CN107699779A - A kind of VN alloy and its production method - Google Patents
A kind of VN alloy and its production method Download PDFInfo
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- CN107699779A CN107699779A CN201710758219.1A CN201710758219A CN107699779A CN 107699779 A CN107699779 A CN 107699779A CN 201710758219 A CN201710758219 A CN 201710758219A CN 107699779 A CN107699779 A CN 107699779A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C35/00—Master alloys for iron or steel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1089—Alloys containing non-metals by partial reduction or decomposition of a solid metal compound
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
Abstract
The invention discloses a kind of VN alloy and its production method.The inventive method includes：Vanadium-containing compound mechanical activation is handled, then adds reaction promoter, carbonaceous material and binding agent under the conditions of vapours and obtains compound；A mechanical-moulded coarse fodder block after compound is placed 24 hours, room temperature ageing processing 2h 3h obtain secondary coarse material block；Secondary coarse material block 250 DEG C of drying stage 200 DEG C in High Purity Nitrogen atmosphere calcining kiln, 1000 DEG C of 15h 17h, temperature rise period 500 DEG C, 1350 DEG C of 7.5h 8.5h, carbonation stage 1000 DEG C, 1500 DEG C of 4h 6h, sintering stage 1350 DEG C, 7h 9h and after being cooled to 75 DEG C 80 DEG C cooling come out of the stove to obtain VN alloy finished product.The inventive method shortens the production time, improves production efficiency, improves product density and the daily output, and vanadium, nitrogen content are also higher in vanadium-nitrogen alloy product.
Description
Technical field
The present invention relates to field of steel production, more particularly to a kind of VN alloy and its production method.
Background technology
At present, when producing V-alloyed steel iron material, realized usually using the method for addition vanadium-containing alloy.In order to reduce vanadium
Addition, the toughness and tenacity for improving steel, vanadium-containing alloy are added preferably in the form of VN alloy, and therefore, steel is produced to excellent
The demand of matter VN alloy increasingly increases.At present, although the production method of VN alloy is more, such as the nitridation of vacuum method, normal pressure
Method etc., and production has been reached higher level, but the problems such as yield is relatively low, quality is unstable all be present in it, in order to improve vanadium
The product quality of nitrogen alloy, production cost is reduced, be badly in need of a kind of production method of high-quality, economic VN alloy.
Prior art discloses a kind of production method of VN alloy：First will be by vfanadium compound, reaction promoter, carbon containing thing
After matter is placed 24 hours with bonding compound, then the compound machinery after placement is shaped to coarse fodder block, then coarse fodder block is entered
Row Ageing Treatment, i.e., by coarse fodder block, naturally dry, processing time are more than or equal to 48 hours at normal temperatures.
The coarse fodder block density of this production method obtained by molding is low, and moisture content is up to 5% or so, and its shortcoming has：1st, its is right
The processing time of coarse fodder block is up to 48 hours, thus less efficient.2nd, simultaneously, the VN alloy finally given by the method
The density of product is relatively low, about 2.8g/cm3Left and right, and the density of VN alloy is to influence absorptivity of the molten steel to VN alloy
A key factor, therefore also just reduce absorptivity of the molten steel to it.3rd, when the density of vanadium-nitrogen alloy product is relatively low, also lead
Cause product is more loose, low intensity, and then causes more finished product disintegrating slag and form waste.
The content of the invention
In view of this, the embodiments of the invention provide a kind of VN alloy and its production method, main purpose is to improve effect
Rate, improve vanadium-nitrogen alloy product density.
