CN106119588A - Prepare the method and system of nitrogen-vanadium alloy - Google Patents
Prepare the method and system of nitrogen-vanadium alloy Download PDFInfo
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- CN106119588A CN106119588A CN201610627148.7A CN201610627148A CN106119588A CN 106119588 A CN106119588 A CN 106119588A CN 201610627148 A CN201610627148 A CN 201610627148A CN 106119588 A CN106119588 A CN 106119588A
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910000756 V alloy Inorganic materials 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 142
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 58
- 238000001816 cooling Methods 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 36
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 30
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 230000009467 reduction Effects 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 18
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 17
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 238000003763 carbonization Methods 0.000 claims description 30
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 claims description 26
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 25
- 238000007599 discharging Methods 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 238000005121 nitriding Methods 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000000498 cooling water Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 abstract description 9
- 239000010439 graphite Substances 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 238000010000 carbonizing Methods 0.000 abstract 4
- 238000006396 nitration reaction Methods 0.000 abstract 2
- 238000011946 reduction process Methods 0.000 abstract 2
- 239000004744 fabric Substances 0.000 abstract 1
- 229940056319 ferrosoferric oxide Drugs 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 36
- 238000006243 chemical reaction Methods 0.000 description 28
- 229910001199 N alloy Inorganic materials 0.000 description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 239000008188 pellet Substances 0.000 description 12
- 239000004484 Briquette Substances 0.000 description 10
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 229910052720 vanadium Inorganic materials 0.000 description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 6
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- MVXMNHYVCLMLDD-UHFFFAOYSA-N 4-methoxynaphthalene-1-carbaldehyde Chemical compound C1=CC=C2C(OC)=CC=C(C=O)C2=C1 MVXMNHYVCLMLDD-UHFFFAOYSA-N 0.000 description 1
- 229910000616 Ferromanganese Inorganic materials 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- -1 ferrovanadium nitride Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- IBYSTTGVDIFUAY-UHFFFAOYSA-N vanadium monoxide Chemical compound [V]=O IBYSTTGVDIFUAY-UHFFFAOYSA-N 0.000 description 1
- 125000005287 vanadyl group Chemical group 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Iron (AREA)
Abstract
The invention discloses the method and system preparing nitrogen-vanadium alloy.Wherein, the method preparing nitrogen-vanadium alloy includes: is shaped processing by Vanadium sesquioxide powder and powdered graphite and ferroferric oxide powder, obtains mixed material agglomerate；The feed zone that described mixed material agglomerate is delivered to rotary hearth furnace is carried out cloth, after described mixed material agglomerate sequentially passes through carbonizing reduction district, Nitration synthesis district and cooling zone, discharge through discharge zone, wherein, described mixed material agglomerate enters described carbonizing reduction district and carries out carbonizing reduction process, obtains vanadium carbide and carbon monoxide；Described vanadium carbide enters described Nitration synthesis district and carries out nitrogen treatment with nitrogen, obtains nitrogen-vanadium alloy；Described nitrogen-vanadium alloy enters described cooling zone and carries out cooling process, obtains the nitrogen-vanadium alloy of cooling.The method, with Vanadium sesquioxide as raw material, allocates graphite and ferroso-ferric oxide into, and in rotary hearth furnace, substep carries out carbonizing reduction process and nitrogen treatment, obtains the VN alloy that nitrogen content is high, impurity content is low.
Description
Technical Field
The invention relates to a method for preparing a nitrogen-vanadium alloy and a system for preparing the nitrogen-vanadium alloy.
Background
The nitrided ferrovanadium is a new typeThe vanadium-nitrogen alloy additive has performance superior to that of ferrovanadium and vanadium nitride, and can be widely applied to products such as high-strength screw steel bars, high-strength pipeline steel, high-strength section steel (H-shaped steel, I-shaped steel, channel steel and angle steel), thin slab continuous casting and rolling high-strength steel strips, non-quenched and tempered steel, high-speed tool steel and the like. The specific gravity of the ferrovanadium nitride can reach 5.0g/cm3Compared with the addition of vanadium nitride (the specific gravity is about 3.5), the vanadium nitride alloy has higher absorption rate, the recovery rate of vanadium iron nitride can reach more than 95%, the average absorption rate is higher than that of vanadium-nitrogen alloy by 3-5%, the performance is more stable, and the vanadium nitride alloy has higher refined crystal grains, improved strength, toughness, ductility and the like.
