CN104313338A - Titaniferous metallurgical residue treatment method - Google Patents
Titaniferous metallurgical residue treatment method Download PDFInfo
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- CN104313338A CN104313338A CN201410575186.3A CN201410575186A CN104313338A CN 104313338 A CN104313338 A CN 104313338A CN 201410575186 A CN201410575186 A CN 201410575186A CN 104313338 A CN104313338 A CN 104313338A
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- titaniferous
- acidleach
- residue
- titaniferous metallurgical
- filter residue
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a titaniferous metallurgical residue treatment method and relates to the technical field of metallurgy chemical industry. The titaniferous metallurgical residue treatment method comprises the following processing steps: (1) breaking titaniferous metallurgical residue; (2) burdening residue and carbon powder in a certain mass ratio; (3) in argon protective atmosphere, heating an electric tube furnace to a given temperature, placing burdened ingredients into an aluminium oxide crucible, putting the aluminium oxide crucible into the electric tube furnace at a high temperature, and insulating for a period of time; (4) taking out the aluminium oxide crucible at high temperature, and quenching to obtain broken glass; (5) separating filter residue and filtrate through filtration by utilizing the broken glass acid-pickled and carbonized by HCl; (6) after acid pickling treatment is carried out, carrying out mineral separation on the filter residue by utilizing a magnetic separation or floatation manner, so that separation of TiC and amorphous SiO2 in the filter residue is realized. The titaniferous metallurgical residue treatment method has the advantages that the problems that thorough acid pickling is difficult to realize as perovskite and other minerals exist in the traditional acid process treatment process and pure titanic mineral can not be obtained; meanwhile, alkali treatment is avoided, high temperature is not required any more, and energy consumption in a reaction process is reduced.
Description
Technical field
The present invention relates to a kind of chemical metallurgy technical field, be specially a kind of titaniferous metallurgical slag treatment process.
Background technology
China's titanium aboundresources, accounts for No. 1 in the world, but the utilization ratio of titanium resource is but very low.Mainly adopt blast furnace process to smelt vanadium titano-magnetite (as Flos Bombacis Malabarici iron and steel and Chengde iron and steel) at present, reclaimed iron and vanadium, and titanium is with TiO
2form enters blast furnace slag (massfraction about 25%), because mineral phase structure is complicated, is difficult to recycle.The titanium-containing blast furnace slag of bulk deposition not only takies valuable land resources, the serious waste of titanium resource especially.Therefore, how process titanium-containing blast furnace slag better the comprehensive utilization tool of China's titanium resource is had very great significance.
Current process titaniferous metallurgical slag mainly contain following several method.(1) material of construction such as cement and concrete is prepared.But document 1 (Xu Chushao, Chen Guangbi. mining metallurgical engineering, 1985,3:51-54.) report, containing TiO
2the strong crystallizing power of blast furnace slag, makes the activity of cement of production poor.(2) acidic process.Document 2 (Liu Xiaohua, Sui Zhitong. China YouSe Acta Metallurgica Sinica, 2002,6:1281-1284.) report uses sulfuric acid or Leaching in Hydrochloric Acid titanium-containing blast furnace slag separation and Extraction TiO
2.But foreign matter content higher in slag (about 75%), make this technique acid consumption large, cost is high, and spent acid and the tailings of generation are many, and environmental pollution is serious.(3) alkaline process process.Document 3 (Zhou Zhiming, Zhang Binghuai. steel vanadium titanium, 1999,4:37-40.) report uses NaOH or Na
2cO
3separation and Extraction TiO
2.But alkaline process complex treatment process, the cost recovery of sodium salt is high, the volatilization heavy corrosion experimental installation of sodium salt under high temperature.(4) high temperature cabonization low temperature chlorination method.Document 4 (Huang Shouhua, Pan Jingye. steel vanadium titanium, 1994,2:17-21.) report makes in blast furnace slag TiO by carburizing reagent
2be converted into TiC, then make it chlorination by chlorination reaction and become TiCl
4, as the raw material preparing titanium sponge or titanium white.But a large amount of CaCl generated in process
2and MgCl
2have the advantages that boiling point is high, viscosity strong, exist with liquid phase, make chlorination plant be difficult to long-term normal operation.(5) high-temperature selective crystallization process.The titanium disperseed in titanium-containing blast furnace slag is enriched in a certain titaniferous thing mutually in (uhligite or anosovite), then realize being separated of titaniferous and impurity phase by beneficiation method, but still successfully cannot accomplish this point at present.(6) iron alloy is prepared.Document 5 (Hou Shixi, Ke Changming. iron alloy, 2007,5:20-23.) report adopts ferrosilicon, document 6 (Li Zushu, Xu Chushao. University Of Chongqing's journal, 1996,4:82-86.) report adopts ferrosilicoaluminum to reduce titanium-containing blast furnace slag in the molten state as reductive agent, prepares silicon titanium, sial ferro-titanium.But need titanium, Silicified breccias little as the steel grade of alloying agents simultaneously, limit the extensive use of this method.
