CN101787432A - Method for preparing acid-soluble titanium slag from high-titanium slag - Google Patents
Method for preparing acid-soluble titanium slag from high-titanium slag Download PDFInfo
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- CN101787432A CN101787432A CN201010103667A CN201010103667A CN101787432A CN 101787432 A CN101787432 A CN 101787432A CN 201010103667 A CN201010103667 A CN 201010103667A CN 201010103667 A CN201010103667 A CN 201010103667A CN 101787432 A CN101787432 A CN 101787432A
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- titanium slag
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- 239000010936 titanium Substances 0.000 title claims abstract description 71
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 71
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000002893 slag Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 43
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 41
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000292 calcium oxide Substances 0.000 claims abstract description 22
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 235000010215 titanium dioxide Nutrition 0.000 claims description 23
- 235000012255 calcium oxide Nutrition 0.000 claims description 21
- 238000002386 leaching Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 239000008399 tap water Substances 0.000 claims description 5
- 235000020679 tap water Nutrition 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 239000004571 lime Substances 0.000 claims description 2
- 230000035800 maturation Effects 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 5
- 229910052791 calcium Inorganic materials 0.000 claims 5
- 239000011575 calcium Substances 0.000 claims 5
- 239000002994 raw material Substances 0.000 abstract description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 abstract description 8
- 235000010344 sodium nitrate Nutrition 0.000 abstract description 4
- 239000004317 sodium nitrate Substances 0.000 abstract description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract 2
- 239000011707 mineral Substances 0.000 abstract 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 abstract 1
- 229910002971 CaTiO3 Inorganic materials 0.000 abstract 1
- 229910005451 FeTiO3 Inorganic materials 0.000 abstract 1
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 11
- 229910052742 iron Inorganic materials 0.000 description 9
- 239000012071 phase Substances 0.000 description 7
- 229910000805 Pig iron Inorganic materials 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 238000011084 recovery Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 3
- 238000011284 combination treatment Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229940001516 sodium nitrate Drugs 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for preparing acid-soluble titanium slag from high-titanium slag. The method comprises the following steps: smashing the high-titanium slag, an oxidant (one or mixture of two of sodium nitrate and ammonium nitrate) and calcium oxide or calcium carbonate, mixing, preparing materials, then carrying out mineral phase reconstruction and modification at high temperature to transform rutile or anatase TiO2 and FeTiO3 in the slag to modified CaTiO3 mineral phase, and cooling to obtain an acid-soluble titanium slag raw material which can prepare titanium dioxide powder by using the sulfuric acid method.
Description
One. affiliated technical field
The present invention relates to a kind of titanium slag through behind the ore phase reconstruction, prepare the method for acid-dissolved titanium slag.Specifically, the present invention relates to the method that a kind of energy satisfies the acid-dissolved titanium slag of producing the titanium dioxide requirement, belong to the titanium field of metallurgy.
Two. background technology
Titanium slag mainly is to adopt the method for electrosmelting ilmenite to prepare.Generally make reductive agent with carbon raw materials such as hard coal, coke or refinery cokes, the ferriferous oxide in the ilmenite is reduced to metallic iron enters liquid phase, titanium is enriched in the slag phase, the product that the metal iron phase of clarification back fractional melting obtains is a titanium slag.Titanium slag both can be used as the raw material of Production By Sulfuric Acid Process titanium white, also can be in large quantities as the raw material of producing titanium white in the chlorination process technology.The domestic titanium slag that will be used for the Production By Sulfuric Acid Process titanium white is called acid-dissolved titanium slag.
