CN102605182B - External method for production of 70# ferrotitanium with high titanium - Google Patents
External method for production of 70# ferrotitanium with high titanium Download PDFInfo
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- CN102605182B CN102605182B CN201110442716.3A CN201110442716A CN102605182B CN 102605182 B CN102605182 B CN 102605182B CN 201110442716 A CN201110442716 A CN 201110442716A CN 102605182 B CN102605182 B CN 102605182B
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Abstract
The invention discloses a method for producing 70# ferrotitanium with high titanium by a perrin process. The method comprises the following steps that: rutile, titaniferous iron concentrate, reducing agents, sodium chlorate and lime are uniformly mixed according to a certain proportion, the mixture is placed into a purpose-made sealed high-temperature-resistant and high-pressure-resistant reaction furnace, a proper number of magnesium chips are paved on the top of the mixture, the magnesium chips are ignited by adopting electric ignition outside the furnace for starting smelting reaction, and the sufficient proceeding of the reaction is promoted through the reaction furnace swinging in the smelting reaction process. After the cooling and the pressure relief, the furnace is opened, reactants are taken out, slag and alloy separation is carried out, refining is carried out, and the 70# ferrotitanium with high titanium is obtained. The production method of the 70# ferrotitanium with high titanium disclosed by the invention has the advantages that the process is simple, the equipment investment is low, the production cost is low, the product quality standard is high, the oxygen content is lower than 2 percent, the method conforms to the steel making process requirements, and higher economic benefits and social benefits are realized.
Description
Technical field
The present invention relates to a kind of smelting process of metal, especially a kind of production method that adopts the high ferrotianium of 70# of high pressure resistant high temperature resistant Reaktionsofen.
Background technology
As everyone knows, the high ferrotitanium alloy of titaniferous 65% ~ 75%, owing to having suitable proportion and lower fusing point, is the important source material that steel-making industry is used for smelting all kinds of special steels and steel alloy always.Therefore the production of high ferrotianium is also the hot subject of the ferroalloy industry research always.
The method of at present, producing high ferrotianium mainly contains two kinds: remelting process and perrin process (being metallothermics).Remelting process be the titanium material that gives up be raw material, in the electric furnace under open type or vacuum state, add iron remelting, after slagging-off, be cast into high ferrotianium ingot.The advantage of the method is that Composition Control is accurate, and technique is simple, and titanium recovery rate is high, and product oxygen level is low.For example: Chinese Patent Application No.: 96117080.8, this Invention Announce a kind of open type electric furnace melting down method of producing high ferrotianium.The shortcoming of remelting process is that a large amount of purchases of useless titanium material are had any problem, and the production cost of useless titanium is very large with the fluctuation of pure titanium price, and cost is too high to adopt pure titanium sponge, is difficult to meet the need of market.It is main raw material that perrin process adopts rutile, and aluminium powder, as main reductive agent, adds sodium chlorate (or Potcrate) as heat-generating agent, adds lime and/or fluorite as production high ferrotitanium alloys such as slag formers.It is wide that the method has raw material sources, low price, and production cost is little with pure titanium price volalility, can produce in enormous quantities.Although the high ferrotianium titanium content that traditional perrin process is produced has reached more than 70%, oxygen level is very high, and generally in 8 ~ 12% left and right, this high ferrotianium is tested through steelworks, cannot from molten steel, receive to obtain titanium elements.Domesticly to reducing high ferrotianium oxygen level, be also studied, for example: China Patent No. 201010514572.3 has been announced a kind of technique that adopts calcium-magnesium alloy reductive agent to carry out two step strengthening reduction on the basis of traditional perrin process, has obtained oxygen level at the high ferrotianium below 1%.But the method need to be carried out two step smeltings, and high-temperature fusant is poured the careful safety features of manipulation require of the crucible that fills calcium-magnesium alloy, technique relative complex into.
Summary of the invention
For the deficiency in the high ferrotianium preparation technology of current traditional perrin process, the invention provides a kind of High Temperature High Pressure and rock the method that high ferrotianium is prepared in metallothermic reduction under condition, solve the outer legal system of current traditional burner and for high ferrotianium, had the problem of too high oxygen level.