Summary of the invention
In view of this, the invention provides a kind of titaniferous metallurgical slag treatment process.Technical problem to be solved is, due to the existence of uhligite and other mineral in traditional acidic process, acidleach is difficult to thoroughly, cannot obtain the mineral of pure titanium; Avoid with alkaline purification simultaneously, namely without the need to high temperature again, reduce the energy consumption in reaction process.The present invention first adopts excess toner to carry out carbonization to titanium-containing blast furnace slag, makes titanium be converted into TiC, then by acidleach and ore dressing process, obtains TiC and realize effective separation and Extraction of other elements in slag.
Technical scheme of the present invention is: a kind of titaniferous metallurgical slag treatment process, and this processing step comprises:
(1) pre-treatment: be TiO by titaniferous metallurgical slag main component
2, SiO
2, CaO, Al
2o
3, MgO, carry out crushing grinding, for subsequent use;
(2) prepare burden: with titaniferous metallurgical slag for raw material, slag, carbon dust are prepared burden according to certain mass ratio;
(3) carbothermic reduction: under argon atmosphere, rises to carbonization temperature by electric tube furnace furnace temperature, and mixed batching is put into alumina crucible, transfers into electric tube furnace, held for some time in carbonization temperature;
(4) water-cooled: insulation terminates, and take out under carbonization temperature, direct-water-quenching obtains glass dregs, then puts into loft drier drying.
(5) acidleach: utilize the glass dregs after HCl acidleach carbonization, CaO, MgO and Al
2o
3enter filtrate, by filtering separation filter residue and filtrate.
(6) Mineral separation: after acidleach process, the SiO of TiC and vitreous state
2become the main component in filter residue.Utilize the mode of flotation or magnetic separation to carry out ore dressing process to filter residue, realize the SiO of TiC and vitreous state in filter residue
2separation.
(7) the acidleach process of the middle HCl of step (5), CaO contained in titanium-containing blast furnace slag, MgO, Al
2o
3dissolve in filtrate, in filtrate, first added ammonia precipitation process go out Ca (OH)
2, Mg (OH)
2, Al (OH)
3, gained precipitation NaOH solution stripping sodium aluminate, obtains Al after crystallization
2o
3, then by Ca (OH)
2, Mg (OH)
2caO and MgO is obtained after calcining; NH simultaneously
4cl solution can be reclaimed by low-temperature evaporation cold crystallization and obtain NH
4cl.
Batching quality in described step (2) is slag than ratio: C=100:6.53 ~ 13.06.
Carbonization temperature in described step (3) is 1400 DEG C ~ 1800 DEG C, and protective atmosphere is atmospheric pressure state, and working pressure is normal pressure, and soaking time is 1 ~ 10h.
HCl concentration in described step (5) is the liquid-solid mass ratio of 15% ~ 36%, HCl and slag is 5 ~ 10:1.
Acidleach temperature in described step (5) is 25 ~ 105 DEG C.
