CN107326256B - The method for preparing ferro-molybdenum with wash heat refining based on the reduction of aluminothermy self- propagating gradient - Google Patents
The method for preparing ferro-molybdenum with wash heat refining based on the reduction of aluminothermy self- propagating gradient Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C35/00—Master alloys for iron or steel
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- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
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Abstract
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, belongs to technical field of iron alloy.This method include by pretreatment of raw material, and in mass ratio, MoO3: Fe2O3Powder: aluminium powder: CaO=1.0: (0.32~0.95): (0.48~0.69): (0.82~1.62) weighing material；Then aluminothermy self-propagating reaction being carried out by the way of gradient charging and obtaining high-temperature fusant, carry out gradient reduction melting, charging keeps the temperature molten point, CaO-CaF is added into high-temperature fusant after finishing2Base refining slag carries out wash heat refining, obtains ferro-molybdenum after finally removing the gred.This method realizes the control of reaction process and temperature and the thorough reduction of metal oxide, and it is smaller with aluminium coefficient gradients, aluminium residual is lower in alloy melt, and realizes the thorough progress of slag gold interfacial chemical reaction and the separation of slag gold, realizes that aluminium oxide etc. is mingled with effective removing.
Description
Technical field
It is the invention belongs to technical field of iron alloy, in particular to a kind of to be refined based on the reduction of aluminothermy self- propagating gradient with wash heat
The method for preparing ferro-molybdenum.
Background technique
Molybdenum-iron is one of important ferroalloy of steel and iron industry, and molybdenum-iron is used for steel and iron industry alloy addition.Molybdenum is added in steel grade
The intensity and toughness (especially high-temperature behavior) that steel can be improved, improve the harden ability and hardenability of steel part.Currently, domestic and international molybdenum
The molybdenum content of iron all between 55%~75%, the molybdenum-iron product molybdenum content of domestic mainstream all 60% or so, these molybdenum-irons
Preparation is all prepared using aluminothermic process, that is, the perrin process often said, stove used by perrin process is one and is placed on sand base
Cylinder, interior block clay bricking makees reducing agent with siliceous 75% ferrosilicon and a small amount of aluminum shot, after once furnace tube is added in furnace charge, use
The preparation of top methods of printing, i.e., lighted a fire on charge level with initiator (nitre, aluminium skimmings or magnesium chips), and intense reaction occurs after igniting,
Then calmness, slagging, dismounting furnace tube, molybdenum-iron ingot is first cooling in sand nest, then send chilling room bath cooling, is finally crushed,
Finishing obtains product molybdenum-iron.It when carrying out aluminothermic process with this traditional formula and preparing molybdenum-iron, has the following disadvantages: 1) anti-
Answer temperature high, generally at 2000 DEG C or more, furnace charge is once added, and reaction process temperature is difficult to control；2) reaction system rises rapidly
Temperature drop temperature, slag gold effective separation time is insufficient, leads to that slag gold inferior separating effect, inclusion content is high in alloy.3) reaction is used
To nitre or fluorite can generate nitrogen oxides or fluoride during the preparation process, pollute.
Chinese patent (104762544 A of CN) describe it is a kind of use carbon dust as reducing agent, by mixture powder and reduction
Product is obtained after furnace cooling after roasting under the conditions of being not higher than 1600 DEG C of temperature after agent mixing, slag iron then is carried out to product
Separation, obtains ferro-molybdenum.This method deposits the disadvantages of carbon content is high in the alloy.
The present invention is based on prepare at present reaction process temperature during ferro-molybdenum be difficult to control, slag gold inferior separating effect,
The disadvantage of inclusion content height, high pollution etc. in alloy proposes to prepare molybdenum with wash heat refining based on the reduction of aluminothermy self- propagating gradient
The method of ferroalloy.
