CN110331329B - Preparation method of ferro-molybdenum alloy for smelting high-speed steel - Google Patents
Preparation method of ferro-molybdenum alloy for smelting high-speed steel Download PDFInfo
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Abstract
The invention discloses a preparation method of a ferro-molybdenum alloy for smelting high-speed steel, which comprises the following steps: firstly, adding molybdenum oxide, a loosening agent, a fluxing agent, a reducing agent and a desulfurizing agent into a mixer, uniformly mixing to obtain a mixed raw material, then adding the mixed raw material into a furnace cavity of an electric furnace, heating and preserving heat at 100-300 ℃ for 5-10 min, then heating to 1300-1800 ℃ and preserving heat for 40-110 min, finishing smelting of mixed auxiliary materials, naturally cooling to room temperature to obtain a ferromolybdenum alloy cake, and crushing to obtain the ferromolybdenum alloy for smelting high-speed steel. The method omits auxiliary materials with high unit cost as reducing agents, greatly reduces the ferromolybdenum alloy smelting cost, and increases the carbon content in ferromolybdenum alloy products. In addition, the electric furnace is adopted for heating, so that the process of ferromolybdenum smelting can be controlled by adjusting the temperature and the time, and the purposes of energy conservation and emission reduction are achieved.
Description
Technical Field
The invention belongs to the technical field of alloy material preparation, and particularly relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel.
Background
Molybdenum is used as a metal product, and has the characteristics of higher melting point, good high-temperature strength, excellent thermal shock resistance, lower high-temperature creep rate, smaller neutron absorption cross section, quick heat and electricity conduction response, low linear expansion coefficient and the like, so that the molybdenum can be widely applied to the fields of vacuum high-temperature furnace bodies, electronic instruments, aerospace, weapon equipment, ships, nuclear power and the like; as chemical products, including molybdenum disulfide with lubricating effect, ammonium molybdate and molybdenum oxide with catalytic effect, the molybdenum disulfide, the ammonium molybdate and the molybdenum oxide with catalytic effect are widely applied to the fields of machinery, petroleum, textile, printing and dyeing, papermaking, pigments and the like; in the field of steel smelting, molybdenum has a solid solution strengthening effect on ferrite, so that the strength and hardness of steel can be enhanced, and the re-passivation capability of steel can be improved, so that the pitting corrosion resistance and crevice corrosion resistance of stainless steel can be improved, the high temperature strength of steel can be improved, the high temperature durability and creep property of steel can be greatly improved, the acid and alkali resistance of steel can be improved, secondary strengthening effect can be achieved, the wear resistance and toughness of steel can be improved, the hardenability and weldability of steel can be improved, and according to the report of related documents, the application of molybdenum as an additive in the field of molybdenum-containing steel smelting accounts for more than 80% of the total consumption of molybdenum in the whole world.
In the field of molybdenum-containing steel smelting, commonly used molybdenum-containing additives mainly comprise traditional ferromolybdenum alloy, pure molybdenum oxide blocks, composite molybdenum oxide blocks, steel-making metal molybdenum strips and the like. The traditional ferromolybdenum preparation adopts an external silicoaluminothermic reduction method, and the method mainly has the defects of high consumption cost of raw and auxiliary materials, overhigh reduction reaction temperature, difficulty in controlling the intermediate process, aggravated environmental pollution of generated flue gas and waste slag, poor working condition of a smelting site, high labor cost and the like. The molybdenum oxide block is used as a steelmaking additive, so that although one smelting process is reduced, the processing cost of the ferro-molybdenum alloy is reduced, and the environmental pollution is reduced, the molybdenum oxide block has the defects of low density, volatility and the like, and can cause the adverse factors of low yield of molybdenum metal, pollution damage of steelmaking equipment, adjustment of the traditional steelmaking process and the like in the smelting process of the molybdenum-containing steel. For the steelmaking molybdenum strip, the preparation of the steelmaking molybdenum strip needs processes of roasting, water washing, acid-base leaching, ammonia leaching, drying, secondary roasting, two-stage reduction, pressing, sintering, forging and the like, the processing process is overlong, the production cost is overhigh, the pollution of three wastes is serious, and the molybdenum strip has higher density, can sink at the bottom of molten steel in the steelmaking process, is not beneficial to uniform diffusion of molybdenum elements and reduces the yield of molybdenum metal. The commonly used molybdenum-containing additive can be used for smelting high-speed steel, but has the disadvantages of high raw material consumption and auxiliary material cost, difficult control of reaction process and temperature, environmental pollution aggravation, resource waste, low molybdenum yield, overhigh product preparation cost and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which reduces the smelting cost of the ferromolybdenum alloy and increases the carbon content in the ferromolybdenum alloy product.
