CN100436601C - Method for separating and extracting iron, vanadium and titanium from vanadium-titanium magnetite - Google Patents
Method for separating and extracting iron, vanadium and titanium from vanadium-titanium magnetite Download PDFInfo
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- CN100436601C CN100436601C CNB2006100204362A CN200610020436A CN100436601C CN 100436601 C CN100436601 C CN 100436601C CN B2006100204362 A CNB2006100204362 A CN B2006100204362A CN 200610020436 A CN200610020436 A CN 200610020436A CN 100436601 C CN100436601 C CN 100436601C
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Abstract
The present invention provides a method for separating and extracting iron, vanadium and titanium from vanadium titano-magnetite, which comprises the following steps: 1) after being pelletized or briquetted, vanadium titano-magnetite powder, a reducer and a binding agent are dried; 2) the vanadium titano-magnetite powder, the reducer and the binding agent are loaded in a reduction furnace, are heated to 1400 to 1500DEG C, and are directly reduced to prepare metallized pellets. The ratio of the partial pressure of carbon monoxide to the partial pressure of carbon dioxide is at most 2.0; 3) the metallized pellets are loaded in the furnace and are processed by melting and slag iron separation at the temperature of 1560 to 1700DEG C to obtain vanadium-bearing hot metal and titaniferous steel slag; 4) vanadium is extracted from the vanadium-bearing hot metal by a fire method to obtain hot metal and vanadium slag; 5) the vanadium slag is processed to obtain V2O5; 6) the titaniferous steel slag is processed by a sulfuric acid method or a chlorination method to prepare titanium white. The present invention has high reduction reaction speed, the reduction only takes 5 to 50 minutes, and the recovery rates of the iron, the vanadium and the titanium can achieve more than 90%.
Description
Technical field
The present invention relates to a kind of from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium.
Background technology
Vanadium titano-magnetite is a kind of compound mineral intergrowth, mainly is distributed in the areas such as Flos Bombacis Malabarici, Xichang, Hebei and Anhui of China, wherein especially with Panxi Diqu reserves maximum, and about 10,000,000,000 tons.Contain multiple elements such as iron, vanadium and titanium in the vanadium titano-magnetite, have comprehensive utilization value.
Method to direct reduction of V-Ti magnetite separating and extracting Fe, vanadium and titanium mainly contains three kinds of methods: first kind is: sodium pelletizing oxidizing roasting → water law vanadium extraction → rotary kiln for directly reducing → electric furnace is molten to be divided; Second kind is: titanium is carried in the molten branch → water law vanadium extraction of rotary kiln for directly reducing → electric furnace; The third is: the cooled agglomerated pellet direct-reduction process.The shortcoming of first method is that Production Flow Chart is long, the sodium agent consume high, the ferrovanadium titanium recovery rate is low (wherein iron recovery is about 85%, vanadium recovery about 60%, titanium recovery rate be about 75%); The shortcoming of second method be the vanadium extraction effect instability of carrying titanium, vanadium titanium flow to be difficult to control and the acid solution consumption big, and vanadium titanium recovery rate lower (wherein vanadium recovery is about 68%, titanium recovery rate is about 80%); Though the third method has advantages such as technical process is short, sodium agent consumption is low, has the shortcoming that the recovery time is long, production efficiency is low.
Application number is 200510020117.7, denomination of invention is the method for separation and Extraction metallic element " a kind of from vanadium titano-magnetite ", what adopt is that the titanium technical process is proposed in the molten branch of direct reduction → electric furnace → molten branch slag vanadium extraction, directly the reduction operation only reclaims iron, shortcomings such as being recovered in the slag of vanadium and titanium carried out, and the difficulty that possesses skills is big, the vanadium titanium products is of low quality.
Summary of the invention
Technical problem to be solved by this invention provides the high method of separating and extracting Fe, vanadium and titanium from vanadium titano-magnetite of short, ferrovanadium titanium comprehensive recovery height of a kind of technical process and recovery time and production efficiency.
The technical scheme that technical solution problem of the present invention adopts is: the method for separating and extracting Fe, vanadium and titanium from vanadium titano-magnetite, and this method may further comprise the steps: 1) v-ti magnetite breeze, reducing agent and binding agent are made ball or briquetting post-drying; 2) pack into and be heated to 1400～1500 ℃ of direct-reductions in the reduction furnace and make metallized pellet, the ratio of carbon monoxide pressure of tension and partial pressure of carbon dioxide is not more than 2.0 in the gas phase; 3) metallized pellet is packed under 1560～1700 ℃, melt with slag iron in the stove and separate, obtain vanadium-bearing hot metal and titaniferous slag; 4) vanadium-bearing hot metal is carried out the pyrogenic process vanadium extraction, obtain molten iron and vanadium slag; 5) vanadium slag is processed, obtained V
2O
56) the titaniferous slag is produced titanium white with sulfuric acid process or chloridising processing.