Summary of the invention
It is difficult to control, in slag gold inferior separating effect, alloy in view of reaction process temperature during preparing ferro-molybdenum at present
The disadvantage of inclusion content height, high pollution etc. proposes to prepare ferro-molybdenum with wash heat refining based on the reduction of aluminothermy self- propagating gradient
Method.I.e. first with MoO3、Fe2O3Deng for raw material, aluminothermy self-propagating reaction is carried out by the way of gradient charging and obtains high temperature
Melt carries out gradient reduction melting, i.e., will launch being gradually decrease to by being higher than stoichiometric ratio lower than chemistry with aluminum amount for material
Measure ratio, and using batch charging or continuous charging mode realize reaction process and temperature control and metal oxide it is thorough
Bottom reduction, and it is smaller with aluminium coefficient gradients, aluminium residual is lower in alloy melt；Charging keeps the temperature molten point after finishing, then to height
High alkalinity CaO-CaF is added in warm melt2Base refining slag adjusts the basicity and fusing point of slag, carries out wash heat refining, realizes Zha Jin circle
Face chemically reacts the thorough progress separated with slag gold；Ferro-molybdenum is obtained after finally removing the gred.
The present invention is based on the methods that the reduction of aluminothermy self- propagating gradient prepares ferro-molybdenum with wash heat refining, specifically include following
Step:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, obtains pretreated aluminothermy self-propagating reaction raw material；
The aluminothermy self-propagating reaction raw material includes MoO3、Fe2O3Powder, aluminium powder and CaO；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3: Fe2O3Powder: aluminium powder:
CaO=1.0: (0.32~0.95): (0.48~0.69): (0.82~1.62)；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Fe2O3≤
0.2mm；Aluminum powder particle size≤2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction is carried out using one of following two feed way:
Feed way one:
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into several pieces；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, with aluminum amount according to reactive chemistry metering ratio
1.10~1.30 times are gradually decrease to 0.9~0.7 times of stoichiometric ratio；It obtains that aluminium powder is added according to chemical equation
Gross mass is theoretical addition gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× (90~100) %；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 10~30% of total mixture material quality, and
The mixed material of reacting furnace is added in first, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
To first high-temperature fusant for being adequate to bring about subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Feed way two:
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.9~0.7 times of stoichiometric ratio by 1.10~1.30 times of stoichiometric ratio, wherein matches aluminum amount gradient
Change frequency meets relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, 0 < a≤0.05；
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×(90
~100) %；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700~1800 DEG C, soaking time
5~15min；
Step 4: wash heat refining
(1) the 85~95% of the alumina base slag total volume on upper layer are removed, it is molten to the alumina base of remaining volume
Slag and the alloy melt of lower layer carry out eccentric mechanical stirring, 50~150rpm of speed of agitator；Controlled at 1700~1800 DEG C；
(2) lasting to stir after melt mixed is uniform, and using high purity inert gas as carrier gas, to uniformly mixed melt
It is blown CaO-CaF2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self-propagating reaction raw material: CaO-CaF2Base
Refining slag=1.0: (0.02~0.10)；CaO-CaF2Base refining slag is one of following two:
The first: in mass ratio 10~25% CaF2, surplus CaO；
Second: in mass ratio 10~25% CaF2, 5~10% Na2O, surplus CaO；
(3) it is blown CaO-CaF2After base refining slag, kept the temperature at 1700~1800 DEG C and continue eccentric mechanical stirring 10~
30min obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, ferro-molybdenum is obtained.
The chemical component and its mass fraction that ferro-molybdenum prepared by the present invention contains are as follows: Mo is 55.0~75.0%, Al
≤ 2.0%, O≤1%, surplus Fe.
In the step 1, the pretreated mode are as follows:
By MoO3, Fe2O3Powder, CaO are roasted respectively, and 150~400 DEG C of maturing temperature, 12~48h of calcining time.
In the step 2, the several pieces are n parts, n >=4.
In the step 3, the equipment of the electromagnetic induction is intermediate frequency furnace, and the frequency of electromagnetic field is more than or equal to
1000Hz。
In the step 4, the eccentric mechanical stirring, eccentricity is 0.2~0.4；
In the step 4, the blowing is preferably blown in Medium frequency induction furnace bottom.
