CN109097600A - It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide - Google Patents

It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide Download PDF

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Publication number
CN109097600A
CN109097600A CN201811063113.0A CN201811063113A CN109097600A CN 109097600 A CN109097600 A CN 109097600A CN 201811063113 A CN201811063113 A CN 201811063113A CN 109097600 A CN109097600 A CN 109097600A
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China
Prior art keywords
titanium slag
titanium
ilmenite concentrate
reducing agent
preparation
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Pending
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CN201811063113.0A
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Chinese (zh)
Inventor
李凯茂
王斌
韩可喜
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Priority to CN201811063113.0A priority Critical patent/CN109097600A/en
Publication of CN109097600A publication Critical patent/CN109097600A/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1204—Obtaining 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
    • C22B34/1209—Obtaining 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1204—Obtaining 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
    • C22B34/1213—Obtaining 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 wet processes, e.g. using leaching methods or flotation techniques

Abstract

The present invention relates to sulfate process titanium dioxide production fields, especially a kind of to efficiently solve the problems, such as that acid-dissolved titanium slag acidolysis rate is low, iron powder additional amount is high and the preparation method of the titanium slag for being used to prepare sulfate process titanium dioxide at high cost, include the following steps: a, raw material preparation: (1) raw material includes ilmenite concentrate and reducing agent；(2) corresponding impurity element or microelement should meet the mass percent range for accounting for ilmenite concentrate；B, electric furnace smelting；C, titanium slag is cooling；D, titanium slag is crushed；E, ball milling；F, acidolysis；G, titanium slag product is obtained.By optimizing the preparation process of sulfate process titanium dioxide titanium slag, ilmenite concentrate and reducing agent raw material are screened first, secondly, obtaining final product by electric furnace smelting, cooling, broken, ball milling and hydrolysis step.The present invention successfully solves the problems, such as that acid-dissolved titanium slag acidolysis rate is low, iron powder additional amount is high and at high cost, is particularly suitable among the production for preparing the titanium slag of sulfate process titanium dioxide.

