CN103008098A - Solid phase reinforcement reduction-magnetic separation method of vanadium titano-magnetite - Google Patents
Solid phase reinforcement reduction-magnetic separation method of vanadium titano-magnetite Download PDFInfo
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- CN103008098A CN103008098A CN2012105695898A CN201210569589A CN103008098A CN 103008098 A CN103008098 A CN 103008098A CN 2012105695898 A CN2012105695898 A CN 2012105695898A CN 201210569589 A CN201210569589 A CN 201210569589A CN 103008098 A CN103008098 A CN 103008098A
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- magnetite
- iron powder
- iron
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Abstract
The invention belongs to the non-blast furnace smelting field of vanadium titano-magnetite, and specifically relates to a solid phase reinforcement reduction-magnetic separation method of the vanadium titano-magnetite. The method comprises the steps of mixing the vanadium titano-magnetite and anthracite duff, adding additives of CsF2, Na2CO3 or Fe2O3, mixing the above materials uniformly, adding a binding agent, mold pressing into a cylindrical sample, reducing the cylindrical sample for 30-120 min at a temperature of 1,100-1,400 DEG C to obtain reduced iron powder, cooling the reduced iron powder by water quenching or naturally cooling to a room temperature, grinding fine, and magnetic separating to obtain iron powder with a recovery rate of 94-97%. The method is simple in operation, reduces energy consumption and saves cost by replacing coke by the anthracite, and promotes growth of iron crystals after adding CsF2, Fe2O3 and Na2CO3, thereby increasing metallization ratio. At the same time, the method facilitates slag-iron separation. Water quenching after reduction can prevent the reduced metal iron and iron suboxide from being re-oxidized into iron oxide, enabling the metallization ratio to be between 86%-98% and the iron recovery rate to reach 94-97%.
Description
Technical field
The invention belongs to the non-blast furnace process of vanadium titano-magnetite field, be specifically related to a kind of vanadium titano-magnetite solid phase and strengthen the method that reduction-magnetic separation separates.
Background technology
World's vanadium titano-magnetite is identified to be had more than 40,000,000,000 tons, mainly is distributed in the countries such as China, Russia, the U.S., South Africa, Canada.There is abundant v-ti magnetite ore resources in China, mainly is distributed in Pan Xi and Chengde area, and wherein the explored prospective reserves of Panxi Diqu surpasses 10,000,000,000 tons, and the explored reserves of Chengde area are above 8,000,000,000 tons.
Vanadium titano-magnetite is a kind of polynary mineral intergrowth, mainly take iron, vanadium, titanium as main, and with valuable elements such as chromium, brill, nickel, copper, anti-, gallium and platinum family elements, therefore v-bearing titanomagnetite smelting can not only obtain metallic iron, also can obtain the valuable elements such as vanadium, titanium, chromium, this uses for vanadium titano-magnetite diversification is provided.Vanadium titano-magnetite mainly is blast furnace process at home, but because the limitation of self, the sticking tank of molten iron can appear in smelting vanadium-titanium magnetite by blast furnace, iron loss is high, deslagging is difficult and the phenomenon such as foamed slag, a kind of difficult mineral of smelting, cause being difficult to realizing on a large scale blast furnace process, and along with the continuous consumption of coke in the world wide, the cost of blast furnace ironmaking also is to increase year by year.Therefore, the non-blast furnace process of vanadium titano-magnetite, especially vanadium titano-magnetite coal-based direct reduction have a very large development space.
DRI is to be lower than under the ore fusion temperature, iron ore is refined into the technical process of iron by solid state reduction, immature in domestic DRI technology, the degree of metalization of iron is not high, the defectives such as production cost height, cause the domestic output of only having about 400,000 tons, well below external more than 7,000 ten thousand tons output, this has seriously restricted the development of the industries such as electric furnace steel making.Therefore, strengthening direct-reduction is very important means that promote the DRI technical development.
Summary of the invention
For the problem that prior art exists, the invention provides a kind of vanadium titano-magnetite solid phase and strengthen the method that reduction-magnetic separation separates, purpose is degree of metalization and the rate of recovery of raising iron, so that iron, vanadium, titanium can better separate.