In the step 4, the high purity inert gas is high-purity argon gas, and purity is more than or equal to 99.95%.
A kind of method that ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient of the invention, with tradition
Aluminium method prepares ferro-molybdenum and compares, have the advantages that significant progress and:
1, aluminothermy self- propagating is carried out with aluminium coefficient material using higher than stoichiometric ratio first, obtains the height of higher temperature
Warm melt is conducive to the subsequent low reaction with aluminium coefficient material and causes；
2, high aluminium coefficient of matching ensure that reducing atmosphere strong in obtained melt, ensure that the thorough of metal oxide
Bottom reduction；
3, material is gradually decreased to less than stoichiometric ratio with aluminium coefficient by being greater than stoichiometric ratio, starts to be melted in this way
Excessive reducing agent in body in conjunction with iron, molybdenum is gradually released, with subsequent addition the low molybdenum in aluminium coefficient material,
The oxide of iron gradually reacts, and realizes residual aluminum in final products and is effectively reduced；
4, charging batch is more or continuous charging gradient is smaller, and smaller with the variation of aluminium coefficient gradients, gradient reduction effect is got over
Obviously, the yield of alloy is higher；Meanwhile control charging rate can control the temperature in reaction process；
5, in wash heat refining process, using the basicity and fusing point of the refining slag adjustment slag of addition, the viscosity of slag is reduced, is mentioned
The high mobility of slag, realizes the thorough progress of slag gold interfacial chemical reaction and the separation of slag gold, realizes that aluminium oxide etc. is mingled with effectively
Removing；Meanwhile melting and wash heat refining process are kept the temperature, system reaction heat is taken full advantage of, energy consumption is reduced.
6, wash heat refining is carried out using electromagnetic induction heating, it is molten for alumina base to form upper layer for additional bias mechanical stirring
Slag blanket, lower layer are golden melt layer, enhance slag gold separation process.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment, the purity of high-purity argon gas is greater than 99.95%；
In following embodiment, molten to divide process and wash heat refinery practice, the equipment of use is intermediate frequency furnace, Medium frequency induction
The frequency of electromagnetic field in furnace is not less than 1000Hz.
Embodiment 1
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.63: 0.59: 0.95；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 5 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.05,1.0,0.90,0.85 times；It obtains being added the gross mass of aluminium powder according to chemical equation to be added always to be theoretical
Quality mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 98%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 20% of total mixture material quality, and first
The mixed material that reacting furnace is added is criticized, magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain foot
To cause first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1800 DEG C, soaking time 15min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.2, speed of agitator 50rpm；Controlled at 1800 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.04；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 90%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 10min is kept the temperature and continued at 1800 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 59.2%, Al
1.80%, O0.8%, surplus Fe.
Embodiment 2
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.68: 0.61: 0.99；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 6 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.1,0.95,0.90,0.85,0.80 times；It obtains being added the gross mass of aluminium powder according to chemical equation to add to be theoretical
Enter gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 97%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 28.6% of total mixture material quality, and the
The mixed material of reacting furnace is added in a batch, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
It is adequate to bring about first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1750 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1750 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.06；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 20%, CaO 80%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1750 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 58.0%, Al
1.50%, O 0.7%, surplus Fe.
Embodiment 3
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.78: 0.62: 1.12；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 8 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.1,1.0,0.95,0.925,0.90,0.875,0.85 times；It obtains that the total of aluminium powder is added according to chemical equation
Quality is theoretical addition gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 99%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 22.2% of total mixture material quality, and the
The mixed material of reacting furnace is added in a batch, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
It is adequate to bring about first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 5min；
Step 4: wash heat refining
(1) the 95% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.3, speed of agitator 150rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 25%, CaO 75%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 30min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 58.7%, Al
1.20%, O 0.5%, surplus Fe.
