CN113736987A - Preparation method of nitrided ferrovanadium alloy - Google Patents
Preparation method of nitrided ferrovanadium alloy Download PDFInfo
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- CN113736987A CN113736987A CN202110882973.2A CN202110882973A CN113736987A CN 113736987 A CN113736987 A CN 113736987A CN 202110882973 A CN202110882973 A CN 202110882973A CN 113736987 A CN113736987 A CN 113736987A
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- 229910000628 Ferrovanadium Inorganic materials 0.000 title claims abstract description 54
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 48
- 239000000956 alloy Substances 0.000 title claims abstract description 48
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 71
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000010438 heat treatment Methods 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 39
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 38
- 239000010439 graphite Substances 0.000 claims abstract description 38
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 43
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 20
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000002910 solid waste Substances 0.000 abstract description 8
- 229910001021 Ferroalloy Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910052720 vanadium Inorganic materials 0.000 description 15
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 15
- 238000001914 filtration Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 7
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 6
- -1 ferrovanadium nitride Chemical class 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005121 nitriding Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910000742 Microalloyed steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/006—Making ferrous alloys compositions used for making ferrous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the technical field of ferroalloy, in particular to a preparation method of nitrided ferrovanadium alloy, which comprises the following steps: washing ferric vanadate mud with hot water at the temperature of 60-80 ℃, and drying to obtain dry-based ferric vanadate; adding vanadium oxide and graphite carbon powder with the granularity of 0.05-0.15 mm into the dry-based ferric vanadate, uniformly mixing, adding water, uniformly mixing, performing and pressing, and drying to obtain a performing material; and thirdly, sequentially carrying out low-temperature heat treatment at 300-400 ℃, medium-temperature heat treatment at 450-950 ℃ and high-temperature heat treatment at 1050-1650 ℃ on the preformed material, and cooling after the heat treatment is finished to obtain the azotized ferrovanadium alloy. The method provided by the invention is simple to operate, the iron vanadate mud subjected to impurity removal is used as a raw material, the high-efficiency utilization of solid wastes is realized, the content of impurities in the iron vanadate mud is reduced, the production cost of the nitrided ferrovanadium alloy is also reduced, and the nitrided ferrovanadium alloy with low cost, low impurities and high nitrogen content can be obtained by the preparation method provided by the invention.
Description
Technical Field
The invention relates to the technical field of ferroalloy, in particular to a preparation method of nitrided ferrovanadium alloy.
Background
Vanadium nitride is used as an important alloy additive of high-strength microalloyed steel, and the addition of ferrovanadium nitride to steel can improve the strength, toughness, wear resistance, corrosion resistance and thermal fatigue resistance of the steel and enable the steel to have excellent weldability. At present, the main methods for producing nitrided ferrovanadium are a solid nitriding method and a liquid nitriding method. Both the two methods use ferrovanadium as raw materials, and simultaneously, a plurality of vanadium-containing oxides and auxiliary materials are selected and introduced with nitrogen gas at certain temperature and pressure for nitriding reaction, but the preparation method of ferrovanadium nitride in the prior art has high raw material cost, complex production process, long reaction time and large energy consumption, and the prepared ferrovanadium nitride has low nitrogen content.
A large amount of vanadium-containing waste materials are generated in the process of producing ammonium vanadate by vanadium precipitation, and the main components of the vanadium-containing waste materials are water and ferric vanadate mud. The ferric vanadate mud is used as a raw material to prepare the ferrovanadium nitride, so that the raw material cost can be reduced, but the phase of the ferric vanadate mud composition is complex, the impurity content is high, and the quality of a final product can be influenced by directly using the ferric vanadate mud as a raw material to prepare the ferrovanadium nitride. And because the ferric vanadate mud has high moisture content, the problem that the materials are not easy to mix uniformly in the mixing process also exists.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a preparation method of nitrided ferrovanadium alloy, which takes the iron vanadate mud subjected to impurity removal as a raw material, realizes the efficient utilization of solid wastes, reduces the content of impurities in the iron vanadate mud, greatly reduces the production cost of nitrided ferrovanadium alloy, can prepare nitrided ferrovanadium alloy with low cost, low impurities and high nitrogen content by the preparation method, and overcomes the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the embodiment of the invention provides a preparation method of a nitrided ferrovanadium alloy, which comprises the following steps:
washing ferric vanadate mud with hot water at the temperature of 60-80 ℃, and drying to obtain dry-based ferric vanadate;
adding vanadium oxide and graphite carbon powder with the granularity of 0.05-0.15 mm into the dry-based ferric vanadate, uniformly mixing, adding water, uniformly mixing, performing and pressing, and drying to obtain a performing material;
and thirdly, sequentially carrying out low-temperature heat treatment at 300-400 ℃, medium-temperature heat treatment at 450-950 ℃ and high-temperature heat treatment at 1050-1650 ℃ on the preformed material, and cooling after the heat treatment is finished to obtain the azotized ferrovanadium alloy.