The nitrogen increasing method in steel generally comprises the following steps: (1) adding nitrogen-rich ferromanganese; (2) adding calcium cyanamide; (3) nitrogen purging, but these methods all have disadvantages: method (1) is expensive; method (2) is low and unstable in yield; the method (3) requires a special apparatus for nitrogen blowing.
Thus, the method for preparing the nitrogen vanadium alloy needs to be improved.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, one purpose of the invention is to provide a method for preparing a nitrogen-vanadium alloy, which takes vanadium trioxide as a raw material, adds graphite and ferroferric oxide, and carries out carbonization-reduction treatment and nitridation treatment in a rotary hearth furnace in a stepwise manner to obtain the vanadium-nitrogen alloy with high nitrogen content and low impurity content.
Thus, according to one aspect of the invention, there is provided a method of making a vanadyl alloy. According to an embodiment of the invention, the method comprises: forming vanadium trioxide powder, graphite powder and ferroferric oxide powder to obtain mixed material lumps; conveying the mixed material blocks to a feeding area of a rotary hearth furnace for distributing, wherein the mixed material blocks sequentially pass through a carbonization-reduction area, a nitridation synthesis area and a cooling area and then are discharged through a discharging area, and the mixed material blocks enter the carbonization-reduction area for carbonization-reduction treatment so as to obtain vanadium carbide and carbon monoxide; the vanadium carbide enters the nitriding synthesis area to be nitrided with nitrogen so as to obtain a vanadium nitride alloy; and the nitrogen vanadium alloy enters the cooling zone to be cooled so as to obtain a cooled nitrogen vanadium alloy.
According to the method for preparing the nitrogen-vanadium alloy, vanadium trioxide is used as a raw material, graphite and ferroferric oxide are added, wherein the ferroferric oxide is used as a catalyst for a nitridation reaction, so that the reaction activity of the material is improved, the activation energy is reduced, and meanwhile, iron elements in the ferroferric oxide can form a vanadium-iron alloy and FeN with vanadium and nitrogen in the nitridation treatment process, so that the nitrogen content in the nitrogen-vanadium alloy is obviously improved. Simultaneously, set up feeding zone, carbonization reduction district, nitrogenize synthetic district, cooling zone and ejection of compact district in the rotary hearth furnace, the material that makes preparation nitrogen vanadium alloy carries out the carbonization reduction treatment step by step and nitrogenize the processing, the nitrogen gas of avoiding nitrogenize synthetic district gets into the carbonization reaction district and makes the CO concentration in carbonization reaction district improve, reducing atmosphere strengthens, thereby it is higher to make carbonization reaction efficiency, raw materials carbonization rate is showing and is improving, still effectively reduce the oxygen content in the pelletizing simultaneously, and then, obtain the vanadium nitrogen alloy that nitrogen content is high, oxygen content is low, the impurity is few. In addition, the method has low production cost, simple method and easy operation.
In addition, the method for preparing the vanadium nitride alloy according to the above embodiment of the invention may further have the following additional technical features:
according to the embodiment of the invention, the mass ratio of the vanadium trioxide powder to the graphite powder to the ferroferric oxide powder is 100: (48-52): (1-3) carrying out the molding treatment.
According to an embodiment of the present invention, the purity of the vanadium trioxide powder is not less than 98%.
According to the embodiment of the invention, the particle sizes of the vanadium trioxide powder and the graphite powder are not more than 200 meshes, and the average particle size of the ferroferric oxide powder is not more than 20 micrometers.
According to the embodiment of the invention, the temperature of the carbonization-reduction treatment is 1180-1250 ℃ and the time is 0.5-1 hour.