Embodiment 4
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.8: 0.63: 1.18；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.75 times of stoichiometric ratio by 1.23 times of stoichiometric ratio, wherein full with aluminum amount change of gradient number
Sufficient relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.02；By calculating, m is 24 times, when the time interval of aluminium powder flow gradients variation is overall reaction
Between divided by m.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
98%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1750 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.3, speed of agitator 100rpm；Controlled at 1750 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.06；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 85%, Na2O is 5%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1750 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 58.0%, Al
1.40%, O 0.6%, surplus Fe.
Embodiment 5
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.84: 0.65: 1.25；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.8 times of stoichiometric ratio by 1.16 times of stoichiometric ratio, wherein is met with aluminum amount change of gradient number
Relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.005；By calculating, m is 72 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
96%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 85% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 80%, Na2O is 10%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 57.5%, Al
1.10%, O 0.4%, surplus Fe.
Embodiment 6
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.89: 0.67: 1.46；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.85 times of stoichiometric ratio by 1.10 times of stoichiometric ratio, wherein full with aluminum amount change of gradient number
Sufficient relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.001；By calculating, m is 250 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
95%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 20min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 20%, CaO 75%, Na2O is 5%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 30min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 55.8%, Al
1.00%, O0.35%, surplus Fe.
Embodiment 7
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.51: 0.54: 0.89；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 5 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.05,1.0,0.90,0.85 times；It obtains being added the gross mass of aluminium powder according to chemical equation to be added always to be theoretical
Quality mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 98%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 20% of total mixture material quality, and first
The mixed material that reacting furnace is added is criticized, magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain foot
To cause first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1800 DEG C, soaking time 15min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.2, speed of agitator 50rpm；Controlled at 1800 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.04；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 90%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 10min is kept the temperature and continued at 1800 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 64.3%, Al
1.82%, O 0.8%, surplus Fe.
Embodiment 8
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.53: 0.55: 0.96；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 6 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.1,0.95,0.90,0.85,0.80 times；It obtains being added the gross mass of aluminium powder according to chemical equation to add to be theoretical
Enter gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 99%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 28.6% of total mixture material quality, and the
The mixed material of reacting furnace is added in a batch, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
It is adequate to bring about first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1750 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1750 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.06；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 20%, CaO 80%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1750 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 64.0%, Al
1.20%, O 0.64%, surplus Fe.
Embodiment 9
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.55: 0.56: 1.06；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 8 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.1,1.0,0.95,0.925,0.90,0.875,0.85 times；It obtains that the total of aluminium powder is added according to chemical equation
Quality is theoretical addition gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 99%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 22.2% of total mixture material quality, and the
The mixed material of reacting furnace is added in a batch, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
It is adequate to bring about first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 5min；
Step 4: wash heat refining
(1) the 95% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.3, speed of agitator 150rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 25%, CaO 75%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 30min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 53.7%, Al
0.80%, O 0.36%, surplus Fe.
Embodiment 10
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.57: 0.56: 1.26；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.82 times of stoichiometric ratio by 1.15 times of stoichiometric ratio, wherein full with aluminum amount change of gradient number
Sufficient relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.003；By calculating, m is 110 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
97%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1750 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.3, speed of agitator 100rpm；Controlled at 1750 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.06；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 85%, Na2O is 5%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1750 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 62.0%, Al
1.30%, O 0.6%, surplus Fe.
Embodiment 11
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.58: 0.75: 1.30；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.76 times of stoichiometric ratio by 1.2 times of stoichiometric ratio, wherein is met with aluminum amount change of gradient number
Relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.001；By calculating, m is 440 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
96%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 85% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 80%, Na2O is 10%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 61.2%, Al
1.20%, O 0.48%, surplus Fe.
Embodiment 12
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.60: 0.78: 1.34；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.8 times of stoichiometric ratio by 1.12 times of stoichiometric ratio, wherein is met with aluminum amount change of gradient number
Relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.0004；By calculating, m is 800 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
92%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 20min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 20%, CaO 75%, Na2O is 5%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 30min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 61.5%, Al
1.00%, O 0.34%, surplus Fe.