The technical scheme of realization the object of the invention is carried out according to following steps:
(1) be (1.1 ~ 1.4) with vanadium titano-magnetite and anchracite duff according to the C/O mol ratio: 1 ratio batching, the mixed compound that forms adds the addition of C aF that accounts for mixture quality 1 ~ 7% in compound in ball mill
2, Na
2CO
3Or Fe
2O
3, add the binding agent that accounts for mixture quality 0.1 ~ 0.2% behind the mixing, under the pressure of 30 ~ 60MPa, be molded into cylindric sample;
(2) cylindric sample being imbedded in the crucible that fills anchracite duff, is 30 ~ 120min in 1100 ~ 1400 ℃ of recovery times, obtains reduced iron powder;
(3) with reduced iron powder shrend cooling or naturally cool to room temperature, with pulverizer reduzate is milled down to 100～300 orders, obtain levigate reduced iron powder;
(4) with the magnetic separation under the magnetic separation strength of 120 ~ 240kA/m of levigate reduced iron powder, scum separates, and the rate of being recycled is 94 ~ 97% iron powder.
Described binding agent is polyvinyl alcohol, and its molecular formula is [C
2H
4O]
n
Characteristics of the present invention and beneficial effect are:
Principle of the present invention is can generate fayalite (2FeO ﹒ SiO in reduction process
2) and hercynite (FeO ﹒ Al
2O
3) etc. complex compound, along with the rising of temperature, this class material can melt, thereby stops up pore, hinders the interior diffusion of gas.Add CaF
2And Na
2CO
3CaO and Na can appear
2O displaces the FeO in the complex compound, has improved the activity of FeO, has promoted the reduction of iron; F
-Ion enters into the network that Si-O tetrahedron forms, and destroys Si-O tetrahedral structure, makes distortion of lattice, reduces reaction activity, has promoted reduction; Na in reducing atmosphere
2CO
3Can generate gaseous metal sodium, enter into easily floating scholar's body lattice, cause distortion of lattice, sodium metal has the effect of nucleating agent simultaneously, so that the nucleus of iron forms easily and grow up, and the present invention adds CaF before reduction
2, Na
2CO
3Or Fe
2O
3The self-fluxing nature additive is conducive to the formation of each phase, causes the expansion of boundary, and this is conducive to the absorption of gas and the raising of reaction rate, particularly works as Fe
2O
3Revert to Fe
3O
4The time, specific volume increases, and the swelling stress that sample is subject to increases, and cracks easily and micropore, has strengthened the interior diffusion of gas.
The inventive method adds reduction roasting behind the additive except vanadium titano-magnetite, also in cooling procedure, adopt nature cooling or Water Quenching, wherein shrend is in order to prevent that metallic iron is oxidized in the temperature drop process, its purpose is exactly for the degree of metalization that improves iron and promotes the iron grain growth, strengthen Direct Reduction, so that slag iron can better separate during magnetic separation, obtain high iron recovery and Ti slag.
The beneficial effect that adopts the inventive method to produce is: the present invention adopts the flow process of coal-based direct reduction-mill ore magnetic selection to reclaim iron, vanadium, titanium, and technological process is short, and is simple to operate, and replaced coke with anthracite, reduced energy consumption, saved cost; Add CaF
2, Fe
2O
3, Na
2CO
3After, promoted growing up of iron crystal grain, not only improved degree of metalization, be conducive to simultaneously slag iron and separate; After the reduction shrend can prevent the metallic iron that restores and at a low price ferriferous oxide be reoxidised into the high price ferriferous oxide so that degree of metalization is between 86～98%, iron recovery reaches 94～97%.
Description of drawings
Fig. 1 is the process chart of the inventive method;
Fig. 2 is the reduzate ore deposit phasor that the embodiment of the invention 3 obtains;
Fig. 3 is the reduzate ore deposit phasor that Comparative Examples obtains.
