CN113736987B - Preparation method of nitrided ferrovanadium alloy - Google Patents
Preparation method of nitrided ferrovanadium alloy Download PDFInfo
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- CN113736987B CN113736987B CN202110882973.2A CN202110882973A CN113736987B CN 113736987 B CN113736987 B CN 113736987B CN 202110882973 A CN202110882973 A CN 202110882973A CN 113736987 B CN113736987 B CN 113736987B
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- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 title claims description 17
- 239000000956 alloy Substances 0.000 title claims description 17
- 229910000628 Ferrovanadium Inorganic materials 0.000 title claims description 12
- 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 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 38
- 239000010439 graphite Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 37
- 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 27
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 229910000640 Fe alloy Inorganic materials 0.000 abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 22
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000002910 solid waste Substances 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910001021 Ferroalloy Inorganic materials 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
- 229910001337 iron nitride Inorganic materials 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 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
- 229910052742 iron Inorganic materials 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
- -1 ferrovanadium nitride Chemical class 0.000 description 2
- 239000007788 liquid Substances 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
- 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
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 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
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- 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
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention relates to the technical field of ferroalloy, in particular to a preparation method of vanadium nitride ferroalloy, which comprises the following steps: washing the ferric vanadate mud with hot water at 60-80 ℃ and drying to obtain dry-base ferric vanadate; adding vanadium oxide with the granularity of 0.05-0.15 mm and graphite carbon powder into the dry-base ferric vanadate, uniformly mixing, adding water, uniformly mixing, performing and pressing, and drying to obtain a preformed 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 nitrided vanadium iron alloy. The method provided by the invention is simple to operate, the purified ferric vanadate mud is used as a raw material, so that the high-efficiency utilization of solid waste is realized, the impurity content in the ferric vanadate mud is reduced, the production cost of the vanadium nitride iron alloy is reduced, and the vanadium nitride iron alloy with low cost, low impurity 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 vanadium nitride ferroalloy.
Background
Vanadium nitride is used as an important alloy additive of high-strength micro-alloy steel, and the addition of vanadium nitride iron alloy into the steel can improve the strength, toughness, wear resistance, corrosion resistance and thermal fatigue resistance of the steel, and can ensure that the steel has excellent weldability. The main methods for producing the vanadium iron nitride at present are a solid nitriding method and a liquid nitriding method. The two methods are both to take the ferrovanadium alloy as the raw material, and simultaneously to select a plurality of vanadium-containing oxides and auxiliary materials to be introduced with nitrogen at a certain temperature and pressure for nitriding reaction, but the preparation method of the ferrovanadium nitride in the prior art has the advantages of high raw material cost, complex production process, long reaction time, high energy consumption and lower nitrogen content of the prepared ferrovanadium nitride.
A large amount of vanadium-containing waste is generated in the process of producing ammonium vanadate by precipitating vanadium, and the main components of the vanadium-containing waste are water and ferric vanadate mud. The method for preparing the vanadium iron nitride by taking the ferric vanadate mud as the raw material can reduce the cost of the raw material, but the ferric vanadate mud has complex composition phase and high impurity content, and the quality of a final product can be influenced by directly preparing the vanadium iron nitride by taking the ferric vanadate mud as the raw material. And as the content of the ferric vanadate mud water is high, the problem that materials are not easy to mix uniformly exists in the mixing process.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a preparation method of vanadium iron nitride alloy, which takes the purified ferric vanadate mud as a raw material, realizes the efficient utilization of solid waste, reduces the content of impurities in the ferric vanadate mud, greatly reduces the production cost of the vanadium iron nitride alloy, and can prepare the vanadium iron nitride alloy with low cost, low impurities and high nitrogen content, thereby overcoming the defects of the prior art.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the embodiment of the invention provides a preparation method of vanadium nitride iron alloy, which comprises the following steps:
washing the ferric vanadate mud with hot water at 60-80 ℃ and drying to obtain dry-base ferric vanadate;
adding vanadium oxide with the granularity of 0.05-0.15 mm and graphite carbon powder into the dry-base ferric vanadate, uniformly mixing, adding water, uniformly mixing, performing and pressing, and drying to obtain a preformed 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 nitrided vanadium iron alloy.