The preparation method of the nitrided ferrovanadium alloy provided by the invention takes the ferric vanadate mud as a raw material, so that the high-efficiency utilization of solid wastes can be realized, and the production cost of the nitrided ferrovanadium alloy can be greatly reduced. According to the preparation method, firstly, the ferric vanadate mud is added into hot water for washing, so that the content of soluble impurities in the ferric vanadate mud can be reduced, then the dry-base ferric vanadate subjected to impurity removal is mixed with vanadium oxide and graphite carbon powder, and various materials can be uniformly mixed in the mixing process by controlling the particle sizes of the vanadium oxide and the graphite carbon powder. Finally, the materials can be accurately controlled to sequentially complete dehydration in a low-temperature heat treatment stage, reduction in a medium-temperature heat treatment stage and nitridation in a high-temperature heat treatment stage by carrying out heat treatment at different temperatures in stages, and each heat treatment stage can shorten the time consumption of the whole preparation period and reduce the energy consumption by controlling the time. The nitrogen content of the vanadium nitride ferroalloy prepared by the preparation method is 20-25%, the vanadium content is 45-55%, and the impurity content of the vanadium nitride ferroalloy is respectively as follows: si is less than or equal to 2.5 percent; s is less than or equal to 0.05 percent; p is less than or equal to 0.07 percent; al is less than or equal to 2.0 percent.
The iron vanadate mud can be iron vanadate mud in vanadium-containing solid waste recovered by adopting vanadium precipitation to produce ammonium vanadate, the wet-based iron vanadate mud in the vanadium-containing solid waste has the water content of 45-55%, the vanadium oxide content of 22-30%, the iron content of 20-25%, the Si content of 0.15-0.25%, the S content of 2-3%, the P content of 0.01-0.02%, the Al content of 0.05-0.15%, and the impurity content of the wet-based iron vanadate mud is increased after being dried.
Preferably, in the first step, the mass ratio of the ferric vanadate mud to the hot water is 1: 1-2, repeatedly washing with hot water for 3-5 times, wherein the drying temperature is 80-90 ℃, and the drying time is 3-5 h. After each washing, the material after washing can be separated from water by adopting a suction filtration mode.
In the process of carrying out washing and impurity removal on the ferric vanadate mud for many times, adopted washing water can be recycled, and no secondary solid waste and waste liquid are generated in the whole process. The ferric vanadate mud with high water content is dried into dry-based ferric vanadate after impurity removal, so that the materials in the subsequent steps can be fully mixed.
Preferably, in the second step, the mass ratio of the dry-based ferric vanadate to the vanadium oxide to the graphite carbon powder is 1-3: 6: 1-2.
According to the method, the solid waste ferric vanadate mud is washed by hot water and then is used as a main vanadium-containing raw material to produce the ferrovanadium nitride alloy, and ferric vanadate is used for replacing part of vanadium oxide.
Preferably, in the second step, the purity of the vanadium oxide is more than 98.5%, the granularity of the vanadium oxide is 0.05-0.10 mm, the purity of the graphite carbon powder is more than 99.0%, the granularity of the graphite carbon powder is 0.05-0.10 mm, and the mass of the water is 10-20% of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder.
The quality of the prepared vanadium nitride ferrovanadium alloy can be improved by controlling the purity of vanadium oxide and graphite carbon powder, and the granularity of the vanadium oxide and the graphite carbon powder is basically consistent with that of dry-based ferric vanadate by controlling the granularity of the vanadium oxide and the graphite carbon powder, so that uniform material mixing is facilitated.
Preferably, in the second step, the mass of the water is 13-16% of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder.
Preferably, in the second step, the pressure of the preforming pressing is 20-30 Mpa.
Preferably, in the second step, the drying temperature is 80-90 ℃, and the drying time is 4-6 h.