Technical scheme of the present invention is achieved in that
Perrin process is produced a method for the high ferrotianium of 70#, comprises starting material preparatory process, smelting procedure and separated finishing procedure.
(1) described starting material preparatory process: select required starting material to carry out technological preparation, comprise the oven dry of rutile, concentrated ilmenite, reductive agent, sodium chlorate, slag former, bake out temperature is 120 ℃ ~ 250 ℃, the furnace charge of oven dry evenly mixes in proportion;
(2) described smelting procedure: mixed furnace charge pack into one can the high-temperature-resistant high-pressure-resistant Reaktionsofen of control pressure in, at compound top, spread appropriate magnesium powder, sealing bell, then airtight Reaktionsofen is fixed on the rocking equipment that can produce vertical plane, the mode of the electricity consumption sparking magnesium powder that ignites outside stove, start and smelt reaction, in reaction process, start rocking equipment, and control furnace pressure between 1MPa ~ 20MPa by the purging valve on Reaktionsofen, after reaction in furnace, stop shaking also exhaust and bleed off pressure to normal pressure, and be cooled to room temperature;
(3) described separated finishing procedure: open Reaktionsofen and take out the slag gold bullion that described smelting procedure produces, carry out slag gold broken apart, separating obtained metal block carries out broken finishing can obtain the high ferrotianium of 70#.
Further preferably: the size range of described rutile and concentrated ilmenite is 80 order to 200 orders, and the size range of slag former is 20 order to 40 orders.
Further preferably: described reductive agent is one or more the combination in aluminium powder, aluminium calcium powder and magnesium powder, and the granularity of reductive agent powder is greater than 20 orders.
Further preferably: the mixing of described rutile, concentrated ilmenite, reductive agent, sodium chlorate, slag former is respectively in mass ratio: 70 ~ 85:10 ~ 25:40 ~ 60:10 ~ 20:3 ~ 6.
Further preferably: described slag former is one or both the combination in lime and fluorite.
The method that a kind of perrin process of the present invention is produced the high ferrotianium of 70#: the closed environment of the controllable high-voltage confined reaction stove with rocking equipment of employing significantly reduces the heat loss of reduction reaction, can reduce the amount of allocating into of heat-generating agent sodium chlorate and reductive agent, saves cost; Airtight environment is still enclosed in system the material splashing in reaction process, and high ferrotianium recovery rate is improved; Rocking that rocking equipment produces carried out sufficient reacting, and slag gold is fully separated, and high ferrotianium recovery rate improves, and oxygen level declines; Being used in combination of aluminium powder, aluminium calcium powder and magnesium powder reduces aluminium content in reaction product, and oxygen level reduces; Compare with traditional perrin process, reaction process does not have dust to produce, and has saved dust removal installation; Because the high temperature hold-time in when reaction is long, sedimentation is abundant, and the golden separator well of slag, has created good condition for next step operation, has reduced cost; In order to prevent the pressure rise overpressure scope of design in enclosed high pressure Reaktionsofen, the automatic pressure relief valve on Reaktionsofen is adjusted internal pressure by venting, plays the effect of safety valve.
The invention has the beneficial effects as follows: the chemical composition of the high ferrotitanium alloy of preparing by the inventive method is: 65%≤Ti
75%, O
2%, Al
4%, Si
1%, C
0.5%, P≤0.03%, S≤0.03%, surplus is iron.Production method technique of the present invention is simple, and facility investment is few, and production cost is low, and target level of product quality is high, and oxygen level, lower than 2%, meets process for making requirement, has higher economic benefit and social benefit.