To reach above-mentioned purpose, invention broadly provides following technical scheme：
On the one hand, the embodiments of the invention provide a kind of production method of VN alloy, including：Vanadium-containing compound is carried out
Mechanical activation processing, adds reaction promoter, carbonaceous material and binding agent and obtains compound；It is small that the compound is placed 24
When after it is mechanical-moulded be a coarse fodder block, a coarse fodder block carries out Ageing Treatment and obtains secondary coarse material block at normal temperatures；Institute
Secondary coarse material block is stated in the calcining kiln of High Purity Nitrogen atmosphere successively by baking stage, temperature rise period, carbonation stage, sintering stage
And cooling stage, afterwards cooling are come out of the stove, and obtain VN alloy finished product；
Vanadium-containing compound, the reaction promoter, the carbonaceous material and the binding agent after the activation process are
It is stirred to obtain the compound under the conditions of temperature is 75 DEG C of -80 DEG C of vapours；
The time of the Ageing Treatment is 2h-3h；
The temperature of the baking stage is 200 DEG C -250 DEG C, drying time 15h-17h；
The temperature of the temperature rise period is 500 DEG C -1000 DEG C, heating-up time 7.5h-8.5h；
The temperature of the carbonation stage is 1000 DEG C -1350 DEG C, carbonization time 4h-6h；
The temperature of the sintering stage is 1350 DEG C -1500 DEG C, sintering time 7h-9h；
The temperature of the cooling stage is 75 DEG C -80 DEG C.
Preferably, the mechanical activation processing is to use Ginding process, milling time 1h；The vanadium-containing compound is ground
Particle diameter after mill is -180 mesh.
Preferably, vanadium-containing compound, the reaction promoter, the carbonaceous material after the activation process and described
The weight ratio of binding agent is 70-85: 3-5: 10-25: 0.1-10.
Preferably, the vanadium-containing compound is powdery vanadic anhydride, vanadium trioxide, vanadium tetraoxide, more vanadic acid
At least one of ammonium, ammonium metavanadate, vanadium hydroxide and vanadic acid.The reaction promoter be ferrous carbonate powder, high-purity iron powder,
Melt vanadium pentoxide powder, vanadium trioxide powder, ferrovanadium dust, VN alloy powder, vanadium carbide powder or metal vanadium powder
End；The carbonaceous material be Scaly graphite powder, amorphous graphite in powder, carbon black powder, charcoal powder and graphite electrode carbon dust at least
It is a kind of.The binding agent is at least one of water, polyvinyl alcohol, tapioca starch and flour, and tapioca starch and flour are slurry.
Preferably, the high pure nitrogen is the various inlet mouth feeding from the calcining kiln；Pressure in the calcining kiln
Power is 0.1kg/cm2-0.2kg/cm2；The heating means of the calcining kiln are that resistance heating, heating plasma or high temperature nitrogen add
Heat；The concentration of volume percent of the nitrogen is 99.999%.
On the other hand, the embodiments of the invention provide a kind of VN alloy, it is prepared by the above method.
Preferably, the density of the VN alloy is 3.5g/cm3-3.9g/cm3, wherein vanadium unit cellulose content is 77%-
79%, nitrogen element content 15%-17%.
Compared with prior art, the beneficial effects of the invention are as follows：
The inventive method is by by the vanadium-containing compound after the activation process, the reaction promoter, the carbon containing thing
Matter and the mixing condition of the binding agent reduce follow-up to be stirred to obtain compound under the conditions of 75 DEG C of -80 DEG C of vapours
The time of Ageing Treatment, 2-3 hours were reduced to by original at least 48 hours, obtained secondary coarse material bulk strength is high, outer sightseeing
Sliding, product density height, moisture content are down to 2% by 5%, can be directly entered nitrogen plate klining knot；Therefore Ageing Treatment is greatly reduced
Time, improve production efficiency；Pass through the temperature and time in each stage of improving secondary coarse material block in calcining kiln, whole process again
The density for the vanadium-nitrogen alloy product for complementing each other to obtain improves, and product is closely knit, and intensity is high, and the improvement of the technique decreases finished product
The waste of disintegrating slag, the daily output may be up to more than 2t, and v element and nitrogen element content are higher in vanadium-nitrogen alloy product.
Embodiment
Be further illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below with compared with
Good embodiment, to embodiment, technical scheme, feature and its effect according to the present patent application, describe in detail as after.Under
State it is bright in multiple embodiments in special characteristic, structure or feature can be combined by any suitable form.