According to the embodiment of the invention, the temperature of the nitriding treatment is 1250-1380 ℃, the time is 1-1.5 hours, and the ratio of the nitrogen partial pressure to the oxygen partial pressure is not lower than 33.
According to another aspect of the invention, the invention provides a system for implementing the method for preparing the nitrogen vanadium alloy. According to an embodiment of the invention, the system comprises: the molding device is provided with a vanadium trioxide powder inlet, a graphite powder inlet, a ferroferric oxide powder inlet and a mixed material block mass outlet; the rotary hearth furnace is sequentially provided with a feeding area, a carbonization-reduction area, a nitrification synthesis area, a cooling area and a discharging area along the moving direction of raw materials, wherein the feeding area is provided with a mixed material briquette inlet which is connected with a mixed material briquette outlet; the carbonization reduction zone has a carbon monoxide outlet; the nitrification synthesis zone has a nitrogen gas inlet; the discharge area is provided with a nitrogen vanadium alloy outlet.
According to the system for preparing the nitrogen-vanadium alloy, the forming device is provided with the vanadium trioxide powder inlet, the graphite powder inlet and the ferroferric oxide powder inlet, vanadium trioxide is used as a raw material, graphite and ferroferric oxide are added, wherein the ferroferric oxide is used as a catalyst for a nitridation reaction, so that the reaction activity of the material is improved, the activation energy is reduced, and meanwhile, iron elements in the ferroferric oxide can form a vanadium-iron alloy and FeN together with vanadium and nitrogen in the nitridation treatment process, so that the nitrogen content in the nitrogen-vanadium alloy is obviously improved. The carbonization-reduction zone and the nitridation synthesis zone are arranged in the rotary hearth furnace, so that raw materials are subjected to carbonization-reduction treatment and nitridation treatment step by step, nitrogen in the nitridation synthesis zone is prevented from entering the carbonization reaction zone, the CO concentration in the carbonization reaction zone is improved, the reducing atmosphere is enhanced, the carbonization treatment efficiency is higher, the raw material carbonization rate is obviously improved, the oxygen content in the pellets is effectively reduced, and further the vanadium-nitrogen alloy with high nitrogen content, low oxygen content and less impurities is obtained. Moreover, the system has simple structure and easy operation.
According to an embodiment of the invention, the rotary hearth furnace further comprises: the first retaining wall is arranged between the carbonization and reduction area and the nitrification synthesis area; a second retaining wall disposed between the nitrification synthesis zone and the cooling zone; and the third retaining wall is arranged between the cooling zone and the discharging zone.
According to an embodiment of the invention, the rotary hearth furnace further comprises: the first nitrogen through hole is arranged on the second baffle wall; and the second nitrogen through hole is arranged on the third baffle wall.
According to an embodiment of the invention, the rotary hearth furnace further comprises: a waterwall disposed on a sidewall of the cooling zone.
According to an embodiment of the invention, the rotary hearth furnace further comprises: and the heat accumulating type burner is arranged in the carbonization and reduction area and the nitrification synthesis area.
According to an embodiment of the invention, the rotary hearth furnace further comprises: and the carbon monoxide conveying channel is respectively connected with the carbon monoxide outlet of the carbonization reduction zone and the air inlet of the heat accumulating type burner.
According to an embodiment of the invention, the rotary hearth furnace further comprises: spiral discharger, spiral discharger sets up the ejection of compact district the nitrogen vanadium alloy exit, spiral discharger includes: a spiral shaft body; and the helical blade is spirally arranged on the helical shaft body.
According to an embodiment of the invention, the screw discharger further comprises: the cooling water channel is arranged inside the spiral discharging device and is arranged along the axial direction of the spiral discharging device; and the nitrogen channel is arranged on the outer side of the cooling water channel, and is axially wrapped by the cooling water channel and provided with a nitrogen inlet and a nitrogen outlet.
