CN101187042A - Method for preparing TiC mTiO sosoloid using titanium complex ore as material - Google Patents
Method for preparing TiC mTiO sosoloid using titanium complex ore as material Download PDFInfo
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Abstract
The invention relates to a method of making TiC,mTiO sosoloid by using a plurality of common titanium complex ores as raw materials, such as rutile, high-titanium slag, titanium concentrate, ilmenite rock mine, ilmenite placer, rich ferrotitanium concentrate ore and the like. The invention is characterized in that titanium complex ores and a proportion of carbonaceous materials of carbite, coke and coal are uniformly mixed and reacted in the device with hot vacuum or inert gas and then the product is separated and purified after wet treatment, and at last achieve high-purity TiC,mTiO(0<=m<infinity) sosoloid. The technical procedures of the invention are that carbonaceous materials are utilized to deacidize titanium complex ores at a temperature of 1000-2000 DEG C under the protection of the vacuum or inert gas. To ensure the purity and the utilization ratio of the product, titanium complex ores and carbonaceous materials are uniformly mixed at a certain proportion and the mixture rich in TiC,mTiO is achieved, the product with more than 95% content of TiC,mTiO is achieved after acid pickling and alkali washing. The method has the advantages of strong application of material, short technological process, simple device, small investment, fast effect, low energy consumption and continuous production and the like.
Description
Technical field
The invention belongs to the nonferrous metallurgy field, particularly a kind of method of producing TiCmTiO sosoloid from multiple titanium oxide complex ore.
Background technology
Titanium and alloy thereof have excellent properties such as density is little, corrosion-resistant, high temperature resistant.It is the single-mode of principal market that world's titanium industry is just being experienced with aerospace, to civil areas such as metallurgy, the energy, traffic, chemical industry, biological medicine attach most importance to the development the multi-mode transition.The country that can carry out the titanium suitability for industrialized production at present in the world has only a few countries such as the U.S., Japan, Russia, China, and world's gross annual output amount of titanium only has tens0000 tons.But because the great strategic value of titanium and the status in national economy, titanium will become " the 3rd metal " that emerges after iron, aluminium, and 21 century will be the century of titanium.
Along with the growth of world's titanium industry, China's titanium industry also presents the fast-developing impetus.But under the impetus of this high growth, titanium sponge but becomes the bottleneck of restriction titanium processing.
The method of current industrial production titanium sponge is magnesium reduction process (Kroll method) and sodium thermoreduction method (Hunter method).Because the Hunter method is than Kroll method production cost height, so have only the Kroll method in industry-wide method at present.
World's titanium industry is through the development of decades, although Kroll method and Hunter method have been carried out a series of improvement, they all are periodical operation, and little improvement can not reduce the price of titanium significantly.Therefore should develop new, continuous process could fundamentally solve this problem of high production cost cheaply.For this reason, the researchist has carried out a large amount of experiments and research.
2004, people such as the Zhu Hongmin of University of Science ﹠ Technology, Beijing proposed with a kind of pure titanium of the direct electrolytic preparation of sosoloid anode TiOmTiC with metallic conductivity method (USTB titanium metallurgical technology).Its principal feature is: with carbon and titanium dioxide or titanium carbide and titanium dioxide is raw material, be mixed into powder by the chemical reaction metering, compression moulding then, in 600～1600 ℃ temperature range, vacuum reaction is made TiOmTiC (0≤m≤1) anode with metallic conduction performance.Halogenide fused salt with basic metal or alkaline-earth metal is an electrolytic solution then, electrolysis under 400～1000 ℃ of temperature: contained carbon and the oxygen of anode forms hydrocarbon gas CO, CO in the electrolytic process
2Gas or oxygen are emitted, and titanium enters fused salt and obtains pure titanium in cathodic deposition with the low price ionic species simultaneously.USTB technology is produced metal titanium and is laid a good foundation for low-cost, pollution-free, serialization.Yet the low cost of being conceived to, scale operation metal titanium need utilize low-grade titanium dioxide resource, and set up the reasonable process route from mineral to the product.
Summary of the invention
The objective of the invention is the direct method (USTB titanium metallurgical technology) of the pure titanium of electrolytic preparation based on a kind of sosoloid anode TiOmTiC (0≤m≤1) with metallic conductivity, purpose is to be raw material with low-grade oxidation titanium ore, through pyrotic smelting, wet method leaches to be handled, preparation TiCmTiO sosoloid, thereby, make USTB titanium metallurgical technology have more wide prospect in industrial application for low-cost, scale operation metal titanium provide practical way.