The technical scheme adopted by the invention is that the preparation method of the ferro-molybdenum alloy for smelting the high-speed steel is implemented according to the following steps:
step 1, mixing a mixture of 3.5-4.5: 2.5-4: 0.3-0.5: 1.5-2: adding 0.7-1 parts of molybdenum oxide, a loosening agent, a fluxing agent, a reducing agent and a desulfurizing agent into a mixer, and uniformly mixing to obtain a mixed raw material;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, wherein the heating temperature is 100-300 ℃, the heat preservation time is 5-10 min, removing the water in the mixed raw material, then heating to 1300-1800 ℃, preserving the heat for 40-110 min, completing the smelting of the mixed auxiliary material, and naturally cooling to the room temperature to obtain a ferromolybdenum alloy cake;
and 3, crushing the ferro-molybdenum alloy cake to obtain the ferro-molybdenum alloy for smelting the high-speed steel.
The present invention is also characterized in that,
in the step 1, the rotating speed of the mixer is 960 r/min-1500 r/min, and the mixing time is 10 min-30 min.
In the step 1, the molybdenum oxide is industrial molybdenum oxide, the content of molybdenum is 45-55%, and the granularity is not more than 3 mm; the loosening agent is ferric oxide powder, the mass fraction of the loosening agent is not less than 98.5%, and the granularity is not more than 1 mm; the fluxing agent is ammonia leaching residue, the molybdenum content of the fluxing agent is 10-30%, and the granularity is not more than 5 mm; the reducing agent is carbon powder, the mass fraction of the reducing agent is not less than 99.5%, and the granularity is not more than 0.5 mm; the desulfurizer is calcium oxide, the mass fraction of the calcium oxide is not less than 98 percent, and the particle size is not more than 0.5 mm.
The preparation method of the ammonia leaching residue comprises the following specific steps:
step 1.1, putting industrial molybdenum oxide and dilute nitric acid into a reaction kettle for acid washing reaction, and then filtering to obtain a solid substance, namely an industrial molybdenum oxide filter cake;
the reaction temperature is 75-90 ℃, and the reaction time is 1-2 h;
the mass ratio of the industrial molybdenum oxide to the dilute nitric acid is 1: 3;
step 1.2, putting the industrial molybdenum oxide filter cake obtained in the step 1.1 and dilute ammonia water into a reaction kettle for ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, namely the free ammonia reaches a certain value, sucking supernatant liquid, and sending the supernatant liquid to an ammonium molybdate storage tank for storage and clarification; then injecting dilute ammonia water into the reaction kettle, carrying out secondary ammonia leaching to improve the metal leaching rate, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the secondary ammonia leaching is finished, wherein the filter residue is ammonia leaching residue, returning the obtained filtrate to primary ammonia leaching, namely injecting the dilute ammonia water into the filtrate for ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the ammonia leaching is finished, namely the ammonia leaching residue, and mixing the filter residues obtained by each ammonia leaching reaction to obtain the ammonia leaching residue.
In the step 3, the particle size of the ferro-molybdenum alloy is between 10mm and 100 mm.
The beneficial effect of the invention is that,
the method abandons the raw material selection of the traditional method, omits auxiliary materials with high unit cost as a reducing agent, selects carbon powder as the reducing agent, greatly reduces the ferromolybdenum alloy smelting cost, and increases the carbon content in the ferromolybdenum alloy product. In addition, the electric furnace is adopted for heating, so that the process of ferromolybdenum smelting can be controlled by adjusting the temperature and the time, and the purposes of energy conservation and emission reduction are achieved.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which is implemented according to the following steps:
step 1, mixing a mixture of 3.5-4.5: 2.5-4: 0.3-0.5: 1.5-2: adding 0.7-1 parts of molybdenum oxide, a loosening agent, a fluxing agent, a reducing agent and a desulfurizing agent into a mixer, and uniformly mixing to obtain a mixed raw material;
the rotating speed of the mixer is 960 r/min-1500 r/min, and the mixing time is 10 min-30 min.