By induction stirring in acidleach process in described step (5), rotating speed is 0 ~ 400r/min.
Ore dressing treatment process in described step (6) is flotation or magnetic separation.
The beneficial effect that compared to the prior art the present invention has is:
(1) the present invention first adopts carbon dust to carry out carbonization to titanium-containing blast furnace slag, obtains glass dregs after having reduced by water-cooled, changes ore deposit phase composite.
(2) the present invention carries out acidleach process to the titanium-containing blast furnace slag after carbonization, filters the SiO of TiC and vitreous state in rear gained slag
2for main component.
(3) the present invention carries out ore dressing process to the slag after acidleach filtration, realizes the SiO of TiC and vitreous state in filter residue
2separation.Avoid with alkaline purification except SiO
2time TiC particle growing up at high temperature, carry out at normal temperatures simultaneously, cost-saving.
(4) the present invention has also reclaimed the beneficial elements such as Al, Ca, Mg effectively from the filtrate filtered out acidleach treating processes, improves the resource recycling rate of titanium-containing blast furnace slag.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Fig. 2 is the XRD interpretation of result figure of composition after carbonizing treatment of the present invention
Fig. 3 is the SEM picture of composition after acidleach process of the present invention.
Embodiment:
In order to make those skilled in the art understand technical scheme of the present invention better, below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment one:
1) titanium-containing blast furnace slag is broken and be milled to 180 order ± 10 orders, mixing.
2) by slag: the mass ratio batching of C=100:6.53, takes titanium-containing blast furnace slag 10 grams, carbon dust 0.653 gram.
3) under argon atmosphere, electric tube furnace furnace temperature is risen to 1600 DEG C.Mixed batching is put into alumina crucible, and heat puts electric tube furnace into, insulation 2h.
4) insulation terminates, and takes out at 1600 DEG C, directly puts into water cooling and obtains glass dregs, then put into loft drier drying.
5) under the temperature condition of 95 DEG C, utilize HCl to carry out acidleach process to the blast furnace slag after carbonization, this HCl concentration is the add-on of 36% ± 1%, HCl is that the ratio being 8:1 with HCl and carbonization blast furnace slag liquid-solid ratio adds, and the duration needed for acidleach is 10h.Filtrate and filter residue is obtained by filtering separation after acidleach completes.
6) after acidleach process, TiC and SiO
2become the main component in filter residue.Utilize the mode of magnetic separation or flotation to carry out ore dressing process to filter residue, realize the SiO of TiC and vitreous state in filter residue
2separation.
7) the filtrate ammoniacal liquor after acidleach and NaOH process, for the rate of recovery beneficial elements such as Ca, Mg, Al.Its treatment process is, because the titanium-containing blast furnace slag be carbonized is by acidleach process, therefore CaO, MgO, Al
2o
3form muriate to be dissolved in filtrate, so add ammoniacal liquor in filtrate, be settled out Ca (OH)
2, Mg (OH)
2, Al (OH)
3, gained precipitation NaOH solution stripping sodium aluminate, obtains Al after crystallization
2o
3, then by Ca (OH)
2, Mg (OH)
2caO and MgO is obtained after calcining; NH simultaneously
4cl solution can be reclaimed by low-temperature evaporation cold crystallization and obtain NH
4cl.
Embodiment two:
1) titanium-containing blast furnace slag is broken and be milled to 180 order ± 10 orders, mixing.
2) by slag: the mass ratio batching of C=100:6.53, takes titanium-containing blast furnace slag 10 grams, carbon dust 0.653 gram.
3) under argon atmosphere, electric tube furnace furnace temperature is risen to 1600 DEG C.Mixed batching is put into alumina crucible, and heat puts electric tube furnace into, insulation 4h.
4) insulation terminates, and takes out at 1600 DEG C, directly puts into water cooling and obtains glass dregs, then put into loft drier drying.