Further, step 1) make pelletizing or material piece moisture be not more than 1.5% after the described oven dry.
Further, the described reductive agent of step 1) is coal dust, electrode block or broken coke button.
Further, the consumption of the described reductive agent of step 1) is 15%～25% of a v-ti magnetite breeze.
Further, the described binding agent of step 1) is wilkinite, water glass or carboxymethyl cellulose.
Further, the consumption of the described binding agent of step 1) is 0.3%～3% of a v-ti magnetite breeze.
Further, the described bake out temperature of step 1) is 200～350 ℃.
Further, step 2) described reductive time is 5～50 minutes.
Further, described vanadium slag is handled of step 5) is to adopt the sodium method to handle.
The invention has the beneficial effects as follows:
1) by control in the Direct Reduction reduction temperature and gas phase in the ratio of carbon monoxide pressure of tension and partial pressure of carbon dioxide, the oxide of realization vanadium is reduced in Direct Reduction and enters iron phase, be after direct-reduction finishes, iron and vanadium are present in the metallized pellet with the simple substance state, titanium is present in the metallized pellet with the oxide state, for the separation of slag iron and vanadium, the titanium comprehensive reutilization of rear step operation have been created advantage.
2) because conventional shaft kiln directly reduced temperature is about 1000 ℃, the rotary kiln for directly reducing temperature is about 1050 ℃, fluid bed direct-reduction temperature is about 900 ℃, rotary hearth furnace direct-reduction temperature is about 1200 ℃; and reduction temperature of the present invention is up to more than 1400 ℃; therefore direct reduction reactor speed is fast; recovery time only needs 5～50 minutes; and the recovery time of conventional blast furnace is about 7 hours, rotary kiln is about 5 hours, shaft furnace is about 10 hours, so the present invention realizes efficient large-scale production easily.
3) degree of metalization of iron of the present invention can reach more than 92%, the rate of recovery of iron, vanadium and titanium all can reach more than 90%, and present various separating and extracting method to vanadium titano-magnetite, the rate of recovery of iron is the highest can only to reach 90%, vanadium, titanium recovery rate all are no more than 85%, therefore, ferrovanadium titanium comprehensive reutilization rate height of the present invention.
Embodiment
Direct reduction of the present invention is meant in reduction furnace (shaft furnace, rotary kiln, tunnel furnace or rotary hearth furnace), and the mode by fuel (as heavy oil, Sweet natural gas, coke-oven gas, coal dust or gas maked coal) heating, microwave heating or plasma heating is heated to 1400～1500 ℃ with raw material and directly reduces.Recovery time is 5～50 minutes, and directly raw material keeps the semi-melting state in the reduction process, and promptly material temperature is between the beginning temperature of fusion and soft heat drippage temperature of vanadium titano-magnetite.Ratio (the PCO/PCO of carbon monoxide pressure of tension in the gas phase (volume content of carbon monoxide in the reduction process escaping gas) and partial pressure of carbon dioxide
2) be not more than 2.0, the oxide compound of the oxide compound of iron and vanadium is reduced to the simple substance state in the raw material, and titanyl compound does not reduce substantially, and the degree of metalization that obtains iron is 85% or more, the reduction degree of the vanadium ratio of total content of vanadium (the elemental vanadium content with) is 75% or more, the reduction degree of titanium is the metallized pellet below 10% for (simple substance titanium content and always the ratio of titanium content) below 10%, fixed carbon content.Metallized pellet packed into to melt with slag iron in electric furnace or the mineral hot furnace separate (the molten branch), molten branch temperature is 1560～1700 ℃, obtain vanadium-bearing hot metal and titaniferous slag, except the metallized pellet of packing into, need not add any reducing agent and slag making materials in the molten branch process.The pyrogenic process vanadium extraction is with vanadium-bearing hot metal pack into converter or hot metal ladle, is blown into oxygen the vanadium oxidation in the molten iron is entered the slag phase, and iron, vanadium are separated, and obtains molten iron and vanadium slag.
