CN101265521A - Method for preparing acid-soluble titanium slag by Panzhihua titanium concentrate - Google Patents

Method for preparing acid-soluble titanium slag by Panzhihua titanium concentrate Download PDF

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CN101265521A
CN101265521A CNA2008103010156A CN200810301015A CN101265521A CN 101265521 A CN101265521 A CN 101265521A CN A2008103010156 A CNA2008103010156 A CN A2008103010156A CN 200810301015 A CN200810301015 A CN 200810301015A CN 101265521 A CN101265521 A CN 101265521A
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titanium
concentrate
ball milling
reduction
magnetic
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梅卫东
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Abstract

The invention provides a method for preparing acid soluble titanium slag from Panzhihua titanium concentrate, which comprises the following steps of: (1) magnetically separating titanium concentrate; (2) mixing coke powder or coal powder with refined titanium concentrate; (3) ball milling; (4) reducing at 950-1,100 DEG C; (5) crushing; (6) ball milling; (7) magnetically separating; and (8) dewatering and drying magnetic substances (iron powder) and non-magnetic substances (acid soluble titanium slag). The inventive method processes titanium concentrate with ball milled powder, and the titanium concentrate deforms under mechanical force and takes place crystal lattice distortion to a large extent, so as to improve reactivity, reduce the initial reduction reaction temperature to allow titanium concentrate to be reduced at low temperature, prevent phase transformation from titanic iron ore to ferropseudobrookite, inhibit enrichment of impurities in ores such as magnesium oxide and manganese oxide, and control the reduction of titanium oxide to ensure iron crystal grain growth. The iron and titanium monomers in the reduction product are easily to be separated, and the titanium oxide content in the obtained titanium slag is over 775%.