5) under the temperature condition of 85 DEG C, utilize HCl to carry out acidleach process to the blast furnace slag after carbonization, this HCl concentration is the add-on of 36% ± 1%, HCl is that the ratio being 8:1 with HCl and carbonization metallurgical slag liquid-solid ratio adds, and the duration needed for acidleach is 2h.Be separated by heat filtering after acidleach completes and obtain filtrate and filter residue.
6) after acidleach process, TiC and SiO
2become the main component in filter residue.Utilize the mode of magnetic separation or flotation to carry out ore dressing process to filter residue, realize the SiO of TiC and vitreous state in filter residue
2separation.
7) the filtrate ammoniacal liquor after acidleach and NaOH process, for the rate of recovery beneficial elements such as Ca, Mg, Al.Its treatment process is, because the titanium-containing blast furnace slag be carbonized is by acidleach process, therefore CaO, MgO, Al
2o
3form muriate to be dissolved in filtrate, so add ammoniacal liquor in filtrate, be settled out Ca (OH)
2, Mg (OH)
2, Al (OH)
3, gained precipitation NaOH solution stripping sodium aluminate, obtains Al after crystallization
2o
3, then by Ca (OH)
2, Mg (OH)
2caO and MgO is obtained after calcining; NH simultaneously
4cl solution can be reclaimed by low-temperature evaporation cold crystallization and obtain NH
4cl.
Embodiment three:
1) titanium-containing blast furnace slag is broken and be milled to 180 order ± 10 orders, mixing.
2) by slag: the mass ratio batching of C=100:7.62, takes titanium-containing blast furnace slag 10 grams, carbon dust 0.762 gram.
3) under argon atmosphere, electric tube furnace furnace temperature is risen to 1600 DEG C.Mixed batching is put into alumina crucible, and heat puts electric tube furnace into, insulation 4h.
4) insulation terminates, and takes out, directly put into water and cool, then put into loft drier drying at 1600 DEG C.
5) under the temperature condition of 95 DEG C, utilize HCl to carry out acidleach process to the blast furnace slag after carbonization, this HCl concentration is the add-on of 36% ± 1%, HCl is that the ratio being 6:1 with HCl and carbonization blast furnace slag liquid-solid ratio adds, and the duration needed for acidleach is 5min.Be separated by heat filtering after acidleach completes and obtain filtrate and filter residue.
6) after acidleach process, TiC and SiO
2become the main component in filter residue.Utilize the mode of magnetic separation or flotation to carry out ore dressing process to filter residue, realize the SiO of TiC and vitreous state in filter residue
2separation.
7) the filtrate ammoniacal liquor after acidleach and NaOH process, for the rate of recovery beneficial elements such as Ca, Mg, Al.Its treatment process is, because the titanium-containing blast furnace slag be carbonized is by acidleach process, therefore CaO, MgO, Al
2o
3form muriate to be dissolved in filtrate, so add ammoniacal liquor in filtrate, be settled out Ca (OH)
2, Mg (OH)
2, Al (OH)
3, gained precipitation NaOH solution stripping sodium aluminate, obtains Al after crystallization
2o
3, then by Ca (OH)
2, Mg (OH)
2caO and MgO is obtained after calcining; NH simultaneously
4cl solution can be reclaimed by low-temperature evaporation cold crystallization and obtain NH
4cl.
Claims (6)
1. a titaniferous metallurgical slag treatment process, is characterized in that:
Step one, titaniferous metallurgical slag is carried out crushing grinding, for subsequent use;
Step 2, with titaniferous metallurgical slag for raw material, slag, carbon dust are prepared burden according to certain mass ratio;
Step 3, under argon atmosphere, electric tube furnace furnace temperature is risen to carbonization temperature, mixed batching is put into alumina crucible, transfers into electric tube furnace in carbonization temperature, held for some time;
Step 4, insulation terminate, and take out under carbonization temperature, directly put into water cooling and obtain glass dregs, then put into loft drier drying;
Step 5, utilize certain proportion HCl solution acidleach glass dregs, by filtering separation filter residue and filtrate;
Step 6, after acidleach process, utilize the mode of flotation or magnetic separation to carry out ore dressing process to filter residue, realize the SiO of TiC and vitreous state in filter residue
2separation;
Step 7, first add ammoniacal liquor precipitate in filtrate, gained precipitation NaOH solution stripping sodium aluminate, obtains Al after crystallization
2o
3, then obtain CaO and MgO by after the calcining of residue precipitation; NH simultaneously
4cl solution can be reclaimed by low-temperature evaporation cold crystallization and obtain NH
4cl.