Embodiment 1:
(main component is: TFe content is 55.90%, FeO content is 23.28%, TiO with the v-ti magnetite breeze
2Content is 11.84%, V
2O
5Content is 0.73%), coal dust (main component is: content of ashes is 11.25%, volatile content is 8.62%, carbon content is 80.19%, pulverized coal consumption be breeze 22%), cause the pelletizing of 30mm behind bentonite (consumption be breeze the 3%) mixing.Under 200 ℃, dry to the pelletizing moisture be 1%.Send into 1400 ℃ reduction furnace reduction 50 minutes, keep PCO/PCO in the stove
2Be 1.0, the degree of metalization of iron reaches 94%, and the reduction degree of vanadium reaches 92%.Metallized pellet packed into, and electric furnace is molten to be divided, and molten branchs temperature is 1600 ℃, acquisition vanadium-bearing hot metal and titaniferous slag.The vanadium-bearing hot metal main component is: C content is 0.02%, V content is 0.67%, Ti content is 0.05%, and titaniferous slag main component is: FeO content is 12.58%, TiO
2Content is 43.65%, V
2O
5Content is 0.18%.To the vanadium extraction of vanadium-bearing hot metal pyrogenic process, obtain molten iron and vanadium slag, wherein the V in the vanadium slag
2O
5Content is 17%, adopts the sodium method to process to vanadium slag, can obtain highly purified V
2O
5Adopt sulfuric acid process to process to the titaniferous slag, acquisition purity is the titanium white more than 99.2%.To melting stage by stage, the rate of recovery of iron, vanadium, titanium is respectively 94%, 92%, 97% from the v-ti magnetite breeze.
Embodiment 2:
(main component is: TFe content is 54.40%, FeO content is 33.19%, TiO with the v-ti magnetite breeze
2Content is 15.92%, V
2O
5Content is 0.55%), coal dust (main component is: content of ashes is 15.72%, fugitive constituent 12.44%, fixed carbon content are 71.84%, pulverized coal consumption be breeze 25%), cause the pelletizing of 3mm behind carboxymethyl cellulose (consumption be breeze the 0.3%) mixing.Under 350 ℃, dry to the pelletizing moisture be 0.5%.Send into 1500 ℃ reduction furnace reduction 5 minutes, keep PCO/PCO in the stove
2Be 0.3, the degree of metalization of iron reaches 97%, and the reduction degree of vanadium reaches 94%.Metallized pellet packed into, and electric furnace is molten to be divided, and molten 1560 ℃ of the temperature of dividing obtain vanadium-bearing hot metal and titaniferous slag.The vanadium-bearing hot metal main component is: C content is 0.018%, V content is 0.56%, Ti content is 0.041%, and titaniferous slag main component is: FeO content is 8.18%, TiO
2Content is 56.38%, V
2O
5Content is 0.14%.To the vanadium extraction of vanadium-bearing hot metal pyrogenic process, obtain molten iron and vanadium slag, wherein the V in the vanadium slag
2O
5Content is 15%, and vanadium slag is processed, and obtains highly purified V
2O
5Adopt sulfuric acid process to process to the titaniferous slag, acquisition purity is the titanium white more than 99.2%.To melting stage by stage, the rate of recovery of iron, vanadium, titanium is respectively 96%, 93%, 96% from the v-ti magnetite breeze.
Embodiment 3:
(main component is: TFe content is 52.50%, FeO content is 30.72%, TiO with the v-ti magnetite breeze
2Content is 13.14%, V
2O
5Content is 0.58%), electrode block (main component is: fixed carbon content 91.88%, consumption be breeze 15%), cause the pelletizing of 15mm behind carboxymethyl cellulose (consumption be breeze the 0.3%) mixing.Under 280 ℃, dry to the pelletizing moisture be 0.7%.Send into 1450 ℃ reduction furnace reduction 30 minutes, keep PCO/PCO in the stove
2Be 2.0, the degree of metalization of iron reaches 95%, and the reduction degree of vanadium reaches 92%.Metallized pellet packed into, and mineral hot furnace is molten divides, and molten branchs temperature is 1700 ℃, acquisition vanadium-bearing hot metal and titaniferous slag.The main component of vanadium-bearing hot metal is: C content is 0.033%, V content is 0.48%, Ti content is 0.035%, and titaniferous slag main component is: FeO content is 12.15%, TiO
2Content is 46.53%, V
2O
5Content is 0.25%.To the vanadium extraction of vanadium-bearing hot metal pyrogenic process, obtain molten iron and vanadium slag, wherein the V in the vanadium slag
2O
5Content is 14.5%, adopts the sodium method to process to vanadium slag, obtains highly purified V
2O
5Adopt sulfuric acid process to process to the titaniferous slag, acquisition purity is the titanium white more than 99.2%.To melting stage by stage, the rate of recovery of iron, vanadium, titanium is respectively 93%, 91%, 97% from the v-ti magnetite breeze.