A kind ofly prepare the method for TiCmTiO sosoloid with the titanium complex ore, it is characterized in that: the titanium oxide content scope is 12～98% in the titanium complex ore, and all iron content is 0.2% to 55%, and all the other are MgO, CaO, SiO
2, Al
2O
3Deng, wherein MgO content is 0～8%, CaO content is 0～10%, SiO
2Content is 0～10%, Al
2O
3Content is 0～5%, and its summation is no more than 20%, and different raw materials are equipped with the carbonaceous material of different content.Wherein adopting rutile concentrate titanium oxide is 92～98%, and all iron content is 0.2% to 6%, and all the other are MgO, CaO, SiO
2, Al
2O
3Deng impurity, carbonaceous material carbon content proportioning is 28～44% of a rutile concentrate weight.Titanium slag titanium oxide content scope is 60～98%, and all iron content scope is 1% to 30%, and all the other are MgO, CaO, SiO
2, Al
2O
3Deng impurity, carbonaceous material carbon content proportioning is 15～60% of a titanium slag weight.Ilmenite concentrate, ilmenite rock ore deposit or ilmenite placer titanium oxide content scope are 40～70%, and all iron content scope is 35～50%, and all the other are MgO, CaO, SiO
2, Al
2O
3Deng impurity, carbonaceous material carbon content proportioning is 15～45% of ilmenite concentrate, ilmenite rock ore deposit or a placer weight.Rich concentrated ilmenite titanium oxide content scope is 12 ± 3%, and all iron content scope is 45～55%, and all the other are MgO, CaO, SiO2, Al
2O
3Deng impurity, carbonaceous material carbon content proportioning is 15～38% of a rich concentrated ilmenite weight.According to said ratio with various rich titanium materials and carbonaceous material uniform mixing; under the condition of vacuum or protection of inert gas; temperature range internal heating in 1000～2000 ℃; after homo(io)thermism; be incubated 0.5～8 hour; reduction titanium complex ore obtains being rich in mixture or mixture and iron shot or the iron block of TiCmTiO.
With iron shot or iron block with after mixture screening of being rich in TiCmTiO or layering separate, obtain being rich in mixture crushing and screening to 44～150 of being rich in TiCmTiO that directly obtain after the mixture product of TiCmTiO or the reduction micron, 44～150 microns content will account for the mixture product more than 40～90%, be 1～40% hydrochloric acid then with the mixture product concentration behind the crushing and screening, phosphoric acid, one or more mixing acid washings in the hydrofluoric acid 1～5 time, each washing time 1～120 minute, liquid-solid ratio 2～30,10～2000 revolutions per seconds of stir speed (S.S.)s, extraction temperature are 15～100 ℃; Filter and dry gained filter residue, promptly obtain TiCmTiO content greater than 95% powder.
The principle of the inventive method is: the complex ore that contains titanium dioxide is with in certain stoichiometric ratio and the carbonaceous material reaction process, ferriferous oxide and carbon reaction generate metallic iron, titanium dioxide and carbon reaction generate TiCmTiO sosoloid, above-mentioned reaction has precedence over the oxide compound of other silicon, magnesium, calcium, aluminium etc. and the reaction of carbon, thereby other oxide compound generates metallurgical slag.Difference according to iron, slag and TiCmTiO sosoloid physicochemical property, iron forms iron shot or iron block and separates by screening or layering, TiCmTiO sosoloid is insoluble to alkali such as mineral acids such as hydrochloric acid, phosphoric acid and hydrofluoric acid and NaOH, and slag is dissolved in acid or alkali, therefore can they be separated by the method for wet method stripping, thereby obtain highly purified TiCmTiO sosoloid.
The advantage of the inventive method is: adaptability to raw material is strong, and technical process is short, and equipment is simple, invest little, instant effect, energy consumption is low, can be continuously produced etc., has boundless prospects for commercial application.
Description of drawings
The SEM Electronic Speculum shape appearance figure of the TiCTiO sosoloid that Fig. 1 prepares for certain rutile concentrate of example 1 usefulness of the present invention.
The x-ray diffraction pattern of the TiCTiO sosoloid that Fig. 2 prepares for certain titanium slag of example 3 usefulness of the present invention.