According to an embodiment of the present invention, the nitrogen inlet is provided at an end of the spiral shaft body, and the nitrogen outlet is provided on the spiral blade.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
figure 1 shows a schematic flow diagram of a method of making a nitrogen vanadium alloy according to one embodiment of the invention;
FIG. 2 shows a schematic structural diagram of a system for preparing a nitrogen vanadium alloy according to one embodiment of the invention;
FIG. 3 shows a schematic structural view of a rotary hearth furnace according to an embodiment of the present invention;
FIG. 4 shows a schematic view of a screw discharger according to an embodiment of the invention;
FIG. 5 shows a schematic structural view of a cross section of a spiral discharger according to an embodiment of the invention;
FIG. 6 is a partial schematic structural view showing a rotary hearth furnace according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are for convenience of description of the present invention only and do not require that the present invention must be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
It should be noted that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Further, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
Method for preparing nitrogen vanadium alloy
According to one aspect of the invention, the invention provides a method of making a nitrogen vanadium alloy. Referring to fig. 1, a method of preparing a nitrogen vanadium alloy is illustrated according to an embodiment of the present invention, the method including:
s100 Molding Process
According to the embodiment of the invention, vanadium trioxide powder, graphite powder and ferroferric oxide powder are subjected to molding treatment to obtain the mixed material block mass. The ferroferric oxide is used as a catalyst of a nitriding reaction, so that the reaction activity of materials is improved, the activation energy is reduced, and meanwhile, in the nitriding treatment process, iron elements in the ferroferric oxide can form a ferrovanadium alloy and FeN with vanadium and nitrogen, so that the nitrogen content in the ferronitrogen alloy is obviously improved.
According to some embodiments of the present invention, the vanadium trioxide powder is mixed with the graphite powder and the ferroferric oxide powder in a mass ratio of 100: (48-52): (1-3) carrying out the molding treatment. Therefore, the graphite has high reduction efficiency and high reduction rate of vanadium trioxide, effectively avoids a large amount of raw materials from remaining, and is favorable for reducing the impurity content of the nitrogen-vanadium alloy. If the proportion of graphite powder is too high, easily lead to the carbon content in the final product vanadium nitride alloy high, influence vanadium nitride alloy's quality, if the proportion of graphite powder is too low, the carbonization reaction can not thoroughly react, and the product recovery rate is low. And the ferroferric oxide is used as a catalyst, so that the catalytic effect cannot be correspondingly improved by adding too much catalyst, but the cost is increased.
According to a particular embodiment of the invention, the purity of the vanadium trioxide powder is not less than 98%. Therefore, the vanadium trioxide powder has high purity and few impurities, and is beneficial to reducing the impurity content of the vanadium-nitrogen alloy and improving the yield of the nitrogen-vanadium alloy.
According to some embodiments of the present invention, the vanadium trioxide powder and the graphite powder have a particle size of no more than 200 meshes, and the ferroferric oxide powder has an average particle size of no more than 20 microns. The inventor has found through a great deal of research that when the average particle size of the reaction raw materials is small, the specific surface area of the raw materials is high, the contact area of the two raw materials is large, the mass transfer efficiency and the heat transfer efficiency of the raw materials are high, and the reaction rate is high. When the raw materials are in the particle size range, the reaction activity of the raw materials is high, the reaction temperature is low, and the reaction time is short.