The drying process in the second step is a dehydration drying process and a preheating process, and the temperature rise time from the subsequent temperature rise to the low-temperature heat treatment temperature can be shortened through the preheating of the second step.
Preferably, in the third step, the heating time of the low-temperature heat treatment is 3-5 hours, the heating time of the medium-temperature heat treatment is 4-8 hours, and the heating time of the high-temperature heat treatment is 6-40 hours.
By adopting the time of each heat treatment stage, the processes of dehydration of the material in the low-temperature heat treatment stage, reduction in the medium-temperature heat treatment stage and nitridation in the high-temperature heat treatment stage can be accurately controlled, so that the time consumption of the whole preparation period is shortened, and the energy consumption is reduced.
Preferably, in the third step, the temperature of the low-temperature heat treatment is 300-350 ℃, the temperature of the medium-temperature heat treatment is 800-900 ℃, and the temperature of the high-temperature heat treatment is 1400-1600 ℃.
The preparation method of the nitrided ferrovanadium alloy provided by the invention takes the iron vanadate mud subjected to impurity removal as a raw material, so that the high-efficiency utilization of solid wastes is realized. The detection shows that the nitrogen content of the vanadium nitride ferroalloy prepared by the preparation method is 20-25 percent, the vanadium content is 45-55 percent, and the impurity content of the vanadium nitride ferroalloy is respectively as follows: si is less than or equal to 2.5 percent; s is less than or equal to 0.05 percent; p is less than or equal to 0.07 percent; al is less than or equal to 2.0 percent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The pusher kiln of the following embodiments is provided with a low temperature region, a medium temperature region and a high temperature region, wherein the low temperature region is used for low temperature heat treatment, the medium temperature region is used for medium temperature heat treatment and the high temperature region is used for high temperature heat treatment.
Example 1
The embodiment provides a preparation method of a nitrided ferrovanadium alloy, which comprises the following steps:
(1) washing the ferric vanadate mud with hot water of 60 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1: 1, stirring for 5min, vacuum filtering, repeatedly washing with water, stirring and filtering for 3 times, and drying at 80 ℃ for 5h to obtain dry-based ferric vanadate.
(2) Adding vanadium oxide with purity of more than 98.5 percent and granularity of 0.05-0.10 mm and graphite carbon powder with purity of more than 99.0 percent and granularity of 0.05-0.10 mm into dry-based ferric vanadate, uniformly mixing (the mass ratio of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder is 3:6:1), adding water, uniformly mixing (the mass of the water is 13 percent of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder), performing and pressing all materials at the pressure of 30MPa, and drying at the temperature of 80 ℃ for 6 hours to obtain a performing material.
(3) Placing the preformed material into a graphite crucible, placing the material and the crucible into a pushed slab kiln, and sequentially heating the material through a low-temperature region, a medium-temperature region and a high-temperature region, setting the temperature of the low-temperature region in the pushed slab kiln to be 300 ℃, the heating time of the low-temperature region to be 5 hours, the temperature of the medium-temperature region to be 950 ℃, the heating time of the medium-temperature region to be 4 hours, the temperature of the high-temperature region to be 1050 ℃, the heating time of the high-temperature region to be 35 hours, cooling to normal temperature after heating is completed, crushing to obtain a nitrogen nitrided ferrovanadium alloy, and detecting to obtain the nitrogen nitrided ferrovanadium alloy with the vanadium content of 45.2%, the nitrogen content of 22.1% and the impurity content of the nitrogen ferrovanadium alloy respectively: si: 2.0 percent; s: 0.04 percent; p: 0.05 percent; al: 1.0 percent.
Example 2
The embodiment provides a preparation method of a nitrided ferrovanadium alloy, which comprises the following steps:
(1) washing the ferric vanadate mud with hot water of 80 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1: 2, stirring for 6min, vacuum filtering, repeating the water washing, stirring and filtering for 4 times, and drying at 85 ℃ for 4h to obtain the dry-based ferric vanadate.
(2) Adding vanadium oxide with purity of more than 98.5 percent and granularity of 0.05-0.10 mm and graphite carbon powder with purity of more than 99.0 percent and granularity of 0.05-0.10 mm into dry-based ferric vanadate, uniformly mixing (the mass ratio of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder is 2.5:6:1.5), adding water, uniformly mixing (the mass of the water is 10 percent of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder), performing and pressing all materials at the pressure of 25MPa for 4 hours at 90 ℃ to obtain a performing material.