Embodiment
Below in conjunction with the preferred embodiment of the present invention, be described in further details:
A kind of perrin process is produced the method for the high ferrotianium of 70#, comprise described starting material preparation: select required starting material to carry out technological preparation, comprise the oven dry of rutile, concentrated ilmenite, reductive agent, sodium chlorate, slag former, bake out temperature is 120 ℃ ~ 250 ℃, and the furnace charge of oven dry evenly mixes in proportion;
Smelting procedure: mixed furnace charge pack into one can the high-temperature-resistant high-pressure-resistant Reaktionsofen of control pressure in, at compound top, spread appropriate magnesium powder, sealing bell, then airtight Reaktionsofen is fixed on the rocking equipment that can produce vertical plane, the mode of the electricity consumption sparking magnesium powder that ignites outside stove, start and smelt reaction, in reaction process, start rocking equipment, and control furnace pressure between 1MPa ~ 20MPa by purging valve, after reaction in furnace, stop shaking also exhaust and bleed off pressure to normal pressure, and be cooled to room temperature;
Separated finishing procedure: open Reaktionsofen and take out the slag gold bullion that described smelting procedure produces, carry out slag gold broken apart, separating obtained metal block carries out broken finishing can obtain the high ferrotianium of 70#.
Wherein the mixing of rutile, concentrated ilmenite, reductive agent, sodium chlorate, slag former is respectively in mass ratio: 70 ~ 85:10 ~ 25:40 ~ 60:10 ~ 20:3 ~ 6.
Wherein reductive agent is selected from one or more the combination in aluminium powder, aluminium calcium powder and magnesium powder, and the granularity of reductive agent powder is less than 1mm.Slag former is one or both the combination in lime and fluorite.
Wherein the size range of rutile and concentrated ilmenite is 80 order to 200 orders, and the size range of slag former is 20 order to 40 orders, and the granularity of reductive agent powder is greater than 20 orders.
The chemical composition of the high ferrotitanium alloy of preparing by the inventive method is: 65%≤Ti
75%, O
2%, Al
4%, Si
1%, C
0.5%, P≤0.03%, S≤0.03%, surplus is iron.
Embodiment 1
By rutile 72.3kg, ilmenite concentrate 22.7kg, aluminium powder 36kg, aluminium calcium powder 12kg, sodium chlorate 15.5kg, calcium oxide 1.8kg, Calcium Fluoride (Fluorspan) 3.5kg is dried respectively at 200 ℃, then adds together mixer with the speed batch mixing of 20 revs/min 30 minutes.Mixed furnace charge adds Reaktionsofen while hot, spreads a small amount of magnesium powder at top, and banking.Then Reaktionsofen is fixed on rocking equipment.By furnace charge in long-range electric ignition device point burner, start melting.Light a fire and after 3 minutes, start rocking equipment and start to wave.Wobble frequency is 20 beats/min, stops after moving 30 minutes.In fusion process, by venting, control Reaktionsofen internal pressure not higher than 5MPa.Light a fire after 1 hour, bleed off pressure to normal pressure.After cooling 24 hours, take out furnace charge.Carry out slag gold separated.The ferro-titanium composition obtaining by weight, Ti:71.2%, O:1.2%, Al:3%, Si:0.8%, C:0.2%, P:0.02%, S:0.01%.
Embodiment 2
By rutile 70kg, ilmenite concentrate 30kg, aluminium powder 33kg, aluminium calcium powder 15kg, sodium chlorate 14kg, calcium oxide 2kg, Calcium Fluoride (Fluorspan) 3kg is dried respectively at 200 ℃, then adds together mixer with the speed batch mixing of 20 revs/min 30 minutes.Mixed furnace charge adds Reaktionsofen while hot, spreads a small amount of magnesium powder at top, and banking.Then Reaktionsofen is fixed on rocking equipment.By furnace charge in long-range electric ignition device point burner, start melting.Light a fire and after 3 minutes, start rocking equipment and start to wave.Wobble frequency is 20 beats/min, stops after moving 30 minutes.In fusion process, by venting, control Reaktionsofen internal pressure not higher than 5MPa.Light a fire after 1 hour, bleed off pressure to normal pressure.After cooling 24 hours, take out furnace charge.Carry out slag gold separated.The ferro-titanium composition obtaining by weight, Ti:68.5%, O:0.8 %, Al:2.3%, Si:0.7%, C:0.15%, P:0.03%, S:0.02%.