S200 reduction nitridation treatment
According to the embodiment of the invention, the mixed material block mass is conveyed to a feeding area of the rotary hearth furnace for distributing, the mixed material block mass sequentially passes through a carbonization-reduction area, a nitridation synthesis area and a cooling area and then is discharged through a discharging area, wherein the mixed material block mass enters the carbonization-reduction area for carbonization-reduction treatment to obtain vanadium carbide and carbon monoxide; allowing vanadium carbide to enter a nitriding synthesis area and carrying out nitriding treatment on the vanadium carbide and nitrogen to obtain a vanadium-nitrogen alloy; and the nitrogen vanadium alloy enters a cooling zone for cooling treatment to obtain the cooled nitrogen vanadium alloy. And carrying out carbonization-reduction treatment and nitridation treatment in a rotary hearth furnace in a stepwise manner to obtain the vanadium-nitrogen alloy with high nitrogen content and low impurity content. The carbonization-reduction treatment and the nitridation treatment are carried out separately, nitrogen in a nitridation synthesis area is prevented from entering a carbonization reaction area, so that the CO concentration in the carbonization reaction area is improved, the reducing atmosphere is enhanced, the carbonization reaction efficiency is higher, the raw material carbonization rate is obviously improved, the oxygen content in the pellets is effectively reduced, and then the vanadium-nitrogen alloy with high nitrogen content, low oxygen content and less impurities is obtained. According to the embodiment of the present invention, the temperature of the carbonization-reduction treatment is 1180-1250 ℃ for 0.5-1 hour. Therefore, the carbonization-reduction efficiency is high, the effect is good, and the vanadium trioxide is ensured to be fully nitrided to generate vanadium carbide.
According to the embodiment of the present invention, the temperature of the nitriding treatment is 1250-1380 ℃ for 1-1.5 hours, and the ratio of the nitrogen partial pressure to the oxygen partial pressure is not lower than 33. From this, the efficient of nitridation to be favorable to the carborundum fully to nitrify, and the ratio of nitrogen partial pressure and oxygen partial pressure is not less than 33, make the nitrogen vanadium alloy of formation handle under the environment of high nitrogen content, avoid nitrogen vanadium alloy to be oxidized in the cooling process effectively, make the purity of nitrogen vanadium alloy higher.
System for preparation nitrogen vanadium alloy
According to another aspect of the invention, the invention provides a system for implementing the method for preparing the nitrogen vanadium alloy. Referring to fig. 2, according to an embodiment of the present invention, the system includes: a forming apparatus 100 and a rotary hearth furnace 200.
According to the embodiment of the invention, the forming device 100 is provided with a vanadium trioxide powder inlet 101, a graphite powder inlet 102, a ferroferric oxide powder inlet 103 and a mixed material briquette outlet 104, and the forming device 100 is used for forming the vanadium trioxide powder, the graphite powder and the ferroferric oxide powder to obtain the mixed material briquette. The ferroferric oxide is used as a catalyst of a nitriding reaction, so that the reaction activity of materials is improved, the activation energy is reduced, and meanwhile, in the nitriding treatment process, iron elements in the ferroferric oxide can form a ferrovanadium alloy and FeN with vanadium and nitrogen, so that the nitrogen content in the ferronitrogen alloy is obviously improved.
Referring to fig. 3, according to an embodiment of the present invention, a feeding region 210, a carbonization-reduction region 220, a nitrogen synthesis region 230, a cooling region 240, and a discharging region 250 are sequentially disposed in a rotary hearth furnace 200 along a direction of movement of a raw material, wherein the feeding region 210 has a mixed material briquette inlet 201, the mixed material briquette inlet 201 is connected to a mixed material briquette outlet 104, a mixed material briquette enters the rotary hearth furnace from the mixed material briquette inlet 201 of the feeding region 210, the carbonization-reduction region 220 has a carbon monoxide outlet 203, vanadium trioxide in the mixed material briquette undergoes a reduction reaction with graphite at a high temperature, the vanadium trioxide is first reduced into vanadium monoxide, and then vanadium carbide is generated, and carbon monoxide is discharged from the carbon monoxide outlet 203; the nitriding synthesis area 230 is provided with a nitrogen inlet 202, and vanadium carbide is subjected to nitriding treatment under a nitrogen environment and a high-temperature condition to generate a vanadium-nitrogen alloy; the discharging area 150 is provided with a nitrogen vanadium alloy outlet 204, and the nitrogen vanadium alloy is discharged from the nitrogen vanadium alloy outlet 204.
According to the embodiment of the invention, the temperature of the rotary hearth furnace for carrying out the carbonization-reduction treatment is 1180-1250 ℃, and the time is 0.5-1 hour. Therefore, the carbonization-reduction efficiency is high, the effect is good, and vanadium trioxide is fully vanadium carbide.