Embodiment 1
1100kg powderies vanadic anhydride (content of vanadium 98%) is more than or equal to 1 by grinding activation process, milling time
Hour, all add 10.5kg into the vanadic anhydride after above-mentioned activation under the conditions of vapours by -180 mesh after grinding
Ferrous carbonate powder, the Scaly graphite powder that 350kg contents are 98%, dry-mixed uniformly rear addition water 80kg, whole addition mixed
Journey is carried out in vapours, obtains compound, a mechanical-moulded coarse fodder block for 50 millimeters of Φ after placing 24 hours, coarse fodder
Block naturally dry obtains secondary coarse material block after 2 hours, the coarse fodder bulk strength height, smooth in appearance, product density after being now molded are high,
Moisture content as little as 2%；Above-mentioned secondary coarse material block is sent into calcining kiln from the charging aperture of VN alloy calcining kiln, meanwhile, by height
Pure nitrogen gas is sent into calcining kiln by different air inlets, and the concentration of volume percent of nitrogen is 99.999%；It is sent into calcining kiln
Calcination processing, the temperature of baking stage are 200 DEG C, drying time 15h, and the temperature of temperature rise period is 500 DEG C, and the heating-up time is
7.5h, the temperature of carbonation stage is 1000 DEG C, carbonization time 4h, and the temperature of sintering stage is 1350 DEG C, sintering time 7h,
Cooling stage to 80 DEG C or so rear coolings are come out of the stove, and kiln inner pressure is pressure-fired, pressure limit 0.2kg/cm3, cool down and come out of the stove
To surface quality is good, reaction is uniform, apparent density 3.90g/cm3Vanadium-nitrogen alloy product 790kg, through analysis product content of vanadium
77.5%, nitrogen content 16.58%, the quantity-produced daily output reaches 2.05t or so.
Embodiment 2
By 1100kg vanadium trioxides (content of vanadium 64.5%) by grinding activation process, it is small that milling time is more than or equal to 1
When, all by -180 mesh after grinding, into the vanadium trioxide after above-mentioned activation, addition 10.5kg melts under the conditions of vapours
Melt vanadium pentoxide powder (all by -200 mesh, vanadic anhydride grade 98%), the Scaly graphite that 290kg contents are 98%
Powder, dry-mixed uniformly rear addition water 140kg, whole mixed process of adding is carried out in vapours, obtains compound, it is small to place 24
When after a mechanical-moulded coarse fodder block for 50 millimeters of Φ, coarse fodder block naturally dry obtains secondary coarse material block after 2.5 hours, now
Coarse fodder bulk strength height, smooth in appearance, product density after shaping is high, moisture content as little as 2.2%；By above-mentioned secondary coarse material block from vanadium
The charging aperture of nitrogen alloy calcining kiln is sent into calcining kiln, meanwhile, high pure nitrogen is sent into calcining kiln by different air inlets, nitrogen
The concentration of volume percent of gas is 99.999%；Calcination processing in calcining kiln is sent into, the temperature of baking stage is 220 DEG C, drying
Time 16h, the temperature of temperature rise period is 750 DEG C, heating-up time 8h, and the temperature of carbonation stage is 1200 DEG C, and carbonization time is
5h, the temperature of sintering stage is 1400 DEG C, sintering time 8h, and cooling stage to 80 DEG C or so rear coolings is come out of the stove, kiln inner pressure
For pressure-fired, pressure limit 0.15kg/cm3, cooling comes out of the stove to obtain that surface quality is good, reaction is uniform, apparent density 3.72g/
cm3Vanadium-nitrogen alloy product 880kg, through analysis product content of vanadium 78.51%, nitrogen content 15.82%, the quantity-produced daily output
Reach 2.1t or so.