The preparation of titanium dioxide mainly contains sulfuric acid process and two kinds of technologies of chlorination process.Chlorination process is produced the titanium slag specification of quality harshness of titanium white, requires with containing TiO
2Titanium slag more than 90% is a raw material, and (CaO+MgO)≤1.5% in the titanium slag.Have only the low ilmenite of the non-iron contamination content of melting could obtain to be suitable for chloride process titanium dioxide and produce required qualified titanium slag, require radioelement and CaO, MgO in the ilmenite raw material, MnO
2, impurity such as P, S content low more good more.And electrosmelting is when containing the high ilmenite of non-iron contaminations such as CaO, MgO, can only obtain to be suitable for the titanium slag of sulfate process titanium dioxide production usefulness, but exist when adopting electrosmelting explained hereafter acid-dissolved titanium slag,, cause the not high problem of the rate of recovery of iron and titanium because need in slag, to keep a certain proportion of FeO.When adopting Titanium White Production By Sulfuric Acid Process, if be raw material with the ilmenite, exist to produce a large amount of green vitriols and a large amount of dilute sulphuric acid wastewater problems, enterprise carries out the expense height that the three wastes are handled, and environmental capacity is little, has limited the development of ilmenite sulfuric acid process.But, when adopting sulfuric acid process, if the miscellany with ilmenite and solubility in acid titanium slag is a raw material, especially be raw material with single higher-grade solubility in acid titanium slag, the iron content waste of output is few, do not have the problem of green vitriol ferrous sulfate, and the diluted acid generation is few, reduced the harm of environment and reduced the control expense of the relevant three wastes, increased the vitality of sulfate process titanium dioxide production technique.
Yet, when adopting the electric furnace reduction concentrated ilmenite separation pig iron to prepare titanium slag, if acquisition acid-dissolved titanium slag, then can not drastic reduction, thereby cause titanium slag to separate with molten iron not exclusively, the titanium slag amount of carrying secretly in the pig iron that obtains is big, brings negative impact on the one hand the processing of the follow-up pig iron, reduces the rate of recovery of titanium and iron on the other hand.If with in the electrosmelting process titanium being separated titanium slag completely with iron, with Titanium White Production By Sulfuric Acid Process, the leaching yield of titanium dioxide can only reach 60wt%～70wt%.
Three. summary of the invention
1. Fa Ming purpose
To carry out ore phase reconstruction through the dark reductive titanium slag that the electric furnace reduction concentrated ilmenite separation pig iron produces, the preparation acid-dissolved titanium slag satisfies the requirement of the acid-dissolved titanium slag of method for producing gtitanium dioxide with sulphuric acid, improves titanium recovery rate.
2. Fa Ming technical scheme
The titanium slag that separates pig iron generation with the electric furnace reduction concentrated ilmenite is a raw material, through obtaining to satisfy raw material---the acid-dissolved titanium slag of Titanium White Production By Sulfuric Acid Process after pulverizing, batching, high temperature modified, the cooling, leaching yield is more than 94.5wt% when leaching with sulfuric acid, and its specific practice is:
1.1 batching: material composition is counted with wt%: titanium slag TiO
2＞80, CaO 0.1～5.0, MgO 0.1～5.0, FeO 0.1～15, properties-correcting agent is for containing CaCO
3Lime carbonate greater than 90 and/or contain CaO greater than choosing any one kind of them in the mixture of 90 unslaked lime and/or lime carbonate and unslaked lime, oxygenant is the NaNO of purity greater than 95wt%
3, and/or purity greater than 95wt%NH
4NO
3, and/or their mixture in choose any one kind of them, with be crushed to granularity less than the titanium slag of 0.15mm and oxygenant and calcium oxide or lime carbonate according to titanium slag: the weight ratio of oxygenant=1: 0.01～0.5, titanium slag: the weight ratio of calcium oxide=1: 0.01～0.5 or titanium slag: the weight ratio of lime carbonate=1: 0.01～0.8 or titanium slag: the mixed batching of the weight ratio of lime carbonate and quicklime mixture=1: 0.01～0.8, time 0.1～3.0h;
1.2 high temperature ore phase reconstruction modification: is 600～1400 ℃ of roastings through the blended material in temperature, and roasting time is 2.0～20 hours, carries out the TiO by rutile-type or Detitanium-ore-type
2And FeTiO
3Change CaTiO into
3Ore phase reconstruction and modification;
1.3 cool off levigate: the material that obtains after high temperature ore phase reconstruction and the modification is cooled to room temperature, is milled down to granularity, just obtain to satisfy the solubility in acid titanium slag of Production By Sulfuric Acid Process titanium white less than 0.15mm;
1.4 sulfuric acid leaches: the solubility in acid titanium slag is the sulphuric acid soln of 85～90wt% with concentration, is 230～250 ℃ of slakings in temperature, behind maturation process 60～90min, is 60～70 ℃ of leachings with tap water in temperature, time 30～90min, titanium dioxide leaching yield 94.6～95.8wt%.