According to the preparation method of the vanadium nitride iron alloy, the iron vanadate mud is used as a raw material, so that the high-efficiency utilization of solid waste can be realized, and the production cost of the vanadium nitride iron alloy can be greatly reduced. According to the preparation method, firstly, 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 granularity of the vanadium oxide and the graphite carbon powder. Finally, through carrying out heat treatment in stages at different temperatures, the dehydration of the material in the low-temperature heat treatment stage, the reduction of the medium-temperature heat treatment stage and the nitridation of the medium-temperature heat treatment stage can be accurately controlled, 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 in the vanadium nitride iron alloy prepared by the preparation method is 20-25%, the vanadium content is 45-55%, and the impurity content in the vanadium nitride iron alloy 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%; al is less than or equal to 2.0 percent.
The ferric vanadate mud can adopt ferric vanadate mud in vanadium-containing solid waste recovered from the ammonium vanadate production by vanadium precipitation, wherein the water content of the wet-based ferric vanadate mud in the vanadium-containing solid waste is 45-55%, the vanadium oxide content is 22-30%, the iron content is 20-25%, the Si content is 0.15-0.25%, the S content is 2-3%, the P content is 0.01-0.02%, the Al content is 0.05-0.15%, and the impurity content of the wet-based ferric 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 carrying out hot water washing 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 suction filtration.
In the process of carrying out multiple water washing impurity removal on ferric vanadate mud, the adopted washing water can be recycled, and no secondary solid waste and waste liquid are generated in the whole process. And removing impurities from the ferric vanadate mud with high water content, and drying to obtain dry-base ferric vanadate, so that the full mixing of materials in the subsequent step is facilitated.
Preferably, in the second step, the mass ratio of the dry-base 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 used as a main raw material containing vanadium to produce the vanadium nitride iron alloy after being washed by hot water, and the 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-basis ferric vanadate, the vanadium oxide and the graphite carbon powder.
The quality of the prepared vanadium nitride iron alloy can be improved by controlling the purity of the vanadium oxide and the graphite carbon powder, and the granularity of the vanadium oxide and the graphite carbon powder is basically consistent with the granularity of the dry-base ferric vanadate by controlling the granularity of the vanadium oxide and the graphite carbon powder, so that the uniform mixing is facilitated.
Preferably, in the second step, the mass of water is 13-16% of the total mass of the dry-basis 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 not only a dehydration drying process but also a preheating process, and the subsequent heating time from the temperature rise to the low-temperature heat treatment temperature can be shortened through the preheating in the second step.
Preferably, in the third step, the heating time of the low-temperature heat treatment is 3 to 5 hours, the heating time of the medium-temperature heat treatment is 4 to 8 hours, and the heating time of the high-temperature heat treatment is 6 to 40 hours.
By adopting the time of each heat treatment stage, the processes of dehydration of materials 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 low temperature heat treatment temperature is 300-350 ℃, the medium temperature heat treatment temperature is 800-900 ℃, and the high temperature heat treatment temperature is 1400-1600 ℃.
The preparation method of the vanadium iron nitride 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 waste is realized. The nitrogen content in the vanadium nitride iron alloy prepared by the preparation method is 20-25%, the vanadium content is 45-55%, and the impurity content in the vanadium nitride iron alloy 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%; al is less than or equal to 2.0 percent.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The push plate kiln of the following embodiment is provided with a low temperature zone, a middle temperature zone and a high temperature zone, wherein the low temperature zone is used for carrying out low temperature heat treatment, the middle temperature zone is used for carrying out middle temperature heat treatment and the high temperature zone is used for carrying out high temperature heat treatment.