The specific embodiment
The chemical composition of the vanadium titano-magnetite described in the embodiment of the invention is: TFe58.61%, FeO27.63%, TiO
27.01%, SiO
23.2%, Al
2O
33.0%, MgO1.35%, CaO0.92%, V
2O
50.291 %, P0.028 %, S0.19%, surplus is impurity.
The present invention is further described below in conjunction with drawings and Examples.
Embodiment 1
(1) be the ratio batching of 1.1:1 with vanadium titano-magnetite and anchracite duff according to the C/O mol ratio, batch mixing in ball mill adds the additive Fe that accounts for mixture quality 7% in mixed material
2O
3, add the binding agent polyethylene glycol that accounts for mixture quality 0.1% behind the mixing, under the pressure of 40MPa, be molded into cylindric sample;
(2) cylindric sample being imbedded in the crucible that fills anchracite duff, is 120min in 1100 ℃ of recovery times, obtains reduced iron powder;
(3) the reduced iron powder shrend is cooled to room temperature, with 2M2-100 type sealed type sample pulverizer reduzate is milled down to 100～300 orders, obtain levigate reduced iron powder, degree of metalization is 86.53%;
(4) with the magnetic separation under the magnetic separation strength of 200kA/m of levigate reduced iron powder, the rate of being recycled is 96.12% iron powder, and its magnetic product component: TFe is that 81.14%, MFe is 73.56%, TiO
2Be that 4.33%, V is 0.274%; Non magnetic product component: TFe is that 7.07%, MFe is 0.96%, TiO
2Be that 15.05%, V is 0.638%, wherein have 56.90% V to enter into the magnetic product, 52.91% Ti enters into non magnetic product.
Embodiment 2
(1) be the ratio batching of 1.4:1 with vanadium titano-magnetite and anchracite duff according to the C/O mol ratio, batch mixing in ball mill adds the additive Na that accounts for mixture quality 3% in mixed material
2CO
3, add the binding agent polyethylene glycol that accounts for mixture quality 0.2% behind the mixing, under the pressure of 60MPa, be molded into cylindric sample;
(2) cylindric sample being imbedded in the crucible that fills anchracite duff, is 60min in 1350 ℃ of recovery times, obtains reduced iron powder;
(3) reduced iron powder is naturally cooled to room temperature, with 2M2-100 type sealed type sample pulverizer reduzate is milled down to 100～300 orders, obtain levigate reduced iron powder;
(4) with the magnetic separation under the magnetic separation strength of 120kA/m of levigate reduced iron powder, the rate of being recycled is 94.82% iron powder,
In the magnetic product: TFe is that 89.50%, MFe is 83.40%, TiO
2Be that 3.05%, V is 0.391%; In the non magnetic product: TFe is that 3.46%, MFe is 0.51%, TiO
2Be that 20.33%, V is 0.511%, wherein have 70.76% V to enter into the magnetic product, 68.03% Ti enters into non magnetic product.
Embodiment 3
(1) be the ratio batching of 1.2:1 with vanadium titano-magnetite and anchracite duff according to the C/O mol ratio, batch mixing in ball mill adds the addition of C aF that accounts for mixture quality 3% in mixed material
2, add the binding agent polyethylene glycol that accounts for mixture quality 0.15% behind the mixing, under the pressure of 50MPa, be molded into cylindric sample;
(2) cylindric sample being imbedded in the crucible that fills anchracite duff, is 30min in 1300 ℃ of recovery times, obtains reduced iron powder;
(3) reduced iron powder is naturally cooled to room temperature, with 2M2-100 type sealed type sample pulverizer reduzate is milled down to 100～300 orders, obtain levigate reduced iron powder, degree of metalization is 89.68%;
(4) with the magnetic separation under the magnetic separation strength of 160kA/m of levigate reduced iron powder, the rate of being recycled is 94.37% iron powder, its ore deposit phasor as shown in Figure 2, in its magnetic product: TFe is that 86.93%, MFe is 77.53%, TiO
2Be that 3.45%, V is 0.35%; In the non magnetic product: TFe is that 5.78%, MFe is 0.88%, TiO
2Be that 20.83%, V is 0.90%, wherein have 63.85% V to enter into the magnetic product, 66.34% Ti enters into non magnetic product.