Embodiment 13
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.31: 0.48: 0.82；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 5 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.05,1.0,0.90,0.85 times；It obtains being added the gross mass of aluminium powder according to chemical equation to be added always to be theoretical
Quality mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 98%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 20% of total mixture material quality, and first
The mixed material that reacting furnace is added is criticized, magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain foot
To cause first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1800 DEG C, soaking time 15min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.2, speed of agitator 50rpm；Controlled at 1800 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.04；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 90%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 10min is kept the temperature and continued at 1800 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 74.2%, Al
1.22%, O 0.78%, surplus Fe.
Embodiment 14
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.32: 0.485: 0.89；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 6 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.1,0.95,0.90,0.85,0.80 times；It obtains being added the gross mass of aluminium powder according to chemical equation to add to be theoretical
Enter gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 98%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 28.6% of total mixture material quality, and the
The mixed material of reacting furnace is added in a batch, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
It is adequate to bring about first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1750 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1750 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.06；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 20%, CaO 80%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1750 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 74.1%, Al
1.18%, O 0.56%, surplus Fe.
Embodiment 15
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.34: 0.49: 1.06；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixture
Material is divided into 8 parts；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, is followed successively by stoichiometric ratio with aluminum amount
1.20,1.1,1.0,0.95,0.925,0.90,0.875,0.85 times；It obtains that the total of aluminium powder is added according to chemical equation
Quality is theoretical addition gross mass mt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt× 99%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 22.2% of total mixture material quality, and the
The mixed material of reacting furnace is added in a batch, and magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, obtain
It is adequate to bring about first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace,
Until all materials are reacted completely, high-temperature fusant is obtained；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 5min；
Step 4: wash heat refining
(1) the 95% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.3, speed of agitator 150rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 25%, CaO 75%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 30min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 72.4%, Al
0.98%, O 0.43%, surplus Fe.
Embodiment 16
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.35: 0.49: 1.22；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.82 times of stoichiometric ratio by 1.14 times of stoichiometric ratio, wherein full with aluminum amount change of gradient number
Sufficient relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.005；By calculating, m is 64 times, when the time interval of aluminium powder flow gradients variation is overall reaction
Between divided by m.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
96%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1750 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.3, speed of agitator 100rpm；Controlled at 1750 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.06；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 85%, Na2O is 5%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1750 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 72.0%, Al
1.02%, O 0.54%, surplus Fe.
Embodiment 17
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.37: 0.5: 1.21；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.86 times of stoichiometric ratio by 1.19 times of stoichiometric ratio, wherein full with aluminum amount change of gradient number
Sufficient relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.003；By calculating, m is 110 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
95%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 10min；
Step 4: wash heat refining
(1) the 85% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 10%, CaO 80%, Na2O is 10%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 20min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 71.8%, Al
0.88%, O 0.37%, surplus Fe.
Embodiment 18
A method of ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient, specifically includes following step
It is rapid:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, specially MoO3In 150 DEG C of roastings 72h, Fe2O3Powder
In 200 DEG C of roastings 12h, CaO in 400 DEG C of roasting 20h, pretreated aluminothermy self-propagating reaction raw material is obtained；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3∶Fe2O3Powder: aluminium powder:
CaO=1.0: 0.39: 0.5: 1.23；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Aluminum powder particle size≤
2mm；Fe2O3Powder≤0.2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with equal
Uniform flow speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added with the flow velocity that gradient is successively decreased in aluminium powder, make the mixed material being continuously added to matches aluminium
Amount is gradually decrease to 0.73 times of stoichiometric ratio by 1.19 times of stoichiometric ratio, wherein full with aluminum amount change of gradient number
Sufficient relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminium
Measure change of gradient coefficient, a=0.001；By calculating, m is 460 times.