3. Fa Ming positively effect
1), titanium recovery rate is increased to 94.6～95.8wt% by 60～70wt%.
2), the refuse amount reduces, three wastes processing costs reduces, and helps environment protection.
Four. embodiment
Embodiment 1
To contain TiO
2The titanium slag of 92.5wt%, contain CaCO
3For the lime carbonate of 98wt%, contain NaNO
3NaNO greater than 95wt%
3Crushed after being dried is stand-by to granularity＜0.15mm respectively.Take by weighing above-mentioned ready titanium slag 100g, lime carbonate 30g, SODIUMNITRATE 10g respectively, place mortar combination treatment 30min, then the material that mixes is placed retort furnace, in temperature is 1050 ℃ of roasting 3h, after being cooled to room temperature, levigate to particle diameter less than 0.15mm, obtain can be used in the acid-dissolved titanium slag 131.5g that sulfuric acid process prepares titanium white.The acid-dissolved titanium slag that obtains after temperature is 230 ℃ of slaking 90min, is 70 ℃ with tap water 600mL in temperature and leaches 30min that the leaching yield of titanium dioxide is 94.6wt% with the sulphuric acid soln of 85wt%.
Embodiment 2
To contain TiO
2The titanium slag of 92.5wt%, contain unslaked lime that CaO is 95wt%, contain NaNO
3NaNO greater than 95wt%
3Crushed after being dried is stand-by to granularity＜0.15mm respectively.Take by weighing above-mentioned ready titanium slag 100g, unslaked lime 20g, SODIUMNITRATE 15g respectively, place mortar combination treatment 20min, then the material that mixes is placed rotary kiln, in temperature is 1100 ℃ of roasting 2h, after being cooled to room temperature, levigate to particle diameter less than 0.15mm, obtain can be used in the acid-dissolved titanium slag 132.2g that sulfuric acid process prepares titanium white.The acid-dissolved titanium slag that obtains after temperature is 240 ℃ of slaking 90min, is 60 ℃ with tap water 600mL in temperature and leaches 60min that the leaching yield of titanium dioxide is 95.8wt% with the sulphuric acid soln of 90wt%.
Embodiment 3
To contain TiO
2The titanium slag of 92.5wt%, contain CaCO
3For the lime carbonate of 98wt%, contain unslaked lime that CaO is 95wt%, contain NaNO
3NaNO greater than 95%
3Crushed after being dried is stand-by to granularity＜0.15mm respectively.Take by weighing above-mentioned titanium slag 100g, lime carbonate 20g, unslaked lime 10g, SODIUMNITRATE 15g respectively, place mortar combination treatment 30min, then the material that mixes is placed rotary kiln, in temperature is 1100 ℃ of roasting 3h, after being cooled to room temperature, levigate to particle diameter less than 0.15mm, obtain can be used in the acid-dissolved titanium slag 134.2g that sulfuric acid process prepares titanium white.The acid-dissolved titanium slag that obtains after temperature is 250 ℃ of slaking 90min, is 60 ℃ with tap water 600mL in temperature and leaches 60min that the leaching yield of titanium dioxide is 95.3wt% with the sulphuric acid soln of 85wt%.