2. titaniferous metallurgical slag treatment process as claimed in claim 1, is characterized in that: the mass ratio batching in described step 2, ratio is slag: carbon dust=100:6.53 ~ 13.06.
3. titaniferous metallurgical slag treatment process as claimed in claim 1, is characterized in that: the carbonization temperature in described step 3 is 1400 DEG C ~ 1800 DEG C, and protective atmosphere is atmospheric pressure state, and soaking time is 1 ~ 10h.
4. titaniferous metallurgical slag treatment process as claimed in claim 1, it is characterized in that: the HCl strength of solution in described step 5 is 15% ~ 36%, described certain proportion is the liquid-solid mass ratio of HCl solution and glass dregs is 5 ~ 10:1.
5. titaniferous metallurgical slag treatment process as claimed in claim 1, it is characterized in that: the acidleach in described step 5, temperature is 25 ~ 105 DEG C.
6. titaniferous metallurgical slag treatment process as claimed in claim 1, is characterized in that: by induction stirring in the acidleach process in described step 5, rotating speed is 0 ~ 400r/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324336A (en) * | 2017-09-01 | 2017-11-07 | 攀钢集团研究院有限公司 | A kind of method that acid-dissolved titanium slag prepares titanium carbide |
| CN107904408A (en) * | 2017-11-13 | 2018-04-13 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of production method for the titanium carbide slag for being used to prepare titanium tetrachloride |
| CN111744677A (en) * | 2020-07-02 | 2020-10-09 | 沈阳五寰工程技术有限公司 | Acid pretreatment-flotation separation method for pyroxene type ilmenite |
| CN113355529A (en) * | 2021-06-15 | 2021-09-07 | 北京科技大学 | Method for enriching metal titanium from titanium-containing blast furnace slag |
| CN114472464A (en) * | 2022-01-14 | 2022-05-13 | 江苏大学 | Method for efficiently recycling iron and phosphorus resources in phosphorus-containing steel slag |
| CN114789086A (en) * | 2022-04-27 | 2022-07-26 | 长沙矿冶研究院有限责任公司 | Flotation method for corrosion pretreatment of low-grade refractory ilmenite |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324336A (en) * | 2017-09-01 | 2017-11-07 | 攀钢集团研究院有限公司 | A kind of method that acid-dissolved titanium slag prepares titanium carbide |
| CN107904408A (en) * | 2017-11-13 | 2018-04-13 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of production method for the titanium carbide slag for being used to prepare titanium tetrachloride |
| CN111744677A (en) * | 2020-07-02 | 2020-10-09 | 沈阳五寰工程技术有限公司 | Acid pretreatment-flotation separation method for pyroxene type ilmenite |
| CN111744677B (en) * | 2020-07-02 | 2022-06-17 | 沈阳五寰工程技术有限公司 | Acid pretreatment-flotation separation method for pyroxene type ilmenite |
| CN113355529A (en) * | 2021-06-15 | 2021-09-07 | 北京科技大学 | Method for enriching metal titanium from titanium-containing blast furnace slag |
| CN114472464A (en) * | 2022-01-14 | 2022-05-13 | 江苏大学 | Method for efficiently recycling iron and phosphorus resources in phosphorus-containing steel slag |
| CN114789086A (en) * | 2022-04-27 | 2022-07-26 | 长沙矿冶研究院有限责任公司 | Flotation method for corrosion pretreatment of low-grade refractory ilmenite |
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