Example 1
The embodiment provides a preparation method of vanadium nitride iron alloy, which comprises the following steps:
(1) Washing ferric vanadate mud with hot water at 60 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1:1, stirring for 5min, vacuum filtering, repeatedly washing, stirring and filtering for 3 times, and drying at 80 ℃ for 5h to obtain the dry-base 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-base ferric vanadate, uniformly mixing (the mass ratio of the dry-base ferric vanadate to the vanadium oxide to 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-base ferric vanadate, the vanadium oxide and the graphite carbon powder), preforming and pressing all materials, wherein the pressing pressure is 30mpa, and drying for 6 hours at 80 ℃ to obtain a preformed material.
(3) Placing the preformed material in a graphite crucible, placing the material and the crucible into a pushed slab kiln to be heated sequentially through a low temperature zone, a medium temperature zone and a high temperature zone, setting the temperature of the low temperature zone in the pushed slab kiln to be 300 ℃, the heating time of the low temperature zone to be 5 hours, the temperature of the medium temperature zone to be 950 ℃, the heating time of the medium temperature zone to be 4 hours, the temperature of the high temperature zone to be 1050 ℃, the heating time of the high temperature zone to be 35 hours, cooling to normal temperature after heating is finished, crushing to obtain the nitrided vanadium iron alloy, and detecting that the vanadium content in the prepared nitrided vanadium iron alloy is 45.2%, the nitrogen content is 22.1%, and the impurity contents in the nitrided vanadium iron alloy are respectively: si:2.0%; s:0.04%; p:0.05%; al:1.0%.
Example 2
The embodiment provides a preparation method of vanadium nitride iron alloy, which comprises the following steps:
(1) Washing ferric vanadate mud with hot water at 80 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1:2, stirring for 6min, vacuum filtering, repeatedly washing, stirring and filtering for 4 times, and drying at 85 ℃ for 4 hours to obtain the dry-base ferric vanadate.
(2) Adding vanadium oxide with the purity of more than 98.5 percent and the granularity of 0.05-0.10 mm and graphite carbon powder with the purity of more than 99.0 percent and the granularity of 0.05-0.10 mm into dry-base ferric vanadate, uniformly mixing (the mass ratio of the dry-base ferric vanadate to the vanadium oxide to 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-base ferric vanadate, the vanadium oxide and the graphite carbon powder), preforming and pressing all materials, and drying the materials at 90 ℃ for 4 hours under 25mpa to obtain the preformed material.
(3) Placing the preformed material in a graphite crucible, placing the material and the crucible into a pushed slab kiln, sequentially heating the materials through a low temperature area, a medium temperature area and a high temperature area, setting the temperature of the low temperature area in the pushed slab kiln to be 300-400 ℃, the heating time of the low temperature area to be 3 hours, the temperature of the medium temperature area to be 450 ℃, the heating time of the medium temperature area to be 8 hours, the temperature of the high temperature area to be 1650 ℃, the heating time of the high temperature area to be 6 hours, cooling to normal temperature after heating is finished, crushing to obtain the nitrided vanadium iron alloy, and detecting that the vanadium content in the prepared nitrided vanadium iron alloy is 50.5%, the nitrogen content is 23.8%, and the impurity content in the nitrided vanadium iron alloy is respectively: si:1.5%; s:0.045%; p:0.06%; al:1.5%.
Example 3
The embodiment provides a preparation method of vanadium nitride iron alloy, which comprises the following steps:
(1) Washing ferric vanadate mud with hot water at 77 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1:1, stirring for 7min, vacuum filtering, repeatedly washing, stirring and filtering for 5 times, and drying at 90 ℃ for 3h to obtain the dry-base 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-base ferric vanadate, uniformly mixing (the mass ratio of the dry-base ferric vanadate to the vanadium oxide to 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-base ferric vanadate, the vanadium oxide and the graphite carbon powder), preforming and pressing all materials, wherein the pressing pressure is 24mpa, and drying for 5 hours at 85 ℃ to obtain a preformed material.