(3) Placing the preformed material into a graphite crucible, placing the material and the crucible into a pushed slab kiln, and sequentially heating the material through a low temperature region, a medium temperature region and a high temperature region, setting the temperature of the low temperature region in the pushed slab kiln to be 300-400 ℃, the heating time of the low temperature region to be 3 hours, the temperature of the medium temperature region to be 450 ℃, the heating time of the medium temperature region to be 8 hours, the temperature of the high temperature region to be 1650 ℃, the heating time of the high temperature region to be 6 hours, cooling to normal temperature after heating is completed, crushing to obtain the nitrogen-nitrided ferrovanadium alloy, detecting, wherein the vanadium content in the prepared nitrogen-nitrided ferrovanadium alloy is 50.5%, the nitrogen content is 23.8%, and the impurity content in the nitrogen-nitrided ferrovanadium alloy is respectively: si: 1.5 percent; s: 0.045%; p: 0.06 percent; al: 1.5 percent.
Example 3
The embodiment provides a preparation method of a nitrided ferrovanadium alloy, which comprises the following steps:
(1) washing the ferric vanadate mud with hot water of 77 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1: 1, stirring for 7min, vacuum filtering, repeatedly washing with water, stirring and filtering for 5 times, and drying at 90 ℃ for 3h to obtain dry-based ferric vanadate.
(2) Adding vanadium oxide with purity of more than 98.5 percent and granularity of 0.05-0.10 mm and graphite carbon powder with purity of more than 99.0 percent and granularity of 0.05-0.10 mm into dry-based ferric vanadate, uniformly mixing (the mass ratio of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder is 3:6:1), adding water, uniformly mixing (the mass of the water is 16 percent of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder), performing and pressing all materials at 24Mpa, and drying at 85 ℃ for 5 hours to obtain a preformed material.
(3) Placing the preformed material into a graphite crucible, placing the material and the crucible into a pushed slab kiln, and sequentially heating the material through a low-temperature region, a medium-temperature region and a high-temperature region, setting the temperature of the low-temperature region in the pushed slab kiln to be 350 ℃, the heating time of the low-temperature region to be 4 hours, the temperature of the medium-temperature region to be 800 ℃, the heating time of the medium-temperature region to be 6 hours, the temperature of the high-temperature region to be 1400 ℃, the heating time of the high-temperature region to be 29 hours, cooling to normal temperature after heating is completed, crushing to obtain the nitrogen nitride ferrovanadium alloy, and detecting to obtain the nitrogen nitride ferrovanadium alloy with the vanadium content as follows: 50.8%, nitrogen content: 24.6 percent, and the impurity contents in the nitrided ferrovanadium alloy are respectively as follows: si: 1.5 percent; s: 0.04 percent; p: 0.05 percent; al: 1.8 percent.
Example 4
The embodiment provides a preparation method of a nitrided ferrovanadium alloy, which comprises the following steps:
(1) washing the ferric vanadate mud with hot water of 72 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1: 2, stirring for 8min, vacuum filtering, repeatedly washing with water, stirring and filtering for 3 times, and drying at 88 ℃ for 4.5h to obtain dry-based ferric vanadate.
(2) Adding vanadium oxide with purity of more than 98.5 percent and granularity of 0.05-0.10 mm and graphite carbon powder with purity of more than 99.0 percent and granularity of 0.05-0.10 mm into dry-based ferric vanadate, uniformly mixing (the mass ratio of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder is 1:6:2), adding water, uniformly mixing (the mass of the water is 20 percent of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder), performing and pressing all materials at the pressure of 28Mpa, and drying at 83 ℃ for 4.5 hours to obtain a performing material.
(3) Placing the preformed material into a graphite crucible, placing the material and the crucible into a pushed slab kiln, and sequentially heating the material through a low-temperature region, a medium-temperature region and a high-temperature region, setting the temperature of the low-temperature region in the pushed slab kiln to be 330 ℃, the heating time of the low-temperature region to be 3.5 hours, the temperature of the medium-temperature region to be 850 ℃, the heating time of the medium-temperature region to be 5 hours, the temperature of the high-temperature region to be 1500 ℃, the heating time of the high-temperature region to be 19 hours, cooling to normal temperature after heating is completed, crushing to obtain the nitrogen nitrided ferrovanadium alloy, detecting, wherein the vanadium content in the prepared nitrogen nitrided ferrovanadium alloy is 45.2 percent, the nitrogen content is 22.1 percent, and the impurity content in the nitrogen ferrovanadium alloy is respectively: si: 1.9 percent; s: 0.048 percent; p: 0.05 percent; al: 1.6 percent.