Comparative Examples
(1) be the ratio batching of 1.2:1 with vanadium titano-magnetite and anchracite duff according to the C/O mol ratio, batch mixing in ball mill adds the addition of C aF that accounts for mixture quality 3% in mixed material
2, add the binding agent polyethylene glycol that accounts for mixture quality 0.15% behind the mixing, under the pressure of 50MPa, be molded into cylindric sample;
(2) cylindric sample being imbedded in the crucible that fills anchracite duff, is 30min in 1300 ℃ of recovery times, obtains reduced iron powder;
(3) the reduced iron powder shrend is cooled to room temperature, with 2M2-100 type sealed type sample pulverizer reduzate is milled down to 100～300 orders, obtain levigate reduced iron powder, degree of metalization is 97.75%;
(4) with the magnetic separation under the magnetic separation strength of 160kA/m of levigate reduced iron powder, the rate of being recycled is 95.02% iron powder, its ore deposit phasor as shown in Figure 3, in its magnetic product: TFe is that 92.04%, MFe is 87.89%, TiO
2Be that 2.05%, V is 0.416%; In the non magnetic product: TFe is that 2.89%, MFe is 1.30%, TiO
2Be that 26.17%, V is 0.577%, wherein have 70.15% V to enter into the magnetic product, 79.37% Ti enters into non magnetic product.
Claims (2)
1. a vanadium titano-magnetite solid phase is strengthened the method that reduction-magnetic separation separates, and it is characterized in that carrying out according to following steps:
(1) be (1.1 ~ 1.4) with vanadium titano-magnetite and anchracite duff according to the C/O mol ratio: 1 ratio batching, the mixed compound that forms adds the addition of C aF that accounts for mixture quality 1 ~ 7% in compound in ball mill
2, Na
2CO
3Or Fe
2O
3, add the binding agent that accounts for mixture quality 0.1 ~ 0.2% behind the mixing, under the pressure of 30 ~ 60MPa, be molded into cylindric sample;
(2) cylindric sample being imbedded in the crucible that fills anchracite duff, is 30 ~ 120min in 1100 ~ 1400 ℃ of recovery times, obtains reduced iron powder;
(3) with reduced iron powder shrend cooling or naturally cool to room temperature, with pulverizer reduzate is milled down to 100～300 orders, obtain levigate reduced iron powder;
(4) with the magnetic separation under the magnetic separation strength of 120 ~ 240kA/m of levigate reduced iron powder, scum separates, and the rate of being recycled is 94 ~ 97% iron powder.
2. a kind of vanadium titano-magnetite solid phase according to claim 1 is strengthened the method that reduction-magnetic separation separates, and it is characterized in that described binding agent is polyvinyl alcohol, and its molecular formula is [C
2H
4O]
n
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Cited By (4)
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| CN103757199A (en) * | 2013-12-05 | 2014-04-30 | 中国科学院过程工程研究所 | Method for preparing vanadium-chromium-titanium slag by utilizing high-chromium vanadium titanium magnet concentrate |
| CN105905902A (en) * | 2016-06-28 | 2016-08-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of titanium carbide raw material |
| CN108212509A (en) * | 2018-01-16 | 2018-06-29 | 东北大学 | Titanium vanadium mineral separation beneficiation method in a kind of hematite-limonite of titaniferous vanadium |
| WO2020151034A1 (en) * | 2019-01-24 | 2020-07-30 | 东北大学 | Method for separation and enrichment of valuable components from titanium-containing iron mineral |
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| CN105905902A (en) * | 2016-06-28 | 2016-08-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of titanium carbide raw material |
| CN108212509A (en) * | 2018-01-16 | 2018-06-29 | 东北大学 | Titanium vanadium mineral separation beneficiation method in a kind of hematite-limonite of titaniferous vanadium |
| WO2020151034A1 (en) * | 2019-01-24 | 2020-07-30 | 东北大学 | Method for separation and enrichment of valuable components from titanium-containing iron mineral |
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Application publication date: 20130403 |