Description

Method with preparing acid-soluble titanium slag by Panzhihua titanium concentrate
Technical field
The invention belongs to the titanium field of metallurgy, particularly relate to a kind of method of producing the acid-dissolved titanium slag that titanium dioxide uses with Flos Bombacis Malabarici ilmenite concentrate preparation.
Background technology
Use acid-dissolved titanium slag to make the raw material of sulfate process titanium dioxide, can omit ferric sulfate reduction and two operations of ferrous sulfate freezing and crystallizing in the titanium white technology, sour consumption in the minimizing process and three wastes quantity have low-cost and oligosaprobic effect.
At present the production way of titanium slag is use Smelting Ilmenite Concentrate in Electric Furnace, and the higher ilmenite concentrate of use rate of decay can be easy to produce titanium dioxide greater than 90% titanium slag.The Flos Bombacis Malabarici ilmenite concentrate belongs to the lower rock ore deposit of rate of decay, the content of magnesia height in the ilmenite concentrate, and content of titanium dioxide is low, and when using electrosmelting, magnesium oxide enrichment in the slag makes the slag melting point height of generation, and viscosity is big, the difficulty of slagging tap, the production difficulty is big.Thereby the Flos Bombacis Malabarici ilmenite concentrate should not be selected to produce titanium slag with electric furnace smelting method.
The Flos Bombacis Malabarici ilmenite concentrate is handled with directly reduction, the isolating method of magnetic separation, its operational path that adopts is: make reductive agent with coke powder, it is titanium slag that ilmenite concentrate adds reductive agent batch mixing-tinning-tunnel kiln reduction-reducing material fragmentation-ore grinding-magnetic separation-obtain nonmagnetics, the magnetic thing is an iron powder, reduction temperature is 1280 ℃, soaking time 16 hours.But it is bad that this technology iron, titanium separate, and the degree of metalization of reduction ilmenite concentrate is lower, and the nonmagnetics grade of titanium dioxide after the magnetic separation is low, and total iron of magnetic thing is low, and the content of titanium dioxide of gained titanium slag is only between 67%-71%.
Ilmenite concentrate reduces in the temperature more than 1200 ℃, can obtain higher reduction degree, but the time occur still 1280 ℃ of reduction that degree of metalization is low to separate bad phenomenon with iron, titanium, its reason is: 1) ilmenite concentrate is greater than 1180 ℃ of reduction the time, ilmenite in the concentrate changes ferrous brookite phase mutually into, and the iron in the ferrous brookite can not be reduced fully; 2) under the condition of high temperature, profile of impurities such as the magnesium oxide in the ilmenite concentrate, silicon-dioxide, Manganse Dioxide can change, and are enriched in the interface of reactant, form one deck barrier, hinder the diffusion of reactant, and also just having hindered reduction reaction carries out smoothly; 3) temperature of reaction is greater than 1200 ℃, and outside deironing was reduced, titanium dioxide also was reduced, and generates carbon nitrogen oxygen titanium, and reductive iron crystal grain and carbon nitrogen oxygen titanium crystal grain are grown up simultaneously, produce chimeric mutually, parcel, make magnetic separation be difficult to iron, titanium monomer separation are come out.
Therefore, the characteristics of Flos Bombacis Malabarici ilmenite concentrate and the ilmenite phase transformation law in reduction process has determined to adopt traditional direct reduction, and magnetic separation separation way is produced acid-dissolved titanium slag and had some difficulties.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method with preparing acid-soluble titanium slag by Panzhihua titanium concentrate, and the content of titanium dioxide of the titanium slag that this method obtains is greater than 75%.
The technical scheme that technical solution problem of the present invention is adopted is: with the method for preparing acid-soluble titanium slag by Panzhihua titanium concentrate, this method may further comprise the steps:
1) ilmenite concentrate magnetic separation obtains refining ilmenite concentrate;
2) getting the coke powder of refining ilmenite concentrate weight 20%-30% or coal dust and refining ilmenite concentrate mixes;
3) with the material ball milling behind the mixing, abrasive grain is less than 400 orders;
4) material behind the ball milling is packed into retort is sent into the reduction furnace reduction, and reduction temperature is 950 ℃-1100 ℃, behind the furnace cooling to 750 ℃, and the cooling of coming out of the stove;
5) take out material, be broken into the following piece material of 30mm;
6) the piece material is sent into the wet-type ball mill ball milling, make raw meal particle size less than 200 orders;
7) slip behind the ball milling is introduced the magnetic separator magnetic separation;
8) collect magnetic thing and nonmagnetics after the magnetic separation respectively;
9) respectively to magnetic thing and nonmagnetics dehydration, the nonmagnetics drying, the magnetic thing is dry under the protective atmosphere condition, and the nonmagnetics that obtains is an acid-dissolved titanium slag, and the magnetic thing is an iron powder.