The x-ray diffraction pattern of the TiC2TiO sosoloid that Fig. 3 prepares for certain ilmenite concentrate of example 4 usefulness of the present invention.
The x-ray diffraction pattern of the 2TiCTiO sosoloid that Fig. 4 prepares for certain ilmenite rock ore deposit of example 5 usefulness of the present invention.
The x-ray diffraction pattern of the TiC that Fig. 5 prepares for certain ilmenite placer of example 6 usefulness of the present invention.
The x-ray diffraction pattern of the TiO that Fig. 6 prepares for certain titanium slag of example 8 usefulness of the present invention.
The SEM Electronic Speculum shape appearance figure of the TiCTiO sosoloid that Fig. 7 prepares for certain ilmenite rock ore deposit of example 10 usefulness of the present invention.
Fig. 8 titanium complex ore prepares the process flow sheet of TiCmTiO sosoloid.
Embodiment
Take by weighing rutile concentrate 200 grams, its composition is 95.96%TiO
2, 1%Fe
2O
3, all the other are trace, restrain than weighing Graphite Powder 99 58.68 according to following chemical reaction metering:
Fe
2O
3+3C＝2Fe+3CO
TiO
2+4C＝TiC·TiO+3CO
Mix, place plumbago crucible, under vacuum, reacted 5 hours down, obtain being rich in the mixture of TiCTiO in 1400 ℃.With the mixture fragmentation, levigately account for 90% to 44～150 microns.Use the dilute hydrochloric acid impregnation product, 80 ℃ of dipping temperatures, dipping time 100 minutes, liquid-solid ratio 16: 1, concentration of hydrochloric acid 20%, 80 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 1 time, obtaining TiCTiO sosoloid (ultimate analysis carbon Sauerstoffatom ratio is 1: 1.02) content is 97.92% powder again.
Embodiment 2
Take by weighing rutile concentrate 200 grams, its composition is 97.13%TiO
2, 0.9%Fe
2O
3, all the other are trace, restrain than weighing Graphite Powder 99 87.82 according to following chemical reaction metering:
Fe
2O
3+3C＝2Fe+3CO
TiO
2+3C＝TiC+2CO
It is mixed, place plumbago crucible, under argon shield, reacted 8 hours down, obtain being rich in the mixture of TiC in 1500 ℃.With the mixture fragmentation, levigately account for 90% to 44～150 microns.Use the dilute hydrochloric acid impregnation product, 60 ℃ of dipping temperatures, dipping time 60 minutes, liquid-solid ratio 12: 1, concentration of hydrochloric acid 15%, 100 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 1 time, obtaining TiC (ultimate analysis carbon Sauerstoffatom ratio is 1: 0.02) content is 98.15% powder again.
Embodiment 3
Take by weighing titanium slag 200 grams, its composition is 77.26%TiO
2, 10.28%FeO, 5.68%MgO, 3.21%SiO
2, 1.69%CaO, 1.26%Al
2O
3, restrain than weighing Graphite Powder 99 49.78 according to following chemical reaction metering:
FeO+C＝Fe+CO
2TiO
2+4C＝TiC·TiO+3CO
It is mixed, place plumbago crucible, under argon shield, reacted 4 hours down, obtain being rich in the mixture of TiCTiO in 1500 ℃.With this mixture fragmentation, levigately account for 90% to 44～150 microns.Use the dilute hydrochloric acid impregnation product, 90 ℃ of dipping temperatures, dipping time 60 minutes, liquid-solid ratio 20: 1, concentration of hydrochloric acid 15%, 100 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 2 times, finally obtaining TiCTiO sosoloid (ultimate analysis shows that carbon Sauerstoffatom ratio is 1: 1.03) content is 95.38%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.33%, 0.51%, 0.65%, 0.07%, 1.31% powder.