The molybdenum oxide is industrial molybdenum oxide, wherein the content of molybdenum is 45-55%, and the granularity is not more than 3 mm;
the loosening agent is ferric oxide powder, the mass fraction of the loosening agent is not less than 98.5%, and the granularity is not more than 1 mm;
the fluxing agent is ammonia leaching residue, the molybdenum content of the fluxing agent is 10-30%, and the granularity is not more than 5 mm;
the reducing agent is carbon powder, the mass fraction of the reducing agent is not less than 99.5%, and the granularity is not more than 0.5 mm;
the desulfurizer is calcium oxide, the mass fraction of the desulfurizer is not less than 98 percent, and the particle size is not more than 0.5 mm;
the preparation method of the ammonia leaching residue comprises the following specific steps:
step 1.1, putting industrial molybdenum oxide and dilute nitric acid into a reaction kettle for acid washing reaction, and then filtering to obtain a solid substance, namely an industrial molybdenum oxide filter cake;
the reaction temperature is 75-90 ℃, and the reaction time is 1-2 h;
the mass ratio of the industrial molybdenum oxide to the dilute nitric acid is 1: 3;
the process can remove alkali metal and alkaline earth metal and part of harmful impurities such as copper, nickel, iron and the like in industrial molybdenum oxide;
step 1.2, putting the industrial molybdenum oxide filter cake obtained in the step 1.1 and dilute ammonia water into a reaction kettle for ammonia leaching, leaching out impurity ions such as copper, zinc, nickel, iron and the like in molybdate, adding the impurity ions into a solution in the form of double salt, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1 hour at the temperature of 70 ℃, namely, absorbing supernatant, sending the supernatant into an ammonium molybdate storage tank for storage and clarification; then injecting dilute ammonia water into the reaction kettle, carrying out secondary ammonia leaching to improve the metal leaching rate, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the secondary ammonia leaching is finished, wherein filter residues are ammonia leaching residues, returning the obtained filtrate to the primary ammonia leaching, namely injecting the dilute ammonia water into the filtrate, carrying out ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the ammonia leaching is finished, namely the ammonia leaching residues, and mixing the filter residues obtained by each ammonia leaching reaction to obtain the ammonia leaching residues in the method;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, heating the mixed raw material under the action of heat radiation, heating to 100-300 ℃, preserving heat for 5-10 min, removing water in the mixed raw material, heating to 1300-1800 ℃, preserving heat for 40-110 min, finishing smelting of mixed auxiliary materials, and naturally cooling to room temperature to obtain a ferromolybdenum alloy cake;
step 3, crushing the ferro-molybdenum alloy cake to obtain ferro-molybdenum alloy for smelting high-speed steel;
the grain size of the ferro-molybdenum alloy is between 10mm and 100 mm.
Compared with the prior art, the method of the invention has the following advantages:
1. the yield of molybdenum metal is improved. In the traditional molybdenum metallurgy industrial chain, the ammonia leaching slag is generally accumulated as solid waste or is treated at low cost, so that the environmental sanitation of a working place is influenced, and the loss of the molybdenum metal amount is also caused.
2. So that the ferromolybdenum smelting is controllable and adjustable. The traditional ferromolybdenum smelting is usually completed by adopting a silicon-aluminum hot furnace external method, once the temperature and the reaction process cannot be controlled after ignition, the reaction temperature is above 2000 ℃, and a large amount of energy consumption and environmental pollution are caused.
3. Greatly reduces the smelting cost of the ferro-molybdenum alloy for preparing high-speed steel. The auxiliary materials usually selected in the traditional ferromolybdenum smelting comprise aluminum powder, ferrosilicon powder and the like, the unit cost is high, the method abandons the selection of raw materials in the traditional method, eliminates the auxiliary materials with high unit cost as a reducing agent, greatly reduces the ferromolybdenum alloy smelting cost, and simultaneously, because the carbon content in high-speed steel is between 0.65 and 1.75 percent, the requirement of smelting high-speed steel on the carbon content in the ferromolybdenum alloy is not high (the carbon content in the traditional ferromolybdenum alloy is not more than 0.1 percent), the carbon powder is selected as the reducing agent in the method, the ferromolybdenum alloy smelting cost is reduced, and the carbon content in the ferromolybdenum alloy product is increased.