Beneficial effect of the present invention: the present invention adopts the ball milling powder to handle ilmenite concentrate, concentrate deforms under mechanical force, produces a large amount of rugged changes of lattice, has improved reactive behavior, reduced the beginning temperature of reduction reaction, made ilmenite concentrate that reduction reaction take place when low temperature; The present invention is lower than reduced iron under 1100 ℃ the cold condition in temperature, avoid ilmenite to be transformed into ferrous brookite phase mutually, suppress impurity enriched such as magnesium oxide, manganese oxide in the mineral, the control titanium dioxide, make the iron grain growth, iron in the reduzate, the easy monomer separation of titanium, the content of titanium dioxide of the titanium slag that obtains is greater than 75%.
Embodiment
Embodiment 1:
1) get 500kg Flos Bombacis Malabarici ilmenite concentrate, granularity is the natural particle size that dispatches from the factory, and uses the dry-type magnetic extractor magnetic separation, obtains 95% refining ilmenite concentrate and 5% mine tailing;
2) get the coke powder and the refining ilmenite concentrate mixing and stirring made from extra care ilmenite concentrate amount 20%;
3) the material adding ball mill with mixing carries out ball milling, and 1 hour ball milling time, abrasive grain is less than 45 orders;
4) the ball milling material is packed into retort is gone into stove 950 ℃ of insulations 4 hours, furnace cooling to 750 cooling fast of ℃ coming out of the stove;
5) take out reducing material, be broken into the following piece material of 30mm;
6) the piece material was sent into the wet-type ball mill ball milling 1 hour, made raw meal particle size less than 200 orders;
7) the ball milling slip is introduced the magnetic separator magnetic separation;
8) magnetic thing and the nonmagnetics after the collection magnetic separation;
9) respectively to the dehydration of magnetic separation product, the nonmagnetics drying, the magnetic thing is dry under the protective atmosphere condition, and the nonmagnetics that obtains is an acid-dissolved titanium slag, and the magnetic thing is for paying the product iron powder.
The titanium slag content of titanium dioxide that obtains is greater than 75%, and granularity is the natural particle size behind the abrasive material, the suitable raw material of doing the acid system titanium white production.
Embodiment 2:
1) get 500kg Flos Bombacis Malabarici ilmenite concentrate, granularity is the natural particle size that dispatches from the factory, and uses the dry-type magnetic extractor magnetic separation, obtains 95% refining ilmenite concentrate and 5% mine tailing;
2) get the coal dust and the refining ilmenite concentrate mixing and stirring made from extra care ilmenite concentrate amount 25%;
3) the material adding ball mill with mixing carries out ball milling, and 2 hours ball milling time, abrasive grain is less than 30 orders;
4) the ball milling material is packed into retort is gone into stove 1000 ℃ of insulations 5 hours, furnace cooling to 750 cooling fast of ℃ coming out of the stove;
5) take out reducing material, be broken into the following piece material of 30mm;
6) the piece material was sent into the wet-type ball mill ball milling 1.5 hours, made raw meal particle size less than 200 orders;
7) the ball milling slip is introduced the magnetic separator magnetic separation;
8) magnetic thing and the nonmagnetics after the collection magnetic separation;
9) respectively to the dehydration of magnetic separation product, the nonmagnetics drying, the magnetic thing is dry under the protective atmosphere condition, and the nonmagnetics that obtains is an acid-dissolved titanium slag, and the magnetic thing is for paying the product iron powder.
The content of titanium dioxide of the titanium slag that obtains is greater than 75%, and granularity is the natural particle size behind the abrasive material, the suitable raw material of doing the acid system titanium white production.
Embodiment 3:
1) get 500kg Flos Bombacis Malabarici ilmenite concentrate, granularity is the natural particle size that dispatches from the factory, and uses the dry-type magnetic extractor magnetic separation, obtains 95% refining ilmenite concentrate and 5% mine tailing;
2) get the coke powder and the refining ilmenite concentrate mixing and stirring made from extra care ilmenite concentrate amount 30%;
3) the material adding ball mill with mixing carries out ball milling, and 3 hours ball milling time, abrasive grain is less than 20 orders.
4) the ball milling material is packed into retort is gone into stove 1100 ℃ of insulations 5 hours, furnace cooling to 750 cooling fast of ℃ coming out of the stove;
5) take out reducing material, be broken into the following piece material of 30mm;
6) the piece material was sent into the wet-type ball mill ball milling 2 hours, made raw meal particle size less than 200 orders;
7) the ball milling slip is introduced the magnetic separator magnetic separation;
8) magnetic thing and the nonmagnetics after the collection magnetic separation;
9) respectively to the dehydration of magnetic separation product, the nonmagnetics drying, the magnetic thing is dry under the protective atmosphere condition, and the nonmagnetics that obtains is an acid-dissolved titanium slag, and the magnetic thing is for paying the product iron powder.
The titanium slag content of titanium dioxide that obtains is greater than 75%, and granularity is the natural particle size behind the abrasive material, the suitable raw material of doing the acid system titanium white production.