Description

It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide
Technical field
The present invention relates to sulfate process titanium dioxide production field, especially a kind of preparation for the titanium slag for being used to prepare sulfate process titanium dioxide Method.
Background technique
The raw material of sulfate process titanium dioxide mainly has ilmenite and high titanium slag, compared with ilmenite, uses titanium slag as sulfuric acid process Titanium white raw material can not only increase the production capacity of unit equipment, shorten process flow, and can also fundamentally solve sulfuric acid process titanium Environmental issue caused by white by-product ferrous sulfate.
The survival pressure of raising with country to environmental requirement, sulfuric acid method titanium pigment factory is increasing, has titanium at present White manufacturing enterprise is forced to stop production or selects titanium slag as a raw material for production because of the processing problem of ferrous sulfate, and environmental issue has become Restrict the greatest problem of sulfate process titanium dioxide enterprise development.It therefore, the use of acid-dissolved titanium slag is that raw material will become sulfate process titanium dioxide Development trend.
There is titanium slag acidolysis rates in domestic titanium slag application process it is low, iron powder additional amount is big, at high cost the problems such as.These are asked Topic has direct relation with titanium slag preparation and application, for this purpose, developing a kind of dedicated titanium slag of sulfate process titanium dioxide is particularly important.
Summary of the invention
Efficiently solve that acid-dissolved titanium slag acidolysis rate is low, iron powder adds technical problem to be solved by the invention is to provide one kind Enter the preparation method of the titanium slag for being used to prepare sulfate process titanium dioxide of the high and at high cost problem of amount.
The technical solution adopted by the present invention to solve the technical problems is: being used to prepare the preparation of the titanium slag of sulfate process titanium dioxide Method includes the following steps: a, raw material preparation: (1) raw material includes ilmenite concentrate and reducing agent, is smelted according to titanium slag to ilmenite concentrate matter Amount and reducing agent quality requirement, ilmenite concentrate and reducing agent should meet: containing TiO in ilmenite concentrate2Mass percent range be 47% ~52%, the control of ilmenite concentrate granularity is 200 mesh >=95%, in reducing agent reducing agent fixed carbon mass percent range be >= 85%, reducing agent particle size range is 1mm~3mm >=90%, 3mm~5mm≤8% and 0~1mm≤2%, ilmenite concentrate and reducing agent Moisture content mass percent≤0.2%；(2) in ilmenite concentrate, corresponding impurity element or microelement, which should meet, accounts for ilmenite concentrate Mass percent range are as follows: CaO≤1.5%, 1%≤MgO≤5%, SiO2≤ 5%, Al2O3≤ 2%, Cr2O3≤ 0.015%, V2O5≤ 0.3%；B, electric furnace smelting: ingredient is carried out using ilmenite concentrate and reducing agent, is added in electric furnace and carries out reducing and smelting, obtain Titanium slag grade range is 70%~80%；C, titanium slag is cooling；D, titanium slag is crushed；E, broken titanium slag is subjected to ball milling； F, the titanium slag after ball milling is subjected to acidolysis, in which: reaction acid concentration is 92%~98%, and acid sludge ratio is 1.55-1.75, when curing Between 2h-3h, 210-240 DEG C of main reaction temperature should close compressed air require when main reaction temperature drops to 180-200 DEG C； G, titanium slag product is obtained.
Further, in step b, smelting endpoint judgment method are as follows: dense with FeO content, flue-gas temperature, CO in titanium slag Degree, flue gas flow are that index is judged.
Further, smelting endpoint judgment criteria are as follows: the mass percent range of FeO be 8-10%, flue-gas temperature≤ 500 DEG C, CO concentration≤45%, flue gas flow≤2500NM3/h。
Further, cooling temperature range is≤450 DEG C in step c, cooling time is 6~12h.
Further, titanium slag particle size after cracking range is 2-10mm in step d.
Further, titanium slag particle size range is -325 mesh≤5% after ball milling in step e.
The beneficial effects of the present invention are: by the preparation process of optimization sulfate process titanium dioxide titanium slag, first to ilmenite concentrate and also Former agent raw material is screened, secondly, obtaining final product by electric furnace smelting, cooling, broken, ball milling and hydrolysis step. The present invention successfully solves the problems, such as that acid-dissolved titanium slag acidolysis rate is low, iron powder additional amount is high and at high cost, is particularly suitable for Among the production for preparing the titanium slag of sulfate process titanium dioxide.
Specific embodiment
It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide, includes the following steps: a, raw material preparation: (1) raw material packet Ilmenite concentrate and reducing agent are included, ilmenite concentrate quality and reducing agent quality requirement, ilmenite concentrate and reducing agent should be expired according to titanium slag smelting Foot: contain TiO in ilmenite concentrate2Mass percent range be 47%~52%, ilmenite concentrate granularity control be 200 mesh >=95%, also In former agent reducing agent fixed carbon mass percent range be >=85%, reducing agent particle size range be 1mm~3mm >=90%, 3mm~ 5mm≤8% and 0~1mm≤2%, ilmenite concentrate and reducing agent moisture content mass percent≤0.2%；(2) it in ilmenite concentrate, corresponds to Impurity element or microelement should meet the mass percent range for accounting for ilmenite concentrate are as follows: CaO≤1.5%, 1%≤MgO≤ 5%, SiO2≤ 5%, Al2O3≤ 2%, Cr2O3≤ 0.015%, V2O5≤ 0.3%；B, ilmenite concentrate and reduction electric furnace smelting: are utilized Agent carries out ingredient, is added in electric furnace and carries out reducing and smelting, and obtaining titanium slag grade range is 70%~80%；C, titanium slag is cooling； D, titanium slag is crushed；E, broken titanium slag is subjected to ball milling；F, the titanium slag after ball milling is subjected to acidolysis, in which: reaction acid is dense Degree is 92%~98%, and acid sludge ratio is 1.55-1.75, curing time 2h-3h, 210-240 DEG C of main reaction temperature, to main reaction temperature When degree drops to 180-200 DEG C, compressed air require should be closed；G, titanium slag product is obtained.