Embodiment 4
Take by weighing ilmenite concentrate 200 grams, its composition is 47.60%TiO
2, 31.00% full Fe, 29.23%FeO, 11.02%Fe
2O
3, 5.81%MgO, 3.32%SiO
2, 1.48%CaO, 1.52%Al
2O
3, restrain than weighing Graphite Powder 99 38.50 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
3TiO
2+5C＝TiC·2TiO+4CO
It is mixed, place plumbago crucible, under vacuum, reacted 4 hours down, obtain being rich in mixture and the iron block of TiC2TiO in 1700 ℃.With iron block with after mixture separates, with the mixture fragmentation, levigately account for 90% to 44～150 microns.Use the diluted hydrofluoric acid impregnation product, 60 ℃ of dipping temperatures, dipping time 90 minutes, liquid-solid ratio 15: 1, hydrofluoric acid concentration 12%, 80 revolutions per seconds of stirring velocitys.Filter and the oven dry product, again with similarity condition washing 1 time, with 1 time (other condition is constant) of 30%NaOH washing, obtaining TiC2TiO sosoloid (ultimate analysis shows that carbon Sauerstoffatom ratio is 1: 2.09) content is 96.78%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.36%, 0.63%, 0.62%, 0.06%, 1.60% powder.(wherein soda acid wash sequencing can change)
Embodiment 5
Take by weighing ilmenite rock ore deposit 200 grams, its composition is 46.87%TiO
2, 30.83% full Fe, 31.63%FeO, 9.02%Fe
2O
3, 5.60%MgO, 3.22%SiO
2, 1.61%CaO, 1.86%Al
2O
3, restrain than weighing Graphite Powder 99 47.41 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
3TiO
2+7C＝2TiC·TiO+5CO
It is mixed, place plumbago crucible, under argon shield, reacted 8 hours down, obtain being rich in mixture and the iron shot of 2TiCTiO in 1400 ℃.With iron shot with after mixture separates, with mixture fragmentation, levigate to 44～150 microns.With the mixing acid impregnation product of dilute hydrochloric acid and hydrofluoric acid, 60 ℃ of dipping temperatures, dipping time 80 minutes, liquid-solid ratio 8: 1, concentration of hydrochloric acid 20%, hydrofluoric acid concentration 15%, volume ratio is 3: 1,8 revolutions per seconds of stirring velocitys.Filter and the oven dry product, again with similarity condition washing 1 time, with 1 time (other condition is constant) of 20%KOH washing, obtaining 2TiCTiO sosoloid (ultimate analysis shows that carbon Sauerstoffatom ratio is 2: 1.08) content is 96.74%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.36%, 0.74%, 0.68%, 0.07%, 1.91% powder.(wherein soda acid wash sequencing can change)
Embodiment 6
Take by weighing ilmenite placer 200 grams, its composition is 61.65%TiO
2, 24.97% full Fe, 5.78%FeO, 29.30%Fe
2O
3, 0.12%MgO, 0.77%SiO
2, 0.10%CaO, 1.15%Al
2O
3, restrain than weighing Graphite Powder 99 70.60 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
TiO
2+3C＝TiC+2CO
It is mixed, place plumbago crucible, under argon shield, reacted 8 hours down, obtain being rich in mixture and the iron shot of TiC in 1500 ℃.With iron shot with after mixture separates, with mixture fragmentation, levigate to 44～150 microns.Use the diluted hydrofluoric acid impregnation product, 40 ℃ of dipping temperatures, dipping time 100 minutes, liquid-solid ratio 12: 1, hydrofluoric acid concentration 30%, 2 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 1 time, obtaining TiC (ultimate analysis shows that carbon Sauerstoffatom ratio is 1: 0.03) content is 97.55%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.31%, 0.47%, 0.42%, 0.04%, 1.21% powder.
