twice in material, is first sent into magnetic It selects machine to carry out first time magnetic separation under 1300-1500Gs magnetic field strength, obtains titanium-containing magnet mine and tailing, then by tailing in 6000- Second of magnetic separation is carried out under 6500Gs magnetic field strength, obtains ilmenite concentrate.
Comparative example 1
The difference of this comparative example and embodiment 3 is, ilmenite and coal dust 5:0.8 in mass ratio.
Comparative example 2
The difference of this comparative example and embodiment 3 is, is heated to 1000 DEG C of reaction 1h.
Comparative example 3
The difference of this comparative example and embodiment 3 is that the field strength of first time magnetic separation is 2500-3500Gs;Second of magnetic separation Field strength be 4000-4500Gs.
Examples 1 to 3 and the obtained product of comparative example 1~3 are subjected to attribute test, and carried out pair with traditional preparation methods Than each component content is as follows in product:
TiO2 Fe2O3 FeO P
Embodiment 1 50.4% 5.8% 38.2% 0.024%
Embodiment 2 50.8% 5.6% 38.4% 0.024%
Embodiment 3 51.4% 5.2% 38.9% 0.024%
Comparative example 1 44.7% 18.7% 25.3% 0.023%
Comparative example 2 43.2% 21.5% 22.6% 0.025%
Comparative example 3 45.6% 16.9% 27.1% 0.024%
Conventional method 43.5% 23.0% 21.0% 0.025%
The above results show that the present invention under middle cryogenic conditions, makees reducing agent using coal dust, utilize rotary kiln or tunnel Kiln realizes the Fe in ilmenite2O3It is reduced into FeO, significantly improves the solubility of ilmenite, while improving TiO2Main content is made High-quality ilmenite concentrate reduces the production cost of titanium dioxide, improves the quality of titanium dioxide.The present invention improves under conditions of middle low temperature The quality index of ilmenite, the product for avoiding conventional high-temperature condition from handling are reoxidized and at high cost, what the present invention was restored Ilmenite is no longer reoxidized, and has at low cost, stable product quality, and adaptable feature can significantly reduce downstream titanium white The cost of powder user improves the quality level of entire titanium dioxide industry.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (4)

1. a kind of ilmenite low-temperature reduction technique, it is characterised in that: the following steps are included:
S1, mixing: under normal temperature conditions, ilmenite and coal dust 5:1 in mass ratio~1.2 are mixed;
S2, reaction: sending material into rotary kiln or tunnel oven after mixing, firing coal-dust, is heated to 600 DEG C~700 DEG C reactions 0.5~1h;
S3, separation: after being cooled to room temperature after reaction, material after cooling is handled through gas flow sizing machine, and carries out magnetic separation twice, first First time magnetic separation is carried out in 1000-2000Gs, obtains titanium-containing magnet mine and tailing, tailing is carried out second then at 5000-8000Gs Secondary magnetic separation, obtains ilmenite concentrate.
2. a kind of ilmenite low-temperature reduction technique as described in claim 1, it is characterised in that: S1 step, ilmenite and coal dust The mass ratio pressed is 5:1.
3. a kind of ilmenite low-temperature reduction technique as described in claim 1, it is characterised in that: S2 step, be heated to 630 DEG C~ 650℃。
4. a kind of ilmenite low-temperature reduction technique as described in claim 1, it is characterised in that: S3 step, the first time magnetic The field strength of choosing is 1300-1500Gs;The field strength of second of magnetic separation is 6000-6500Gs.
CN201811589287.0A 2018-12-25 2018-12-25 A kind of ilmenite low-temperature reduction technique Pending CN109666805A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112410539A (en) * 2020-10-30 2021-02-26 河南佰利联新材料有限公司 Method for sorting titanium middlings containing weak magnetic gangue minerals

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101758240A (en) * 2009-12-17 2010-06-30 李建国 Method for producing reduced ilmenite powder for welding rod through rotary kiln
CN102352433A (en) * 2011-10-20 2012-02-15 天津市宏远钛铁有限公司 Process for producing reduced titanium iron powder by rotary kiln
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
CN104651601A (en) * 2015-02-06 2015-05-27 天津市宏远钛铁有限公司 Process for producing reduced ilmenite for welding rod through microwave heating
CN106521139A (en) * 2017-01-05 2017-03-22 重庆大学 Method for preparing high titanium slag through low temperature reduction and separation of titanium-containing iron ore
CN106893856A (en) * 2017-03-28 2017-06-27 江苏省冶金设计院有限公司 Process the method and system of schreyerite
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
CN108251635A (en) * 2018-01-16 2018-07-06 东北大学 Titanium vanadium mineral separation beneficiation method in a kind of bloodstone of titaniferous vanadium

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101758240A (en) * 2009-12-17 2010-06-30 李建国 Method for producing reduced ilmenite powder for welding rod through rotary kiln
CN102352433A (en) * 2011-10-20 2012-02-15 天津市宏远钛铁有限公司 Process for producing reduced titanium iron powder by rotary kiln
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
CN104651601A (en) * 2015-02-06 2015-05-27 天津市宏远钛铁有限公司 Process for producing reduced ilmenite for welding rod through microwave heating
CN106521139A (en) * 2017-01-05 2017-03-22 重庆大学 Method for preparing high titanium slag through low temperature reduction and separation of titanium-containing iron ore
CN106893856A (en) * 2017-03-28 2017-06-27 江苏省冶金设计院有限公司 Process the method and system of schreyerite
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
CN108251635A (en) * 2018-01-16 2018-07-06 东北大学 Titanium vanadium mineral separation beneficiation method in a kind of bloodstone of titaniferous vanadium

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112410539A (en) * 2020-10-30 2021-02-26 河南佰利联新材料有限公司 Method for sorting titanium middlings containing weak magnetic gangue minerals

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