The present invention first sieves ilmenite concentrate and reducing agent raw material by the preparation process of optimization sulfate process titanium dioxide titanium slag Choosing, secondly, obtaining final product by electric furnace smelting, cooling, broken, ball milling and hydrolysis step.The present invention successfully solves Acid-dissolved titanium slag acidolysis rate of having determined is low, iron powder additional amount is high and problem at high cost, before having very wide marketing Scape.The present invention achieves positive technical effect by the optimization to production technology.
In order to advanced optimize above-mentioned preparation method, in stepb, smelting endpoint judgment method are as follows: contained with FeO in titanium slag Amount, flue-gas temperature, CO concentration, flue gas flow are that index is judged.Concretely, smelting endpoint judgment criteria are as follows: the matter of FeO Amount percentage range is 8-10%, flue-gas temperature≤500 DEG C, CO concentration≤45%, flue gas flow≤2500NM3/h。
In the step c step that titanium slag is cooling, since the cooling degree of titanium slag is mutually constituted titanium slag object and low price Ti content There is larger impact, and these factors and titanium slag acidolysis rate, iron powder additional amount, oxidant additional amount have direct relation.Titanium slag acidolysis Rate is mainly related with titanium slag rutile content, anosovite content, needs anosovite content >=90%, rutile content≤5%.And Iron powder additional amount, oxidant additional amount and titanium slag middle or low price Ti content are related.In general, in step c, cooling temperature range is≤ 450 DEG C, cooling time is 6~12h.
In step d, titanium slag particle size after cracking size is mainly related with subsequent ball milling, and titanium slag particle size after cracking preferred scope is 2- 10mm.And titanium slag particle size after cracking directly affects titanium slag acidolysis rate, in step e, titanium slag particle size range is preferably -325 mesh after ball milling ≤ 5%.
Embodiment
Embodiment 1
Firstly, choosing ilmenite concentrate TiO247%, 200 mesh of granularity be 95%, reducing agent fixed carbon be 85%, granularity 1mm~ 3mm is 91.5%, ilmenite concentrate and reducing agent moisture content are 0.05%, V2O5For 0.1%, Cr2O3Micro, CaO 0.95%, MgO are 4.85%, SiO2For 2.8%, Al2O3It is 1.5%；Then, ilmenite concentrate and reducing agent are subjected to ingredient by a certain percentage, electricity is added Reducing and smelting is carried out in furnace, according to FeO content in titanium slag be 8.2%, flue-gas temperature is 480 DEG C, CO concentration is 42%, flue gas temperature Degree is 2350NM3The comprehensive descisions such as/h are come out of the stove, and obtaining titanium slag grade is 76%；Then cooling treatment, cooling temperature are carried out to titanium slag Degree is 180 DEG C, cooling time 10h, obtaining in titanium slag anosovite content is 91%, and rutile content 3.5%, Low-valent Titanium contains Amount is 14.6%；Then, titanium slag after cooling is crushed, particle size after cracking is controlled in 2-10mm；Then, titanium slag carries out after being crushed Ball milling, obtaining titanium slag granularity is -325 mesh≤4.5%；Finally, reaction acid concentration 96% puts into acid by titanium slag by acid sludge than 1.62 It solves pot and carries out acidolysis, at 235 DEG C, the curing time controls in 3h the control of main reaction temperature, drops to 195 DEG C to main reaction temperature When, close compressed air require.
After this method is implemented, titanium slag acidolysis rate can reach 96.5%, and when acidolysis does not have to plus iron powder amount or oxidant.By mine Slag ratio example 0.8:1 produces titanium white, and cost advantage is obvious.
Embodiment 2
Firstly, choosing ilmenite concentrate TiO249%, 200 mesh of granularity be 97%, reducing agent fixed carbon be 88%, granularity 1mm~ 3mm is 96%, ilmenite concentrate and reducing agent moisture content are 0.05%, V2O5For 0.1%, Cr2O3Micro, CaO 0.92%, MgO are 4.05%, SiO2For 1.8%, Al2O3It is 1.2%；Then, ilmenite concentrate and reducing agent are subjected to ingredient by a certain percentage, electricity is added Reducing and smelting is carried out in furnace, according to FeO content in titanium slag be 8.5%, flue-gas temperature is 495 DEG C, CO concentration is 45%, flue gas temperature Degree is 2500NM3The comprehensive descisions such as/h are come out of the stove, and obtaining titanium slag grade is 78%；Then cooling treatment, cooling temperature are carried out to titanium slag Degree is 350 DEG C, cooling time 8h, obtaining in titanium slag anosovite content is 93.5%, rutile content 4.5%, Low-valent Titanium Content is 17.2%；Then, titanium slag after cooling is crushed, particle size after cracking is controlled in 2-10mm；Then, be crushed after titanium slag into Row ball milling, obtaining titanium slag granularity is -325 mesh≤3.5%；Finally, reaction acid concentration 94% is put by titanium slag by acid sludge than 1.68 Acidolysis pot carries out acidolysis, and at 225 DEG C, the curing time controls in 2.5h the control of main reaction temperature, drops to 190 to main reaction temperature DEG C when, close compressed air require.
After this method is implemented, titanium slag acidolysis rate can reach 96%, and when acidolysis does not have to plus iron powder amount.In slag ratio 1.2: 1 production titanium white, cost advantage are obvious.
Embodiment 3
Firstly, choosing ilmenite concentrate TiO251%, 200 mesh of granularity is 98.5%, and reducing agent fixed carbon is 88%, granularity 1mm ~3mm is 97.5%, ilmenite concentrate and reducing agent moisture content are 0.05%, V2O5For 0.1%, Cr2O3It is micro, CaO 0.52%, MgO For 2.05%, SiO2For 1.05%, Al2O3It is 0.6%；Then, ilmenite concentrate and reducing agent are subjected to ingredient by a certain percentage, added Enter and carry out reducing and smelting in electric furnace, according to FeO content in titanium slag be 8.3%, flue-gas temperature is 500 DEG C, CO concentration is 45%, cigarette Temperature degree is 2500NM3The comprehensive descisions such as/h are come out of the stove, and obtaining titanium slag grade is 80%；Then cooling treatment is carried out to titanium slag, it is cold But temperature is 450 DEG C, cooling time 6h, obtaining in titanium slag anosovite content is 90.5%, rutile content 5%, at a low price Ti content is 18%；Then, titanium slag after cooling is crushed, particle size after cracking is controlled in 2-10mm；Then, be crushed after titanium slag into Row ball milling, obtaining titanium slag granularity is -325 mesh≤2.5%；Finally, reaction acid concentration 92% is put by titanium slag by acid sludge than 1.72 Acidolysis pot carries out acidolysis, and at 220 DEG C, the curing time controls in 2h the control of main reaction temperature, drops to 180 DEG C to main reaction temperature When, close compressed air require.
After this method is implemented, titanium slag acidolysis rate can reach 95%, and when acidolysis does not have to plus iron powder amount.In slag ratio 1.4: 1 production titanium white, cost advantage are obvious.