Embodiment 7
Take by weighing rich concentrated ilmenite 200 grams, its composition is 12.46%TiO
2, 51.16% full Fe, 30.78%FeO, 39.04%Fe
2O
3, 5.78%MgO, 4.26%SiO
2, 3.69%CaO, 3.02%Al
2O
3, restrain than weighing Graphite Powder 99 35.30 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
2TiO
2+4C＝TiC·TiO+3CO
It is mixed, place plumbago crucible, under argon shield, reacted 6 hours down, obtain being rich in mixture and the iron shot of TiCTiO in 1500 ℃.With iron shot with after mixture separates, with mixture fragmentation, levigate to 44～150 microns.Use the dilute hydrochloric acid impregnation product, 40 ℃ of dipping temperatures, dipping time 120 minutes, liquid-solid ratio 25: 1, concentration of hydrochloric acid 10%, 6 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 1 time, use 40%Na more again
2CO
3Wash 1 time (other condition is constant), obtaining TiCTiO (ultimate analysis carbon Sauerstoffatom ratio is 1: 1.26) sosoloid content is 95.04%, FeO, MgO, SiO
2, CaO, Al
2O
3Content is respectively 0.30%, 1.12%, 0.41%, 0.05%, 3.08% powder.(wherein soda acid wash sequencing can change)
Embodiment 8
Take by weighing titanium slag 200 grams, its composition is 76.86%TiO
2, 11.64%FeO, 5.18%MgO, 3.22%SiO
2, 1.71%CaO, 1.39%Al
2O
3, restrain than weighing Graphite Powder 99 26.94 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
TiO
2+C＝TiO+CO
It is mixed, place plumbago crucible, under vacuum, reacted 4 hours down, obtain being rich in the mixture of TiO in 1800 ℃.With this mixture fragmentation, levigately account for 80% to 44～150 microns.Use the dilute phosphoric acid impregnation product, 60 ℃ of dipping temperatures, dipping time 100 minutes, liquid-solid ratio 10: 1, phosphoric acid concentration 18%, 30 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 1 time, obtaining TiO (ultimate analysis carbon Sauerstoffatom ratio is 0.03: 1) content is 97.13%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.34%, 0.57%, 0.45%, 0.06%, 1.45% powder.
Embodiment 9
Take by weighing ilmenite concentrate 200 grams, its composition is 48.46%TiO
2, 30.75% full Fe, 30.26%FeO, 10.42%Fe
2O
3, 5.38%MgO, 3.79%SiO
2, 1.96%CaO, 1.83%Al
2O
3, restrain than weighing Graphite Powder 99 26.94 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
3TiO
2+7C＝2TiC·TiO+5CO
It is mixed, place plumbago crucible, under argon shield, reacted 3 hours down, obtain being rich in mixture and the iron block of 2TiCTiO in 1600 ℃.With iron block with after mixture separates, with the mixture fragmentation, levigately account for 85% to 44～150 microns.Use the dilute phosphoric acid impregnation product, 50 ℃ of dipping temperatures, dipping time 40 minutes, liquid-solid ratio 20: 1, phosphoric acid concentration 25%, 60 revolutions per seconds of stirring velocitys.Filter and the oven dry product, again with similarity condition washing 1 time, with 1 time (other condition is constant) of 25%NaOH washing, obtaining 2TiCTiO sosoloid (ultimate analysis carbon Sauerstoffatom ratio is 2: 1.07) content is 96.39%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.36%, 0.75%, 0.51%, 0.07%, 1.92% powder.(wherein soda acid wash sequencing can change)
Take by weighing ilmenite rock ore deposit 200 grams, its composition is 47.83%TiO
2, 32.16% full Fe, 33.16%FeO, 9.23%Fe
2O
3, 4.58%MgO, 2.76%SiO
2, 1.08%CaO, 1.96%Al
2O
3, restrain than weighing Graphite Powder 99 43.90 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
2TiO
2+4C＝TiC·TiO+3CO
It is mixed, place plumbago crucible, under vacuum, reacted 4 hours down, obtain being rich in mixture and the iron shot of TiCTiO in 1600 ℃.With iron shot with after mixture separates, with the mixture fragmentation, levigately account for 90% to 44～150 microns.Use the dilute phosphoric acid impregnation product, 50 ℃ of dipping temperatures, dipping time 60 minutes, liquid-solid ratio 18: 1, phosphoric acid concentration 22%, 70 revolutions per seconds of stirring velocitys.Filter and oven dry product with similarity condition washing 1 time, are used 35%Na more again
2CO
3Wash 1 time (other condition is constant), obtaining TiCTiO sosoloid (ultimate analysis carbon Sauerstoffatom ratio is 1: 1.12) content is 96.21%, FeO, MgO, SiO