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, the reality of aluminium powder adds
Entering gross mass is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×
92%；
It is anti-that aluminothermy self-propagating reaction raw material is added continuously to progress aluminothermic reduction in reacting furnace after continuous material-mixing machine mixing
It answers, until all materials obtain high-temperature fusant after reacting completely；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, on
Layer is alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700 DEG C, soaking time 20min；
Step 4: wash heat refining
(1) the 90% of the alumina base slag total volume on upper layer is removed, alumina base slag to remaining volume and
The alloy melt of lower layer carries out eccentric mechanical stirring, eccentricity 0.4, speed of agitator 100rpm；Controlled at 1700 DEG C；
(2) lasting to stir after melt mixed is uniform, and from intermediate frequency furnace bottom using high purity inert gas as carrier gas,
CaO-CaF is blown to uniformly mixed melt2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self- propagating is anti-
Answer raw material: CaO-CaF2Base refining slag=1.0: 0.08；CaO-CaF2The ingredient and its mass percent that base refining slag contains are as follows:
CaF2For 20%, CaO 75%, Na2O is 5%.
(3) it is blown CaO-CaF2After base refining slag, eccentric mechanical stirring 30min is kept the temperature and continued at 1700 DEG C, is stopped inclined
Aligning mechanical stirring, obtains ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, obtains high-quality ferro-molybdenum.
The chemical component and its mass fraction that ferro-molybdenum manufactured in the present embodiment contains are as follows: Mo 71.1%, Al
0.60%, O 0.28%, surplus Fe.
Claims (6)
1. a kind of method for preparing ferro-molybdenum with wash heat refining based on the reduction of aluminothermy self- propagating gradient, which is characterized in that specific
The following steps are included:
Step 1: material pretreatment
Aluminothermy self-propagating reaction raw material is pre-processed respectively, obtains pretreated aluminothermy self-propagating reaction raw material；
The pretreated mode are as follows: by MoO3, Fe2O3Powder, CaO are roasted respectively, and 150~400 DEG C of maturing temperature,
12~48h of calcining time；
The aluminothermy self-propagating reaction raw material includes MoO3、Fe2O3Powder, aluminium powder and CaO；
According to the ratio, pretreated aluminothermy self-propagating reaction raw material, in mass ratio, MoO are weighed3: Fe2O3Powder: aluminium powder: CaO=
1.0: (0.32~0.95): (0.48~0.69): (0.82~1.62)；
In the aluminothermy self-propagating reaction raw material, the granularity of each raw material is respectively as follows: MoO3≤2mm；Fe2O3≤0.2mm；Aluminium
Powder Particle Size≤2mm；CaO granularity≤0.2mm；
Step 2: aluminothermy self-propagating reaction
Aluminothermy self-propagating reaction is carried out using one of following two feed way:
Feed way one:
The aluminothermy self-propagating reaction raw material in addition to aluminium powder of weighing is uniformly mixed, mixed material is obtained, by mixed material point
For several pieces；
The sequence of reacting furnace is added according to every part of mixed material, matches aluminium respectively, with aluminum amount according to the 1.10 of reactive chemistry metering ratio
~1.30 times are gradually decrease to 0.9~0.7 times of stoichiometric ratio；Total matter that aluminium powder is added is obtained according to chemical equation
Gross mass m is added to be theoretical in amountt, the gross mass that is actually added into of aluminium powder is ma, wherein ma=mt×(90~100)%；
Wherein, the quality of first mixed material that reacting furnace is added accounts for the 10 ~ 30% of total mixture material quality, and first
The mixed material of reacting furnace is added, magnesium powder need to be added as ignition substance, light mixed material and cause self-propagating reaction, be enough
Cause first high-temperature fusant of subsequent reactions；
According to the sequence that the stoichiometric ratio with aluminum amount successively reduces, successively plus other parts of mixed materials are into reacting furnace, until
All materials are reacted completely, obtain high-temperature fusant；