Example 5
The embodiment provides a preparation method of a nitrided ferrovanadium alloy, which comprises the following steps:
(1) washing the ferric vanadate mud with hot water of 65 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1: 1, stirring for 10min, vacuum filtering, repeatedly washing with water, stirring and filtering for 5 times, and drying at 83 ℃ for 3.5h to obtain dry-based ferric vanadate.
(2) Adding vanadium oxide with purity of more than 98.5 percent and granularity of 0.05-0.10 mm and graphite carbon powder with purity of more than 99.0 percent and granularity of 0.05-0.10 mm into dry-based ferric vanadate, uniformly mixing (the mass ratio of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder is 3:6:2), adding water, uniformly mixing (the mass of the water is 18 percent of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder), performing and pressing all materials at 21Mpa, and drying at 86 ℃ for 5.5 hours to obtain a preformed material.
(3) Placing the preformed material into a graphite crucible, placing the material and the crucible into a pushed slab kiln, and sequentially heating the material through a low-temperature region, a medium-temperature region and a high-temperature region, setting the temperature of the low-temperature region in the pushed slab kiln to be 350 ℃, the heating time of the low-temperature region to be 4.5 hours, the temperature of the medium-temperature region to be 900 ℃, the heating time of the medium-temperature region to be 7 hours, the temperature of the high-temperature region to be 1600 ℃, the heating time of the high-temperature region to be 18 hours, cooling to normal temperature after heating is completed, crushing to obtain the nitrogen nitrided ferrovanadium alloy, detecting, wherein the vanadium content in the prepared nitrogen nitrided ferrovanadium alloy is 45.2 percent, the nitrogen content is 22.1 percent, and the impurity content in the nitrogen ferrovanadium alloy is respectively: si: 1.8 percent; s: 0.049 percent; p: 0.05 percent; al: 1.7 percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The preparation method of the nitrided ferrovanadium alloy is characterized by comprising the following steps of:
washing ferric vanadate mud with hot water at the temperature of 60-80 ℃, and drying to obtain dry-based ferric vanadate;
adding vanadium oxide and graphite carbon powder with the granularity of 0.05-0.15 mm into the dry-based ferric vanadate, uniformly mixing, adding water, uniformly mixing, performing and pressing, and drying to obtain a performing material;
and thirdly, sequentially carrying out low-temperature heat treatment at 300-400 ℃, medium-temperature heat treatment at 450-950 ℃ and high-temperature heat treatment at 1050-1650 ℃ on the preformed material, and cooling after the heat treatment is finished to obtain the azotized ferrovanadium alloy.
2. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: in the first step, the mass ratio of the ferric vanadate mud to the hot water is 1: 1-2, repeatedly washing with hot water for 3-5 times, wherein the drying temperature is 80-90 ℃, and the drying time is 3-5 h.
3. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: in the second step, the mass ratio of the dry-based ferric vanadate to the vanadium oxide to the graphite carbon powder is 1-3: 6: 1-2.
4. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: in the second step, the purity of the vanadium oxide is more than 98.5%, the granularity of the vanadium oxide is 0.05-0.10 mm, the purity of the graphite carbon powder is more than 99.0%, the granularity of the graphite carbon powder is 0.05-0.10 mm, and the mass of the water is 10-20% of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder.
5. The method for preparing a nitrided ferrovanadium alloy according to claim 4, wherein: in the second step, the mass of the water is 13-16% of the total mass of the dry-based ferric vanadate, the vanadium oxide and the graphite carbon powder.
6. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: and in the second step, the pressure of the preforming pressing is 20-30 Mpa.
7. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: in the second step, the drying temperature is 80-90 ℃, and the drying time is 4-6 h.
8. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: in the third step, the time of the low-temperature heat treatment is 3-5 hours, the time of the medium-temperature heat treatment is 4-8 hours, and the time of the high-temperature heat treatment is 6-40 hours.
9. The method for preparing a nitrided ferrovanadium alloy according to claim 1, wherein: in the third step, the temperature of the low-temperature heat treatment is 300-350 ℃, the temperature of the medium-temperature heat treatment is 800-900 ℃, and the temperature of the high-temperature heat treatment is 1400-1600 ℃.
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