2, CaO, Al
2O
3Content is respectively 0.34%, 0.81%, 0.52%, 0.06%, 2.06% powder.(wherein soda acid wash sequencing can change)
Embodiment 11
Take by weighing ilmenite placer 200 grams, 60.06%TiO
2, 25.07% full Fe, 6.17%FeO, 29.01%Fe
2O
3, 1.16%MgO, 1.06%SiO
2, 0.32%CaO, 1.26%Al
2O
3, restrain than weighing Graphite Powder 99 51.15 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
2TiO
2+4C＝TiC·TiO+3CO
It is mixed, place plumbago crucible, under vacuum, reacted 5 hours down, obtain being rich in mixture and the iron shot of TiCTiO in 1550 ℃.With iron shot with after mixture separates, with the mixture fragmentation, levigately account for 85% to 44～150 microns.Use the dilute hydrochloric acid impregnation product, 70 ℃ of dipping temperatures, dipping time 120 minutes, liquid-solid ratio 12: 1, concentration of hydrochloric acid 10%, 40 revolutions per seconds of stirring velocitys.Filter and the oven dry product, again with similarity condition washing 1 time, with 1 time (other condition is constant) of 15%NaOH washing, obtaining TiCTiO sosoloid (ultimate analysis carbon Sauerstoffatom ratio is 1: 1.08) content is 97.22%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.31%, 0.52%, 0.57%, 0.06%, 1.32% powder.(wherein soda acid wash sequencing can change)
Embodiment 12
Take by weighing rich concentrated ilmenite 200 grams, its composition is 13.12%TiO
2, 52.66% full Fe, 32.27%FeO, 39.53%Fe
2O
3, 5.16%MgO, 4.86%SiO
2, 3.91%CaO, 2.86%Al
2O
3, restrain than weighing Graphite Powder 99 40.35 according to following chemical reaction metering:
FeO+C＝Fe+CO
Fe
2O
3+3C＝2Fe+3CO
TiO
2+3C＝TiC+2CO
It is mixed, place plumbago crucible, under vacuum, reacted 8 hours down, obtain being rich in mixture and the iron shot of TiC in 1450 ℃.With iron shot with after mixture separates, with the mixture fragmentation, levigately account for 90% to 44～150 microns.Use the dilute hydrochloric acid impregnation product, 80 ℃ of dipping temperatures, dipping time 100 minutes, liquid-solid ratio 16: 1, concentration of hydrochloric acid 20%, 80 revolutions per seconds of stirring velocitys.Filter and the oven dry product, with similarity condition washing 1 time, obtaining TiC (ultimate analysis carbon Sauerstoffatom ratio is 1: 0.21) content is 95.02%, FeO, MgO, SiO again
2, CaO, Al
2O
3Content is respectively 0.32%, 1.14%, 0.53%, 0.07%, 2.92% powder.
Claims (2)
1. one kind prepares the method for TiCmTiO sosoloid with the titanium complex ore, and it is characterized in that ingredient requirement: the titanium oxide content scope is 12～98% in the titanium complex ore, and all iron content is 0 2% to 55%, and MgO content is 0～8%, and CaO content is 0～10%, SiO
2Content is 0～10%, Al
2O
3Content is 0～5%, MgO, CaO, SiO
2, Al
2O
3Summation is no more than 20%; Be equipped with the carbonaceous material of different content for different raw materials, adopting rutile concentrate titanium is raw material, and require: oxide compound is 92～98%, and all iron content is 0.2% to 6%, and all the other are MgO, CaO, SiO
2, Al
2O
3And impurity, carbonaceous material carbon content proportioning is 28～44% of a rutile concentrate weight; The employing titanium slag is a raw material, and require: the titanium oxide content scope is 60～98%, and all iron content scope is 1% to 30%, and all the other are MgO, CaO, SiO
2, Al
2O
3And impurity, carbonaceous material carbon content proportioning is 15～60% of a titanium slag weight; Adopting ilmenite concentrate, ilmenite rock ore deposit or ilmenite placer is raw material: require: the titanium oxide content scope is 40～70%, and all iron content scope is 35～50%, and all the other are MgO, CaO, SiO
2, Al
2O
3And impurity, carbonaceous material carbon content proportioning is 15～45% of ilmenite concentrate, ilmenite rock ore deposit or a placer weight; Adopting rich concentrated ilmenite is raw material, and require: the titanium oxide content scope is 12 ± 3%, and all iron content scope is 45～55%, and all the other are MgO, CaO, SiO
2, Al
2O
3And impurity, carbonaceous material carbon content proportioning is 15～38% of a rich concentrated ilmenite weight.