Example 1
The invention relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which is implemented according to the following steps:
step 1, selecting an industrial molybdenum oxide raw material with a molybdenum content of 45% and a granularity of not more than 3mm, ferric oxide powder with a mass fraction of not less than 98.5% and a granularity of not more than 1mm, carbon powder with a mass fraction of not less than 99.5% and a granularity of not more than 0.5mm, ammonia leaching residue with a molybdenum content of 12% and a granularity of not more than 5mm, and calcium oxide powder with a mass fraction of not less than 98% and a granularity of not more than 0.5mm, and sequentially mixing the raw materials according to a mass ratio of 3.7: 3.5: 1.72: 0.35: 0.73, adding the mixture into a mixer, and uniformly mixing to obtain mixed raw materials;
the rotating speed of the mixer is 1000r/min, and the mixing time is 20 min;
the preparation method of the ammonia leaching residue comprises the following specific steps:
step 1.1, putting industrial molybdenum oxide and dilute nitric acid into a reaction kettle for acid washing reaction, and then filtering to obtain a solid substance, namely an industrial molybdenum oxide filter cake;
the reaction temperature is 75 ℃, and the reaction time is 1 h;
the mass ratio of the industrial molybdenum oxide to the dilute nitric acid is 1: 3;
step 1.2, putting the industrial molybdenum oxide filter cake obtained in the step 1.1 and dilute ammonia water into a reaction kettle for ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, namely the free ammonia reaches a certain value, sucking supernatant liquid, and sending the supernatant liquid to an ammonium molybdate storage tank for storage and clarification; then injecting dilute ammonia water into the reaction kettle, carrying out secondary ammonia leaching to improve the metal leaching rate, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the secondary ammonia leaching is finished, wherein filter residues are ammonia leaching residues, returning the obtained filtrate to the primary ammonia leaching, namely injecting the dilute ammonia water into the filtrate, carrying out ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the ammonia leaching is finished, namely the ammonia leaching residues, and mixing the filter residues obtained by each ammonia leaching reaction to obtain the ammonia leaching residues in the method;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, heating the mixed raw material under the action of heat radiation, wherein the heating temperature is 200 ℃, the heat preservation time is 10min, removing water in the mixed raw material, heating to 1450 ℃, preserving heat for 50min, finishing smelting of the mixed auxiliary material, and naturally cooling to room temperature to obtain a ferromolybdenum alloy cake;
step 3, crushing the ferro-molybdenum alloy cake to obtain ferro-molybdenum alloy for smelting high-speed steel;
the grain size of the ferro-molybdenum alloy is between 10mm and 100 mm.
Through detection, the ferromolybdenum with the molybdenum content of 50 percent by mass has the molybdenum content of 52.46 percent, the carbon content of 4.37 percent and the sulfur content of 0.043 percent.
Example 2
The invention relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which is implemented according to the following steps:
step 1, selecting an industrial molybdenum oxide raw material with a molybdenum content of 50% and a granularity of not more than 3mm, ferric oxide powder with a mass fraction of not less than 98.5% and a granularity of not more than 1mm, carbon powder with a mass fraction of not less than 99.5% and a granularity of not more than 0.5mm, ammonia leaching residue with a molybdenum content of 12% and a granularity of not more than 5mm, and calcium oxide powder with a mass fraction of not less than 98% and a granularity of not more than 0.5mm, and sequentially according to a mass ratio of 4: 3.1: 1.75: 0.36: 0.71, adding the mixture into a mixer, and uniformly mixing to obtain a mixed raw material;
the rotating speed of the mixer is 960r/min, and the mixing time is 20 min;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, heating the mixed raw material under the action of heat radiation, wherein the heating temperature is 200 ℃, the heat preservation time is 10min, removing water in the mixed raw material, then heating to 1550 ℃, preserving heat for 70min, finishing smelting of the mixed auxiliary material, and naturally cooling to room temperature to obtain a ferromolybdenum alloy cake;
step 3, crushing the ferro-molybdenum alloy cake to obtain ferro-molybdenum alloy for smelting high-speed steel;
the grain size of the ferro-molybdenum alloy is between 10mm and 100 mm.
Through detection, the ferromolybdenum containing 55% of molybdenum by mass has the molybdenum content of 56.89%, the carbon content of 3.96% and the sulfur content of 0.062%.