According to the embodiment of the invention, the temperature of the nitriding treatment in the rotary hearth furnace is 1250-1380 ℃, the time is 1-1.5 hours, and the ratio of the nitrogen partial pressure to the oxygen partial pressure is not lower than 33. From this, the efficient of nitridation to be favorable to the carborundum fully to nitrify, and the ratio of nitrogen partial pressure and oxygen partial pressure is not less than 33, make the nitrogen vanadium alloy of formation handle under the environment of high nitrogen content, avoid nitrogen vanadium alloy to be oxidized in the cooling process effectively, make the purity of nitrogen vanadium alloy higher.
According to some embodiments of the invention, the rotary hearth furnace 200 further comprises: a first retaining wall 260, a second retaining wall 270, and a third retaining wall 280, wherein the first retaining wall 260 is disposed between the carbide reduction zone 220 and the nitride synthesis zone 230; the second barrier 270 is disposed between the nitride synthesis region 230 and the cooling region 240; a third dam 280 is disposed between the cooling zone 240 and the discharge zone 250. Therefore, the retaining wall is utilized to effectively separate the carbonization reduction zone, the nitridation synthesis zone and the cooling zone, and mutual influence among the zones is avoided.
According to an embodiment of the present invention, the rotary hearth furnace 200 further includes: first nitrogen gas through-hole 205 and second nitrogen gas through-hole 206, wherein, first nitrogen gas through-hole 205 sets up on second barricade 270 for nitrogen gas is carried in the nitrogenization synthesis district, and second nitrogen gas through-hole 206 sets up on third barricade 280 for discharge nitrogen gas to the ejection of compact district, avoid the nitrogen vanadium alloy to be oxidized in ejection of compact process. The first nitrogen gas through hole 205 and the second nitrogen gas through hole 206 may be one or more according to the amount of nitrogen gas required for actual production.
Referring to fig. 6, according to some embodiments of the invention, the rotary hearth furnace 200 further includes: and a second nitrogen gas inlet 205, the second nitrogen gas inlet 205 being provided on the entire top wall of the rotary hearth furnace, for supplying sufficient nitrogen gas to the rotary hearth furnace so that the reaction space of the rotary hearth furnace is in a nitrogen atmosphere.
According to an embodiment of the invention, the rotary hearth furnace further comprises: and the water cooling wall is arranged on the side wall of the cooling area. From this, carry out cooling treatment to the nitrogen vanadium alloy who generates fast through the water-cooling wall, the cooling effect is good, and is fast.
According to an embodiment of the invention, the rotary hearth furnace further comprises: and the heat accumulating type burner is arranged in the carbonization-reduction area and the nitridation synthesis area, is used for heating the carbonization-reduction area and the nitridation synthesis area, and provides a high-temperature environment for carbonization-reduction treatment and nitridation treatment.
According to an embodiment of the invention, the system further comprises: and the carbon monoxide conveying channel is respectively connected with a carbon monoxide outlet of the carbonization reduction zone and an air inlet of the heat accumulating type burner, and is used for conveying the carbon monoxide generated by the carbonization reduction reaction to the heat accumulating type burner as a fuel of the heat accumulating type burner, so that comprehensive high-efficiency utilization of energy is realized, the production cost is lower, and the pollution of the carbon monoxide to the environment is also avoided.
According to an embodiment of the invention, the rotary hearth furnace further comprises: a spiral discharger 290 disposed at the nitrogen vanadium alloy outlet of the discharge zone, as shown in fig. 4, the spiral discharger 290 comprising: a spiral shaft body 291 and a spiral blade 292, the spiral blade 292 is spirally arranged on the spiral shaft body 291, and the spiral discharger 290 is used for discharging the product.