Claims (6)

1. being used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide, which comprises the steps of:
A, raw material preparation:
(1) raw material includes ilmenite concentrate and reducing agent, is smelted according to titanium slag to ilmenite concentrate quality and reducing agent quality requirement, ilmenite concentrate It should meet with reducing agent: containing TiO in ilmenite concentrate2Mass percent range be 47%~52%, ilmenite concentrate granularity control be 200 Mesh >=95%, it is 1mm~3mm that reducing agent fixed carbon mass percent range, which is >=85%, reducing agent particle size range, in reducing agent >=90%, 3mm~5mm≤8% and 0~1mm≤2%, ilmenite concentrate and reducing agent moisture content mass percent≤0.2%；
(2) in ilmenite concentrate, corresponding impurity element or microelement should meet the mass percent range for accounting for ilmenite concentrate are as follows: CaO≤1.5%, 1%≤MgO≤5%, SiO2≤ 5%, Al2O3≤ 2%, Cr2O3≤ 0.015%, V2O5≤ 0.3%；
B, electric furnace smelting:
Ingredient is carried out using ilmenite concentrate and reducing agent, is added in electric furnace and carries out reducing and smelting, obtaining titanium slag grade range is 70% ~80%；
C, titanium slag is cooling；
D, titanium slag is crushed；
E, broken titanium slag is subjected to ball milling；
F, the titanium slag after ball milling is subjected to acidolysis, in which: reaction acid concentration is 92%~98%, and acid sludge ratio is 1.55-1.75, ripe Change time 2h-3h, 210-240 DEG C of main reaction temperature should close compressed air when main reaction temperature drops to 180-200 DEG C Flow；
G, titanium slag product is obtained.
2. being used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide as described in claim 1, it is characterised in that: in step b, Smelting endpoint judgment method are as follows: judged using FeO content, flue-gas temperature, CO concentration, flue gas flow in titanium slag as index.
3. being used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide as claimed in claim 2, it is characterised in that: smelting endpoint Judgment criteria are as follows: the mass percent range of FeO is 8-10%, flue-gas temperature≤500 DEG C, CO concentration≤45%, flue gas flow ≤2500NM3/h。
4. being used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide as described in claim 1, it is characterised in that: in step c, Cooling temperature range is≤450 DEG C, and cooling time is 6~12h.
5. being used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide as described in claim 1, it is characterised in that: in step d, Titanium slag particle size after cracking range is 2-10mm.
6. being used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide as described in claim 1, it is characterised in that: in step e, Titanium slag particle size range is -325 mesh≤5% after ball milling.
CN201811063113.0A 2018-09-12 2018-09-12 It is used to prepare the preparation method of the titanium slag of sulfate process titanium dioxide Pending CN109097600A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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CN111547765A (en) * 2020-05-18 2020-08-18 攀钢集团攀枝花钢铁研究院有限公司 Method for improving acidolysis rate of titanium slag
CN112481509A (en) * 2020-11-27 2021-03-12 攀钢集团钛业有限责任公司 Method for judging titanium slag smelting end point
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
CN115287473A (en) * 2022-08-09 2022-11-04 攀钢集团攀枝花钢铁研究院有限公司 Titanium slag smelting method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111547765A (en) * 2020-05-18 2020-08-18 攀钢集团攀枝花钢铁研究院有限公司 Method for improving acidolysis rate of titanium slag
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Application publication date: 20181228