Claims (2)

1. with the method for preparing acid-soluble titanium slag by Panzhihua titanium concentrate, it is characterized in that this method may further comprise the steps:
1) ilmenite concentrate magnetic separation obtains refining ilmenite concentrate;
2) getting the coke powder of refining ilmenite concentrate weight 20%-30% or coal dust and refining ilmenite concentrate mixes;
3) with the material ball milling behind the mixing, abrasive grain is less than 400 orders;
4) material behind the ball milling is packed into retort is sent into the reduction furnace reduction, and reduction temperature is 950 ℃-100 ℃, behind the furnace cooling to 750 ℃, and the cooling of coming out of the stove;
5) take out material, be broken into the following piece material of 30mm;
6) the piece material is sent into the wet-type ball mill ball milling, make raw meal particle size less than 200 orders;
7) slip behind the ball milling is introduced the magnetic separator magnetic separation;
8) collect magnetic thing and nonmagnetics after the magnetic separation respectively;
9) respectively to magnetic thing and nonmagnetics dehydration, the nonmagnetics drying, the magnetic thing is dry under the protective atmosphere condition, and the nonmagnetics that obtains is an acid-dissolved titanium slag, and the magnetic thing is an iron powder.
2. the method with preparing acid-soluble titanium slag by Panzhihua titanium concentrate as claimed in claim 1 is characterized in that step 4 is: with the retort of packing into of the material behind the ball milling, send into the reduction furnace reduction, reduction temperature is 950 ℃-100 ℃, behind the furnace cooling to 750 ℃, and the cooling of coming out of the stove.
CNA2008103010156A 2008-04-10 2008-04-10 Method for preparing acid-soluble titanium slag by Panzhihua titanium concentrate Pending CN101265521A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104611495A (en) * 2014-06-27 2015-05-13 冯志权 Method for preparation of titanium slag by tunnel kiln
CN106115778A (en) * 2016-06-29 2016-11-16 四川龙蟒钛业股份有限公司 The recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag
CN108384948A (en) * 2018-03-29 2018-08-10 唐竹胜 A kind of method that low temperature depth slag sluicing system quickly restores ilmenite concentrate sorting high titanium slag and acid-dissolved titanium slag
CN108998656A (en) * 2018-08-29 2018-12-14 攀钢集团攀枝花钢铁研究院有限公司 Titanium slag preparation method
CN109022773A (en) * 2018-08-28 2018-12-18 河钢股份有限公司承德分公司 A kind of method of comprehensive utilzation ilmenite concentrate
CN109097600A (en) * 2018-09-12 2018-12-28 攀钢集团攀枝花钢铁研究院有限公司 It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide
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
CN112960692A (en) * 2021-04-13 2021-06-15 攀钢集团攀枝花钢铁研究院有限公司 Production method of titanium raw material for sulfate process titanium dioxide
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
CN113462842A (en) * 2021-05-31 2021-10-01 钢研晟华科技股份有限公司 Method for preparing high-titanium slag powder and metal iron powder by reducing ilmenite concentrate powder at low temperature

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104611495A (en) * 2014-06-27 2015-05-13 冯志权 Method for preparation of titanium slag by tunnel kiln
CN106115778A (en) * 2016-06-29 2016-11-16 四川龙蟒钛业股份有限公司 The recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag
CN108384948A (en) * 2018-03-29 2018-08-10 唐竹胜 A kind of method that low temperature depth slag sluicing system quickly restores ilmenite concentrate sorting high titanium slag and acid-dissolved titanium slag
CN109022773A (en) * 2018-08-28 2018-12-18 河钢股份有限公司承德分公司 A kind of method of comprehensive utilzation ilmenite concentrate
CN108998656A (en) * 2018-08-29 2018-12-14 攀钢集团攀枝花钢铁研究院有限公司 Titanium slag preparation method
CN109097600A (en) * 2018-09-12 2018-12-28 攀钢集团攀枝花钢铁研究院有限公司 It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide
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
CN112960692A (en) * 2021-04-13 2021-06-15 攀钢集团攀枝花钢铁研究院有限公司 Production method of titanium raw material for sulfate process titanium dioxide
CN113462842A (en) * 2021-05-31 2021-10-01 钢研晟华科技股份有限公司 Method for preparing high-titanium slag powder and metal iron powder by reducing ilmenite concentrate powder at low temperature
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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