2. a kind of according to claim 1 method for preparing TiCmTiO sosoloid with the titanium complex ore, it is characterized in that working method is: according to the described proportioning raw materials of claim 1, with various rich titanium materials and carbonaceous material uniform mixing, under the condition of vacuum or protection of inert gas, in 1000～2000 ℃ temperature range internal heating, after homo(io)thermism, be incubated 0.5～8 hour, reduction titanium complex ore obtains being rich in mixture or mixture and iron shot or the iron block of TiCmTiO;
Mixture crushing and screening to 44～150 of being rich in TiCmTiO that iron shot or iron block and being rich in of obtaining after mixture screening of being rich in TiCmTiO or layering separate are directly obtained after TiCmTiO mixture product or the reduction micron, 44～150 microns content will account for the mixture product more than 40～90%, be 1～40% hydrochloric acid then with the mixture product concentration behind the crushing and screening, phosphoric acid, one or more mixing acid washings in the hydrofluoric acid 1～5 time, each washing time 1～120 minute, liquid-solid ratio 2～30,10～2000 revolutions per seconds of stir speed (S.S.)s, extraction temperature are 15～100 ℃; Filter and dry gained filter residue, promptly obtain TiCmTiO content greater than 95% powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101216817A CN101187042A (en) | 2007-09-12 | 2007-09-12 | Method for preparing TiC mTiO sosoloid using titanium complex ore as material |
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| CNA2007101216817A CN101187042A (en) | 2007-09-12 | 2007-09-12 | Method for preparing TiC mTiO sosoloid using titanium complex ore as material |
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| CNA2007101216817A Pending CN101187042A (en) | 2007-09-12 | 2007-09-12 | Method for preparing TiC mTiO sosoloid using titanium complex ore as material |
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Cited By (10)
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| CN101914788A (en) * | 2010-07-26 | 2010-12-15 | 攀钢集团有限公司 | Method for preparing metallic titanium |
| CN101947652A (en) * | 2010-09-21 | 2011-01-19 | 攀钢集团有限公司 | Method for preparing C-O-T (carbon-oxygen-titanium) composite anode by microwave heating |
| CN103305875A (en) * | 2013-06-27 | 2013-09-18 | 中国铝业股份有限公司 | Preparation method for preparing anode of metallic titanium by molten salt electrolysis |
| CN103966455A (en) * | 2014-05-16 | 2014-08-06 | 北京科技大学 | Method for extracting titanium from titanium-containing blast furnace slag by aluminothermy |
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| CN101914788A (en) * | 2010-07-26 | 2010-12-15 | 攀钢集团有限公司 | Method for preparing metallic titanium |
| CN101914788B (en) * | 2010-07-26 | 2012-10-03 | 攀钢集团有限公司 | Method for preparing metallic titanium |
| CN101947652A (en) * | 2010-09-21 | 2011-01-19 | 攀钢集团有限公司 | Method for preparing C-O-T (carbon-oxygen-titanium) composite anode by microwave heating |
| CN103305875A (en) * | 2013-06-27 | 2013-09-18 | 中国铝业股份有限公司 | Preparation method for preparing anode of metallic titanium by molten salt electrolysis |
| CN103966455A (en) * | 2014-05-16 | 2014-08-06 | 北京科技大学 | Method for extracting titanium from titanium-containing blast furnace slag by aluminothermy |
| CN103966429A (en) * | 2014-05-26 | 2014-08-06 | 重庆大学 | Method for preparing chloride titanium slag from high-calcium-magnesium titanium concentrate |
| CN104120457A (en) * | 2014-07-10 | 2014-10-29 | 上海大学 | Preparing method of metal-carbide-containing multi-layer multi-component composite material |
| CN104120457B (en) * | 2014-07-10 | 2016-11-23 | 上海大学 | Preparation method containing metal carbides multilamellar multicomponent composite materials |
| CN104451781A (en) * | 2014-12-08 | 2015-03-25 | 中国铝业股份有限公司 | Preparation method of anode for producing metallic titanium by electrolysis |
| CN104498734A (en) * | 2015-01-09 | 2015-04-08 | 重庆大学 | Titanium recovery treatment method for titanium-bearing blast furnace slag based on vacuum carbothermal reduction |
| WO2020098176A1 (en) * | 2018-11-16 | 2020-05-22 | 北京科技大学 | Carbonized/sulfurized ferrotitanium complex ore anode-electrolytic method for preparing metallic titanium |
| US11473207B2 (en) | 2018-11-16 | 2022-10-18 | University Of Science And Technology Beijing | Preparing method for titanium of Ti—C—S anode by carbonized/sulfurized ilmenite |
| WO2023105180A1 (en) * | 2021-12-07 | 2023-06-15 | Chinuka Ltd | Treatment of metal ores |
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