Referring to fig. 5, according to an embodiment of the present invention, the screw discharger further includes: a cooling water passage 293 and a nitrogen gas passage 294, wherein the cooling water passage 293 is disposed inside the spiral discharger 290 and is disposed along an axial direction of the spiral discharger; and a nitrogen gas channel 294 is provided outside the cooling water channel 293, and the nitrogen gas channel 294 axially surrounds the cooling water channel 293, the nitrogen gas channel 294 having a nitrogen gas inlet 296 and a nitrogen gas outlet 295. The produced nitrogen vanadium alloy is subjected to water cooling and air cooling through the cooling water channel 293 and the nitrogen channel 294, so that the rapid cooling of the nitrogen vanadium alloy is facilitated. According to some embodiments of the present invention, the nitrogen gas in the nitrogen channel may be provided by the nitrogen gas from the cooling zone 240, and the nitrogen gas forms a protective atmosphere in the discharging zone 250, preventing re-oxidation of the nitrogen vanadium alloy, and cooling the pellets to below 200 ℃.
Referring to fig. 4 and 5, according to the embodiment of the present invention, the nitrogen gas inlet is provided at an end of the spiral shaft body 291, that is, at one end of the spiral shaft body 291, or at both ends of the spiral shaft body 291, thereby making a flow path of the nitrogen gas through the spiral shaft body longer and more effectively cooling the nitv.
According to some embodiments of the present invention, the nitrogen outlet is provided on the helical blade 292. Thereby make the nitrogen vanadium alloy also cool down through the in-process that the spiral discharger was discharged, the in-process that contacts with the blade, make the cooling effect of nitrogen vanadium alloy better.
The present invention is described below with reference to specific examples, which are intended to be illustrative only and are not to be construed as limiting the invention.
Example 1
The method for preparing the nitrogen vanadium alloy comprises the following specific steps:
(1) will V2O3Graphite powder and Fe3O4And water according to a mass ratio of 100: 48: 1: 8, mixing materials and pressing the pellets to obtain the pellets.
(2) And drying the pellets to obtain dried pellets.
(3) And (2) distributing the dried pellets into a rotary hearth furnace, setting the temperature of a carbonization reaction zone of the rotary hearth furnace to 1200 ℃, setting the reaction time to 0.8h, setting the temperature of a nitridation reaction zone to 1300 ℃, setting the nitridation reaction time to 1.5 h, after the nitridation reaction is finished, cooling the vanadium-nitrogen alloy in a cooling zone and a discharging zone to below 200 ℃ and discharging the vanadium-nitrogen alloy out of the furnace to obtain the vanadium-nitrogen alloy, wherein the vanadium-nitrogen alloy has the N content of 14%, the V content of 73% and the O content of only 1.5%, the nitrogen and vanadium content of the vanadium-nitrogen alloy is high, the oxygen content is low and the quality is excellent.
Example 2
The method for preparing the nitrogen vanadium alloy comprises the following specific steps:
(1) will V2O3Graphite powder and additive Fe3O4And water according to a mass ratio of 100: 52: 3: 10, mixing and pelletizing to obtain the pellets.
(2) And drying the pellets to obtain dried pellets.
(3) And (2) distributing the dried pellets into a rotary hearth furnace, setting the temperature of a carbonization reaction zone of the rotary hearth furnace to 1250 ℃, setting the reaction time to 1h, setting the temperature of a nitridation reaction zone to 1350 ℃, setting the nitridation reaction time to 2 h, finishing the nitridation reaction, cooling the vanadium-nitrogen alloy into a cooling zone and a discharging zone to below 200 ℃, and discharging to obtain the vanadium-nitrogen alloy, wherein the N content of the vanadium-nitrogen alloy is 15.5%, the V content is 76%, the O content is only 1%, the nitrogen and vanadium content of the vanadium-nitrogen alloy are high, the oxygen content is low, and the quality is excellent.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A method of making a nitrogen vanadium alloy, comprising:
forming vanadium trioxide powder, graphite powder and ferroferric oxide powder to obtain mixed material lumps;
the mixed material blocks are conveyed to a feeding area of a rotary hearth furnace for distributing, the mixed material blocks sequentially pass through a carbonization-reduction area, a nitridation synthesis area and a cooling area and then are discharged through a discharging area, wherein,
the mixed material lumps enter the carbonization and reduction area for carbonization and reduction treatment so as to obtain vanadium carbide and carbon monoxide;
the vanadium carbide enters the nitriding synthesis area to be nitrided with nitrogen so as to obtain a vanadium nitride alloy; and
and the nitrogen vanadium alloy enters the cooling zone to be cooled so as to obtain a cooled nitrogen vanadium alloy.