Embodiment 3
1100kg vanadium tetraoxides grade 98% is more than or equal to 1 hour by grinding activation process, milling time, grinding
Afterwards all by -180 mesh, added under the conditions of vapours into the vanadium trioxide after above-mentioned activation 11kg high-purity iron powders,
350kg contents are 95% Scaly graphite powder, and dry-mixed uniformly rear addition flour slurry 98kg, whole mixed process of adding is steamed hot
Carried out in vapour, obtain compound, a mechanical-moulded coarse fodder block for 50 millimeters of Φ after placing 24 hours, coarse fodder block naturally dry
Secondary coarse material block is obtained after 3 hours, the coarse fodder bulk strength height, smooth in appearance, product density after being now molded are high, and moisture content is as little as
2.2%；Above-mentioned secondary coarse material block is sent into calcining kiln from the charging aperture of VN alloy calcining kiln, meanwhile, by high pure nitrogen by
Different air inlets is sent into calcining kiln, and the concentration of volume percent of nitrogen is 99.999%；Calcination processing in calcining kiln is sent into,
The temperature of baking stage is 220 DEG C, drying time 16h, and the temperature of temperature rise period is 750 DEG C, heating-up time 8h, carbonation stage
Temperature be 1200 DEG C, carbonization time 5h, the temperature of sintering stage is 1400 DEG C, sintering time 8h, cooling stage to 80
DEG C or so rear cooling come out of the stove, kiln inner pressure is pressure-fired, pressure limit 0.15kg/cm3, cool down and come out of the stove to obtain surface quality
Well, reaction is uniform, apparent density 3.55g/cm3Vanadium-nitrogen alloy product 805kg, through analysis product content of vanadium 78.51%, nitrogen contains
Amount 15.86%, the quantity-produced daily output reaches 2.15t or so.
Comparative example 1
The difference of this comparative example 1 and embodiment 1 is that it is in normal temperature condition that the addition of compound, which is stirred process,
Lower progress；The moisture content of thick block is up to 4.9% or so after Ageing Treatment；It is 400 DEG C in the temperature of calcining kiln drying stage,
The temperature of carbonation stage is 1600 DEG C, and the temperature of nitridation stage is 1350 DEG C, cooling stage be water cooling to being no more than 100 DEG C, forge
It is 6 hours to burn the time, and the apparent density for finally obtaining VN alloy is 3.2g/cm3, it is 77.25% through analysis product content of vanadium,
Nitrogen content is 15.8%, and the quantity-produced daily output reaches 1100kg.
Comparative example 2
The difference of this comparative example 2 and embodiment 2 is that it is in normal temperature condition that the addition of compound, which is stirred process,
Lower progress；The moisture content of thick block is up to 5.12% or so after Ageing Treatment；It is 300 in the temperature of calcining kiln drying stage
DEG C, the temperature of carbonation stage is 1500 DEG C, and the temperature of nitridation stage is 1250 DEG C, and cooling stage is water cooling to being no more than 100 DEG C,
Calcination time is 6 hours, and the apparent density for finally obtaining VN alloy is 3.2g/cm3, it is through analysis product content of vanadium
77.50%, nitrogen content 16.2%, the quantity-produced daily output reaches 1800kg.
Comparative example 3
The difference of this comparative example 3 and embodiment 3 is that it is in normal temperature condition that the addition of compound, which is stirred process,
Lower progress；The moisture content of thick block is up to 5.04% or so after Ageing Treatment；It is 400 in the temperature of calcining kiln drying stage
DEG C, the temperature of carbonation stage is 1550 DEG C, and the temperature of nitridation stage is 1300 DEG C, and cooling stage is water cooling to being no more than 100 DEG C,
Calcination time is 6 hours, and the apparent density for finally obtaining VN alloy is 3.2g/cm3, it is through analysis product content of vanadium
77.35%, nitrogen content 16.0%, the quantity-produced daily output reaches 1300kg.
By contrasting secondary coarse material block of 1- of the embodiment of the present invention embodiments 3 after Ageing Treatment and comparative example 1- comparative examples
3 prepare knowable to the outward appearance and performance of the coarse fodder block after Ageing Treatment：1-3's of the embodiment of the present invention passes through at 2-3 hour timeliness
The intensity height of the secondary coarse material block of reason, smooth in appearance, product density height, water content are down to 2% or so；Reason is the inventive method
The mixing condition of vanadium-containing compound after activation process, reaction promoter, carbonaceous material and binding agent is designed as be in temperature
Be stirred to obtain compound under the conditions of 75 DEG C of -80 DEG C of vapours, reduce the time of follow-up Ageing Treatment, by it is original at least
It is reduced to 2-3 hours within 48 hours.
The density of the VN alloy of 1- of embodiment of the present invention embodiments 3 is 3.5g/cm3-3.9g/cm3, wherein v element contains
Measure as 77%-79%, nitrogen element content 15%-17%.