Embodiment 4:
(main component is: TFe content is 53.88%, FeO content is 28.56%, TiO with the v-ti magnetite breeze
2Content is 13.52%, V
2O
5Content is 0.57%), broken coke button (main component is: fixed carbon content 85.04%, fugitive constituent 2.06%, consumption be breeze 17%), cause the pelletizing of 25mm behind waterglass (consumption be breeze the 3%) mixing.Under 250 ℃, dry to the pelletizing moisture be 1.2%.Send in 1480 ℃ the reduction furnace reductase 12 5 minutes, and kept PCO/PCO in the stove
2Be 1.2, the degree of metalization of iron reaches 94%, and the reduction degree of vanadium reaches 92%.Metallized pellet packed into, and mineral hot furnace is molten divides, and molten branchs temperature is 1620 ℃, acquisition vanadium-bearing hot metal and titaniferous slag.The vanadium-bearing hot metal main component is: C content is 0.027%, V content is 0.446%, Ti content is 0.021%, and titaniferous slag main component is: FeO content is 14.68%, TiO
2Content is 48.28%, V
2O
5Content is 0.24%.To the vanadium extraction of vanadium-bearing hot metal pyrogenic process, obtain molten iron and vanadium slag, wherein the V in the vanadium slag
2O
5Content is 16.2%, and vanadium slag is processed, and obtains highly purified V
2O
5Adopt chloridising to process to the titaniferous slag, acquisition purity is the titanium white more than 99.2%.To melting stage by stage, the rate of recovery of iron, vanadium, titanium is respectively 91%, 90%, 97% from the v-ti magnetite breeze.
Claims (7)
1, the method for separating and extracting Fe, vanadium and titanium from vanadium titano-magnetite, this method may further comprise the steps: 1) v-ti magnetite breeze, reducing agent and binding agent are made ball or briquetting post-drying, the consumption of described reducing agent is 15%～25% of v-ti magnetite breeze, and the consumption of described binding agent is 0.3%～3% of v-ti magnetite breeze; 2) pack into and be heated to 1400～1500 ℃ of direct-reductions in the reduction furnace and make metallized pellet, the ratio of carbon monoxide pressure of tension and partial pressure of carbon dioxide is not more than 2.0 in the gas phase, and the time of described reduction is 5～50 minutes; 3) metallized pellet is packed under 1560～1700 ℃, melt with slag iron in the stove and separate, obtain vanadium-bearing hot metal and titaniferous slag; 4) vanadium-bearing hot metal is carried out the pyrogenic process vanadium extraction, obtain molten iron and vanadium slag; 5) vanadium slag is processed, obtained V
2O
56) the titaniferous slag is produced titanium white with sulfuric acid process or chloridising processing.
2, according to claim 1 from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium, it is characterized in that: make pelletizing or material piece moisture be not more than 1.5% after the described oven dry of step 1).
3, according to claim 1 from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium, it is characterized in that: the described reductive agent of step 1) is coal dust, electrode block or broken coke button.
4, according to claim 1 from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium, it is characterized in that: the described binding agent of step 1) is wilkinite, water glass or carboxymethyl cellulose.
5, according to claim 1 from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium, it is characterized in that: the described bake out temperature of step 1) is 200～350 ℃.
6, according to claim 1 from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium, it is characterized in that: step 4) is: with vanadium-bearing hot metal pack into converter or hot metal ladle, be blown into oxygen the vanadium oxidation in the molten iron is entered the slag phase, iron, vanadium are separated, obtain molten iron and vanadium slag.
7, according to claim 1 from vanadium titano-magnetite the method for separating and extracting Fe, vanadium and titanium, it is characterized in that: described vanadium slag is handled of step 5) is to adopt the sodium method to handle.
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Cited By (1)
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| CN113481342B (en) * | 2021-07-01 | 2022-10-11 | 钢研晟华科技股份有限公司 | Method for preparing iron and separating vanadium and titanium from vanadium titano-magnetite through calcium-free low-temperature reduction |
| CN113981214A (en) * | 2021-11-16 | 2022-01-28 | 新疆葱岭钒钛有限公司 | Smelting method for preparing pellet vanadium titano-magnetite by internal carbon distribution |
| CN115820966B (en) * | 2022-11-15 | 2024-02-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Reduction and non-blast furnace smelting method for alkaline vanadium-titanium pellet heating and pressing carbon-containing vanadium-titanium pellet |
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| CN1814813A (en) | 2006-08-09 |
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