2. The method according to claim 1, wherein the vanadium trioxide powder is mixed with the graphite powder and the ferroferric oxide powder in a mass ratio of 100: (48-52): (1-3) carrying out the molding treatment.
3. The method according to claim 1 or 2, wherein the purity of the vanadium trioxide powder is not less than 98%.
4. The method according to any one of claims 1 to 3, wherein the vanadium trioxide powder and the graphite powder have a particle size of no more than 200 meshes, and the ferroferric oxide powder has an average particle size of no more than 20 microns.
5. The method as claimed in any one of claims 1 to 4, wherein the temperature of the carbonization-reduction treatment is 1180-1250 ℃ for 0.5 to 1 hour.
6. The method as claimed in any one of claims 1 to 5, wherein the nitriding treatment is carried out at 1250-1380 ℃ for 1 to 1.5 hours and at a ratio of the nitrogen partial pressure to the oxygen partial pressure of not less than 33.
7. A system for implementing the method for preparing the nitrogen vanadium alloy according to any one of claims 1 to 6, which is characterized by comprising the following steps:
the molding device is provided with a vanadium trioxide powder inlet, a graphite powder inlet, a ferroferric oxide powder inlet and a mixed material block mass outlet;
a rotary hearth furnace, wherein the rotary hearth furnace is sequentially provided with a feeding area, a carbonization-reduction area, a nitrification-synthesis area, a cooling area and a discharging area along the moving direction of raw materials,
wherein,
the feeding area is provided with a mixed material block mass inlet which is connected with the mixed material block mass outlet;
the carbonization reduction zone has a carbon monoxide outlet;
the nitrification synthesis zone has a nitrogen gas inlet;
the discharge area is provided with a nitrogen vanadium alloy outlet.
8. The system of claim 7, wherein the rotary hearth furnace further comprises:
the first retaining wall is arranged between the carbonization and reduction area and the nitrification synthesis area;
a second retaining wall disposed between the nitrification synthesis zone and the cooling zone;
a third retaining wall arranged between the cooling zone and the discharge zone,
optionally, the rotary hearth furnace further comprises:
the first nitrogen through hole is arranged on the second baffle wall;
a second nitrogen through hole provided on the third baffle wall,
optionally, the rotary hearth furnace further comprises:
a waterwall disposed on a sidewall of the cooling zone.
9. The system of claim 7 or 8, wherein the rotary hearth furnace further comprises:
the heat accumulating type burner is arranged in the carbonization and reduction area and the nitrification and synthesis area,
optionally, the rotary hearth furnace further comprises:
and the carbon monoxide conveying channel is respectively connected with the carbon monoxide outlet of the carbonization reduction zone and the air inlet of the heat accumulating type burner.
10. The system of any one of claims 7-9, wherein the rotary hearth furnace further comprises:
spiral discharger, spiral discharger sets up the ejection of compact district the nitrogen vanadium alloy exit, spiral discharger includes:
a spiral shaft body; and
a helical blade spirally arranged on the helical shaft body,
optionally, the screw discharger further comprises:
the cooling water channel is arranged inside the spiral discharging device and is arranged along the axial direction of the spiral discharging device; and
the nitrogen channel is arranged on the outer side of the cooling water channel, the cooling water channel is axially wrapped by the nitrogen channel, the nitrogen channel is provided with a nitrogen inlet and a nitrogen outlet,
optionally, the nitrogen inlet is provided at an end of the spiral shaft body and the nitrogen outlet is provided on the spiral blade.
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