The process production efficiency of the present invention is higher, and the daily output may be up to more than 2t, and density is high, and vanadium, nitrogen content are higher,
Compared with Conventional processing methods, the process time is saved, improves product quality and production efficiency.
Disclosed above is only the embodiment of the present invention, but protection scope of the present invention is not limited thereto, and is appointed
What those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should using above-mentioned scope of the claims as
It is accurate.
Claims (7)
1. a kind of production method of VN alloy, including：Vanadium-containing compound is subjected to mechanical activation processing, reaction is added and promotes
Agent, carbonaceous material and binding agent obtain compound；Mechanical-moulded after the compound is placed 24 hours is a coarse fodder block, institute
State a coarse fodder block and carry out Ageing Treatment at normal temperatures and obtain secondary coarse material block；Secondary coarse material block the forging in High Purity Nitrogen atmosphere
Pass through baking stage, temperature rise period, carbonation stage, sintering stage and cooling stage in firing successively, cooling afterwards is come out of the stove, and is obtained
VN alloy finished product；Characterized in that, vanadium-containing compound, the reaction promoter, the carbon containing thing after the activation process
Matter and the binding agent are to be stirred to obtain the compound under the conditions of temperature is 75 DEG C of -80 DEG C of vapours；
The time of the Ageing Treatment is 2h-3h；
The temperature of the baking stage is 200 DEG C -250 DEG C, drying time 15h-17h；
The temperature of the temperature rise period is 500 DEG C -1000 DEG C, heating-up time 7.5h-8.5h；
The temperature of the carbonation stage is 1000 DEG C -1350 DEG C, carbonization time 4h-6h；
The temperature of the sintering stage is 1350 DEG C -1500 DEG C, sintering time 7h-9h；
The temperature of the cooling stage is 75 DEG C -80 DEG C.
2. the production method of a kind of VN alloy according to claim 1, it is characterised in that the mechanical activation, which is handled, is
Using Ginding process, milling time 1h；Particle diameter after the vanadium-containing compound grinding is -180 mesh.
A kind of 3. production method of VN alloy according to claim 1, it is characterised in that containing after the activation process
Vfanadium compound, the reaction promoter, the weight ratio of the carbonaceous material and the binding agent are 70-85: 3-5: 10-25:
0.1-10。
4. the production method of a kind of VN alloy according to claim 1, it is characterised in that the vanadium-containing compound is powder
At least one in shape vanadic anhydride, vanadium trioxide, vanadium tetraoxide, ammonium poly-vanadate, ammonium metavanadate, vanadium hydroxide and vanadic acid
Kind.The reaction promoter is ferrous carbonate powder, high-purity iron powder, melting vanadium pentoxide powder, vanadium trioxide powder, vanadium
Iron powder, VN alloy powder, vanadium carbide powder or metal vanadium powder；The carbonaceous material is Scaly graphite powder, noncrystalline stone
At least one of ink powder, carbon black powder, charcoal powder and graphite electrode carbon dust.The binding agent be water, polyvinyl alcohol, tapioca starch and
At least one of flour, and tapioca starch and flour are slurry.
5. the production method of a kind of VN alloy according to claim 1, it is characterised in that the high pure nitrogen is from institute
The various inlet mouth for stating calcining kiln is sent into；Pressure in the calcining kiln is 0.1kg/cm2-0.2kg/cm2；The calcining kiln
Heating means are resistance heating, heating plasma or high temperature nitrogen heating；The concentration of volume percent of the nitrogen is
99.999%.
6. a kind of VN alloy, it is characterised in that the VN alloy is prepared as the method described in claim any one of 1-5
Obtain.
7. a kind of VN alloy according to claim 1, it is characterised in that the density of the VN alloy is 3.5g/cm3-
3.9g/cm3, wherein vanadium unit cellulose content is 77%-79%, nitrogen element content 15%-17%.
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| CN113430402A (en) * | 2021-06-07 | 2021-09-24 | 湖南众鑫新材料科技股份有限公司 | Raw material forming method in vanadium-nitrogen alloy production process |
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