The closed environment of the controllable high-voltage confined reaction stove with rocking equipment that embodiment 1,2 adopts significantly reduces the heat loss of reduction reaction, can reduce the amount of allocating into of heat-generating agent sodium chlorate and reductive agent, saves cost; Airtight environment is still enclosed in system the material splashing in reaction process, and high ferrotianium recovery rate is improved; Rocking that rocking equipment produces carried out sufficient reacting, and slag gold is fully separated, and high ferrotianium recovery rate improves, and oxygen level declines; Being used in combination of aluminium powder, aluminium calcium powder and magnesium powder reduces aluminium content in reaction product, and oxygen level reduces; Compare with traditional perrin process, reaction process does not have dust to produce, and has saved dust removal installation; Because the high temperature hold-time in when reaction is long, sedimentation is abundant, and the golden separator well of slag, has created good condition for next step operation, has reduced cost; In order to prevent the pressure rise overpressure scope of design in enclosed high pressure Reaktionsofen, the automatic pressure relief valve on Reaktionsofen is adjusted internal pressure by venting, plays the effect of safety valve.
Beneficial effect of the present invention is: production method technique is simple, and facility investment is few, and production cost is low, and target level of product quality is high, and oxygen level, lower than 2%, meets process for making requirement, has higher economic benefit and social benefit.The chemical composition of the high ferrotitanium alloy of preparing by the inventive method is: 65%≤Ti
75%, O
2%, Al
4%, Si
1%, C
0.5%, P≤0.03%, S≤0.03%, surplus is iron.In the high ferrotianium that the present invention produces, titanium content is high, and product oxygen level is low, meets process for making requirement, is conducive to receive to obtain titanium elements, thereby increases the rate of recovery of titanium, increases economic efficiency.
Claims (5)
1. perrin process is produced a method for the high ferrotianium of 70#, comprises starting material preparatory process, smelting procedure and separated finishing procedure, it is characterized in that:
(1) described starting material preparatory process: select required starting material to carry out technological preparation, comprise the oven dry of rutile, concentrated ilmenite, reductive agent, sodium chlorate, slag former, bake out temperature is 120 ℃ ~ 250 ℃, the furnace charge of oven dry evenly mixes in proportion;
(2) described smelting procedure: mixed furnace charge pack into one can the high-temperature-resistant high-pressure-resistant Reaktionsofen of control pressure in, at compound top, spread appropriate magnesium powder, sealing bell, then airtight Reaktionsofen is fixed on the rocking equipment that can produce vertical plane, the mode of the electricity consumption sparking magnesium powder that ignites outside stove, start and smelt reaction, in reaction process, start rocking equipment, and control furnace pressure between 1MPa ~ 20MPa by the purging valve on Reaktionsofen, after reaction in furnace, stop shaking also exhaust and bleed off pressure to normal pressure, and be cooled to room temperature;
(3) described separated finishing procedure: open Reaktionsofen and take out the slag gold bullion that described smelting procedure produces, carry out slag gold broken apart, separating obtained metal block carries out broken finishing can obtain the high ferrotianium of 70#.
2. the method for producing the high ferrotianium of 70# according to the said perrin process of claim 1, is characterized in that: the size range of described rutile and concentrated ilmenite is 80 order to 200 orders, the size range of slag former is 20 order to 40 orders.
3. according to the said perrin process of claim 1, produce the method for the high ferrotianium of 70#, it is characterized in that: described reductive agent is one or more the combination in aluminium powder, aluminium calcium powder and magnesium powder, and the granularity of reductive agent powder is greater than 20 orders.
4. the method for producing the high ferrotianium of 70# according to the said perrin process of claim 1, is characterized in that: the mixing of described rutile, concentrated ilmenite, reductive agent, sodium chlorate, slag former is respectively in mass ratio: 70 ~ 85:10 ~ 25:40 ~ 60:10 ~ 20:3 ~ 6.
5. according to the said perrin process of claim 1, produce the method for the high ferrotianium of 70#, it is characterized in that: described slag former is one or both the combination in lime and fluorite.
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| CN107058802B (en) * | 2017-04-06 | 2018-06-19 | 江苏江南铁合金有限公司 | A kind of preparation method of 70 ferrotianium of low aluminum nitrogen |
| CN114959325A (en) * | 2022-06-08 | 2022-08-30 | 攀钢集团钒钛资源股份有限公司 | Preparation method of vanadium-aluminum alloy |
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