Example 3
The invention relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which is implemented according to the following steps:
step 1, selecting an industrial molybdenum oxide raw material with a molybdenum content of 55% and a granularity of not more than 3mm, ferric oxide powder with a mass fraction of not less than 98.5% and a granularity of not more than 1mm, carbon powder with a mass fraction of not less than 99.5% and a granularity of not more than 0.5mm, ammonia leaching residue with a molybdenum content of 12% and a granularity of not more than 5mm, and calcium oxide powder with a mass fraction of not less than 98% and a granularity of not more than 0.5mm, and sequentially mixing the raw materials according to a mass ratio of 4.4: 2.8: 1.76: 0.37: 0.7, adding the mixture into a mixer, and uniformly mixing to obtain mixed raw materials;
the rotating speed of the mixer is 1000r/min, and the mixing time is 20 min;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, heating the mixed raw material under the action of heat radiation, wherein the heating temperature is 200 ℃, the heat preservation time is 10min, removing water in the mixed raw material, then heating to 1650 ℃, preserving heat for 90min, finishing smelting of the mixed auxiliary material, and naturally cooling to room temperature to obtain a ferromolybdenum alloy cake;
step 3, crushing the ferro-molybdenum alloy cake to obtain ferro-molybdenum alloy for smelting high-speed steel;
the grain size of the ferro-molybdenum alloy is between 10mm and 100 mm.
Through detection, the ferromolybdenum with the molybdenum content of 60 percent by mass has the molybdenum content of 62.38 percent, the carbon content of 3.50 percent and the sulfur content of 0.058 percent.
Example 4
The invention relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which is implemented according to the following steps:
step 1, mixing a mixture of a: 3: 0.4: 1.8: adding 0.9 of molybdenum oxide, a loosening agent, a fluxing agent, a reducing agent and a desulfurizing agent into a mixer, and uniformly mixing to obtain a mixed raw material;
the rotating speed of the mixer is 960r/min, and the mixing time is 10 min;
the molybdenum oxide is industrial molybdenum oxide, wherein the content of molybdenum is 45%, and the granularity is not more than 3 mm;
the loosening agent is ferric oxide powder, the mass fraction of the loosening agent is not less than 98.5%, and the granularity is not more than 1 mm;
the fluxing agent is ammonia leaching residue, the molybdenum content of the fluxing agent is 10 percent, and the granularity is not more than 5 mm;
the reducing agent is carbon powder, the mass fraction of the reducing agent is not less than 99.5%, and the granularity is not more than 0.5 mm;
the desulfurizer is calcium oxide, the mass fraction of the desulfurizer is not less than 98 percent, and the particle size is not more than 0.5 mm;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, heating the mixed raw material under the action of heat radiation, wherein the heating temperature is 100 ℃, the heat preservation time is 5min, removing water in the mixed raw material, then heating to 1300 ℃, preserving heat for 40min, finishing smelting of the mixed auxiliary material, and naturally cooling to room temperature to obtain a ferromolybdenum alloy cake;
step 3, crushing the ferro-molybdenum alloy cake to obtain ferro-molybdenum alloy for smelting high-speed steel;
the grain size of the ferro-molybdenum alloy is between 10mm and 100 mm.
Example 5
The invention relates to a preparation method of a ferromolybdenum alloy for smelting high-speed steel, which is implemented according to the following steps:
step 1, mixing a mixture of a: 4: 0.5: 2: adding the molybdenum oxide, the loosening agent, the fluxing agent, the reducing agent and the desulfurizing agent of 1 into a mixer, and uniformly mixing to obtain a mixed raw material;
the rotating speed of the mixer is 1500r/min, and the mixing time is 30 min;
the molybdenum oxide is industrial molybdenum oxide, wherein the content of molybdenum is 55%, and the granularity is not more than 3 mm;
the loosening agent is ferric oxide powder, the mass fraction of the loosening agent is not less than 98.5%, and the granularity is not more than 1 mm;
the fluxing agent is ammonia leaching residue, the molybdenum content of the fluxing agent is 30%, and the granularity is not more than 5 mm;
the reducing agent is carbon powder, the mass fraction of the reducing agent is not less than 99.5%, and the granularity is not more than 0.5 mm;
the desulfurizer is calcium oxide, the mass fraction of the desulfurizer is not less than 98 percent, and the particle size is not more than 0.5 mm;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, heating the mixed raw material under the action of heat radiation, wherein the heating temperature is 300 ℃, the heat preservation time is 10min, removing water in the mixed raw material, then heating to 1800 ℃, preserving heat for 110min, finishing smelting of the mixed auxiliary material, and naturally cooling to room temperature to obtain a ferromolybdenum alloy cake;
step 3, crushing the ferro-molybdenum alloy cake to obtain ferro-molybdenum alloy for smelting high-speed steel;
the grain size of the ferro-molybdenum alloy is between 10mm and 100 mm.