Claims (1)
1. the method from preparing acid-soluble titanium slag by high titanium slag through comprises batching, and the modification of high temperature ore phase reconstruction is cooled off levigately, and sulfuric acid leaches 4 steps, it is characterized in that:
1.1 batching: material composition is counted with wt%: titanium slag TiO
2＞80, CaO 0.1～5.0, MgO 0.1～5.0, FeO 0.1～15, properties-correcting agent is for containing CaCO
3Lime carbonate greater than 90 and/or contain CaO greater than choosing any one kind of them in the mixture of 90 unslaked lime and/or lime carbonate and unslaked lime, oxygenant is the NaNO of purity greater than 95wt%
3, and/or purity greater than 95wt%NH
4NO
3, and/or their mixture in choose any one kind of them, with be crushed to granularity less than the titanium slag of 0.15mm and oxygenant and Yangization Calcium or Tan Suan Calcium according to titanium slag: the weight ratio of oxygenant=1: 0.01～0.5, titanium slag: the weight ratio of Yangization Calcium=1: 0.01～0.5 or titanium slag: the weight ratio of Tan Suan Calcium=1: 0.01～0.8 or titanium slag: the mixed batching of the weight ratio of Tan Suan Calcium and quicklime mixture=1: 0.01～0.8, time 0.1～3.0h;
1.2 high temperature ore phase reconstruction modification: is 600～1400 ℃ of roastings through the blended material in temperature, and roasting time is 2.0～20 hours, carries out the TiO by rutile-type or Detitanium-ore-type
2And FeTiO
3Change CaTiO into
3Ore phase reconstruction and modification;
1.3 cool off levigate: the material that obtains after high temperature ore phase reconstruction and the modification is cooled to room temperature, is milled down to granularity, just obtain to satisfy the solubility in acid titanium slag of Production By Sulfuric Acid Process titanium white less than 0.15mm;
1.4 sulfuric acid leaches: the solubility in acid titanium slag is the sulphuric acid soln of 85～90wt% with concentration, is 230～250 ℃ of slakings in temperature, behind maturation process 60～90min, is 60～70 ℃ of leachings with tap water in temperature, time 30～90min, titanium dioxide leaching yield 94.6～95.8wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101036676A CN101787432B (en) | 2010-02-02 | 2010-02-02 | Method for preparing acid-soluble titanium slag from high-titanium slag |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101036676A CN101787432B (en) | 2010-02-02 | 2010-02-02 | Method for preparing acid-soluble titanium slag from high-titanium slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101787432A true CN101787432A (en) | 2010-07-28 |
| CN101787432B CN101787432B (en) | 2011-09-14 |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583515A (en) * | 2012-01-09 | 2012-07-18 | 安徽工业大学 | Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag |
| CN102745743A (en) * | 2012-08-08 | 2012-10-24 | 长沙矿冶研究院有限责任公司 | Method for preparing artificial rutile by titanium slags |
| CN104894384A (en) * | 2015-06-26 | 2015-09-09 | 河南理工大学 | Process using red mud to extract titanium |
| CN107460345A (en) * | 2016-06-02 | 2017-12-12 | 昆明冶金高等专科学校 | A kind of method for producing high titanium slag |
| CN113522224A (en) * | 2021-07-02 | 2021-10-22 | 商洛学院 | Method for preparing calcium titanate adsorption material by using low-grade rutile concentrate |
| CN115092967A (en) * | 2022-07-27 | 2022-09-23 | 成都纺织高等专科学校 | Method for preparing polyaluminium sulfate iron titanium |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1243840C (en) * | 2003-10-31 | 2006-03-01 | 攀枝花钢铁有限责任公司钢铁研究院 | Improve titanium slag TiO2Method of grading |
| CN101186335B (en) * | 2007-12-20 | 2010-07-21 | 昆明理工大学 | Method for preparing artificial rutile by microwave heating and oxidation sintering |
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2010
- 2010-02-02 CN CN2010101036676A patent/CN101787432B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583515A (en) * | 2012-01-09 | 2012-07-18 | 安徽工业大学 | Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag |
| CN102583515B (en) * | 2012-01-09 | 2014-04-02 | 安徽工业大学 | Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag |
| CN102745743A (en) * | 2012-08-08 | 2012-10-24 | 长沙矿冶研究院有限责任公司 | Method for preparing artificial rutile by titanium slags |
| CN104894384A (en) * | 2015-06-26 | 2015-09-09 | 河南理工大学 | Process using red mud to extract titanium |
| CN104894384B (en) * | 2015-06-26 | 2017-03-08 | 河南理工大学 | A kind of red mud puies forward titanium technique |
| CN107460345A (en) * | 2016-06-02 | 2017-12-12 | 昆明冶金高等专科学校 | A kind of method for producing high titanium slag |
| CN113522224A (en) * | 2021-07-02 | 2021-10-22 | 商洛学院 | Method for preparing calcium titanate adsorption material by using low-grade rutile concentrate |
| CN115092967A (en) * | 2022-07-27 | 2022-09-23 | 成都纺织高等专科学校 | Method for preparing polyaluminium sulfate iron titanium |
| CN115092967B (en) * | 2022-07-27 | 2024-03-15 | 成都纺织高等专科学校 | Method for preparing polymeric aluminum ferric titanium sulfate |
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| Publication number | Publication date |
|---|---|
| CN101787432B (en) | 2011-09-14 |
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