Feed way two:
Aluminothermy self-propagating reaction raw material in addition to aluminium powder is uniformly mixed, mixed material is obtained, by mixed material with uniform flow
Speed is fed in continuous material-mixing machine；
Meanwhile continuous material-mixing machine is added in the flow velocity that aluminium powder is successively decreased with gradient, make the mixed material being continuously added to aluminum amount by
1.10~1.30 times of stoichiometric ratio are gradually decrease to 0.9~0.7 times of stoichiometric ratio, wherein match aluminum amount change of gradient
Number meets relational expression:
M=(b-c) ÷ a (1)
In formula, m is the number with aluminum amount change of gradient, and b is highest with aluminum amount, and c is minimum aluminum amount of matching, and a is with aluminum amount ladder
Spend variation coefficient, 0 < a≤0.05；
It obtains being added the gross mass of aluminium powder according to chemical equation and gross mass m is added to be theoreticalt, being actually added into for aluminium powder be total
Quality is ma, wherein gross mass m is added in theorytIt is m with gross mass is actually added intoaMeet following relationship: ma=mt×(90~
100)%；
Aluminothermy self-propagating reaction raw material is added continuously to carry out thermite reaction in reacting furnace after continuous material-mixing machine mixing, directly
High-temperature fusant is obtained after reacting completely to all materials；
Step 3: molten point under electromagnetic field effect
High-temperature fusant is heated using electromagnetic induction, molten point of heat preservation is carried out, realizes the separation of slag gold, obtain layering melt, upper layer is
Alumina base slag, lower layer's alloy melt；Wherein, during melting point, controlled at 1700~1800 DEG C, soaking time 5~
15min；
Step 4: wash heat refining
(1) the 85 ~ 95% of the alumina base slag total volume on upper layer are removed, alumina base slag to remaining volume and under
The alloy melt of layer carries out eccentric mechanical stirring, 50~150rpm of speed of agitator；Controlled at 1700~1800 DEG C；
(2) lasting to stir after melt mixed is uniform, and using high purity inert gas as carrier gas, it is blown to uniformly mixed melt
CaO-CaF2Base refining slag carries out wash heat refining；Wherein, in mass ratio, aluminothermy self-propagating reaction raw material: CaO-CaF2Base refining
Slag=1.0: (0.02~0.10)；CaO-CaF2Base refining slag is one of following two:
The first: in mass ratio 10~25% CaF2, surplus CaO；
Second: in mass ratio 10~25% CaF2, 5~10% Na2O, surplus CaO；
(3) it is blown CaO-CaF2After base refining slag, is kept the temperature at 1700 ~ 1800 DEG C and continue eccentric 10~30min of mechanical stirring, obtained
To ferro-molybdenum melt；
Step 5: cooling
After ferro-molybdenum melt is cooled to room temperature, the smelting slag on top is removed, ferro-molybdenum is obtained；
The chemical component and its mass fraction that the ferro-molybdenum of preparation contains are as follows: Mo is 55.0~75.0%, Al≤2.0%, O
≤ 1%, surplus Fe.
2. the method that ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient as described in claim 1,
It is characterized in that, in the step 2, the several pieces are n parts, n >=4.
3. the method that ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient as described in claim 1,
It is characterized in that, in the step 3, the equipment of the electromagnetic induction is intermediate frequency furnace, and the frequency of electromagnetic field is greater than etc.
In 1000Hz.
4. the method that ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient as described in claim 1,
It is characterized in that, in the step 4, the eccentric mechanical stirring, eccentricity is 0.2 ~ 0.4.
5. the method that ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient as described in claim 1,
It is characterized in that, in the step 4, the blowing is preferably blown in Medium frequency induction furnace bottom.
6. the method that ferro-molybdenum is prepared with wash heat refining based on the reduction of aluminothermy self- propagating gradient as described in claim 1,
It is characterized in that, in the step 4, the high purity inert gas is high-purity argon gas, and purity is more than or equal to 99.95%.
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