The preparation method for producing the ferromolybdenum alloy for the high-speed steel, which is disclosed by the invention, has the advantages that the batching cost of raw and auxiliary materials can be greatly reduced, the smelting time of the ferromolybdenum alloy is shortened, the smelting temperature of the ferromolybdenum alloy is accurately controlled and reduced, the resource utilization rate is improved, meanwhile, the smelting process of the ferromolybdenum alloy is refined, the working condition of a smelting site is improved, the production energy consumption of the ferromolybdenum alloy is greatly reduced, the environmental protection problem caused by smelting smoke is reduced, and the obvious economic benefit and social benefit are achieved.
Claims (3)
1. The preparation method of the ferro-molybdenum alloy for smelting the high-speed steel is characterized by comprising the following steps:
step 1, mixing a mixture of 3.5-4.5: 2.5-4: 0.3-0.5: 1.5-2: adding 0.7-1 parts of molybdenum oxide, a loosening agent, a fluxing agent, a reducing agent and a desulfurizing agent into a mixer, and uniformly mixing to obtain a mixed raw material; the molybdenum oxide is industrial molybdenum oxide, the content of molybdenum is 45-55%, and the granularity is not more than 3 mm; the loosening agent is ferric oxide powder, the mass fraction of the loosening agent is not less than 98.5%, and the granularity is not more than 1 mm; the fluxing agent is ammonia leaching residue, the molybdenum content of the fluxing agent is 10-30%, and the granularity is not more than 5 mm; the reducing agent is carbon powder, the mass fraction of the reducing agent is not less than 99.5%, and the granularity is not more than 0.5 mm; the desulfurizer is calcium oxide, the mass fraction of the desulfurizer is not less than 98 percent, and the particle size is not more than 0.5 mm;
the preparation method of the ammonia leaching residue comprises the following specific steps:
step 1.1, putting industrial molybdenum oxide and dilute nitric acid into a reaction kettle for acid washing reaction, and then filtering to obtain a solid substance, namely an industrial molybdenum oxide filter cake;
the reaction temperature is 75-90 ℃, and the reaction time is 1-2 h;
the mass ratio of the industrial molybdenum oxide to the dilute nitric acid is 1: 3;
step 1.2, putting the industrial molybdenum oxide filter cake obtained in the step 1.1 and dilute ammonia water into a reaction kettle for ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, namely the free ammonia reaches a certain value, sucking supernatant liquid, and sending the supernatant liquid to an ammonium molybdate storage tank for storage and clarification; then injecting dilute ammonia water into the reaction kettle, carrying out secondary ammonia leaching to improve the metal leaching rate, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the secondary ammonia leaching is finished, wherein filter residues are ammonia leaching residues, returning the obtained filtrate to primary ammonia leaching, namely injecting the dilute ammonia water into the filtrate for ammonia leaching, adjusting the temperature of the reaction kettle to 70 ℃, dropwise adding the dilute ammonia water into the mixed solution until the pH value of the solution is 8.5-9.0, reacting for 1h at the temperature of 70 ℃, discharging and filtering after the ammonia leaching is finished, namely the ammonia leaching residues are obtained, and mixing the filter residues obtained by each ammonia leaching reaction to obtain the ammonia leaching residues;
step 2, adding the mixed raw material obtained in the step 1 into an electric furnace cavity for heating and heat preservation, wherein the heating temperature is 100-300 ℃, the heat preservation time is 5-10 min, removing the water in the mixed raw material, then heating to 1300-1800 ℃, preserving the heat for 40-110 min, completing the smelting of the mixed auxiliary material, and naturally cooling to the room temperature to obtain a ferromolybdenum alloy cake;
and 3, crushing the ferro-molybdenum alloy cake to obtain the ferro-molybdenum alloy for smelting the high-speed steel.
2. The method for preparing a ferro-molybdenum alloy for smelting high-speed steel according to claim 1, wherein in the step 1, the rotating speed of a mixer is 960 r/min-1500 r/min, and the mixing time is 10 min-30 min.
3. A method of preparing a ferro-molybdenum alloy for smelting high speed steel as claimed in claim 1, wherein in said step 3, the ferro-molybdenum alloy has a grain size of 10mm to 100 mm.
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