(3) Placing the preformed material in a graphite crucible, placing the material and the crucible into a pushed slab kiln to be heated sequentially through a low temperature zone, a medium temperature zone and a high temperature zone, setting the temperature of the low temperature zone in the pushed slab kiln to be 350 ℃, the heating time of the low temperature zone to be 4 hours, the temperature of the medium temperature zone to be 800 ℃, the heating time of the medium temperature zone to be 6 hours, the temperature of the high temperature zone to be 1400 ℃, the heating time of the high temperature zone to be 29 hours, cooling to normal temperature after heating is completed, crushing to obtain the vanadium-iron nitride alloy, and detecting that the vanadium content in the prepared vanadium-iron nitride alloy is: 50.8% of nitrogen: 24.6 percent, the impurity content in the nitrided ferrovanadium alloy is respectively as follows: si:1.5%; s:0.04%; p:0.05%; al:1.8%.
Example 4
The embodiment provides a preparation method of vanadium nitride iron alloy, which comprises the following steps:
(1) Washing ferric vanadate mud with hot water at 72 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1:2, stirring for 8min, vacuum filtering, repeatedly washing, stirring and filtering for 3 times, and drying at 88 ℃ for 4.5h to obtain the dry-base 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-base ferric vanadate, uniformly mixing (the mass ratio of the dry-base ferric vanadate to the vanadium oxide to 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-base ferric vanadate, the vanadium oxide and the graphite carbon powder), preforming and pressing all materials, and drying for 4.5 hours at 83 ℃ under 28mpa to obtain a preformed material.
(3) Placing the preformed material in a graphite crucible, placing the material and the crucible into a pushed slab kiln, sequentially heating the materials through a low temperature area, a medium temperature area and a high temperature area, setting the temperature of the low temperature area in the pushed slab kiln to be 330 ℃, the heating time of the low temperature area to be 3.5 hours, the temperature of the medium temperature area to be 850 ℃, the heating time of the medium temperature area to be 5 hours, the temperature of the high temperature area to be 1500 ℃, the heating time of the high temperature area to be 19 hours, cooling to normal temperature after heating is finished, crushing to obtain the nitrided vanadium-iron alloy, and detecting that the vanadium content in the prepared nitrided vanadium-iron alloy is 45.2%, the nitrogen content is 22.1%, and the impurity contents in the nitrided vanadium-iron alloy are respectively: si:1.9%; s:0.048%; p:0.05%; al:1.6%.
Example 5
The embodiment provides a preparation method of vanadium nitride iron alloy, which comprises the following steps:
(1) Washing ferric vanadate mud with hot water at 65 ℃, wherein the mass ratio of the ferric vanadate mud to the hot water is 1:1, stirring for 10min, vacuum filtering, repeatedly washing, stirring and filtering for 5 times, and drying at 83 ℃ for 3.5h to obtain the dry-base 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-base ferric vanadate, uniformly mixing (the mass ratio of the dry-base ferric vanadate to the vanadium oxide to 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-base ferric vanadate, the vanadium oxide and the graphite carbon powder), preforming and pressing all materials, and drying for 5.5 hours at 86 ℃ under 21mpa to obtain a preformed material.
(3) Placing the preformed material in a graphite crucible, placing the material and the crucible into a pushed slab kiln, sequentially heating the materials through a low temperature area, a medium temperature area and a high temperature area, setting the temperature of the low temperature area in the pushed slab kiln to be 350 ℃, the heating time of the low temperature area to be 4.5 hours, the temperature of the medium temperature area to be 900 ℃, the heating time of the medium temperature area to be 7 hours, the temperature of the high temperature area to be 1600 ℃, the heating time of the high temperature area to be 18 hours, cooling to normal temperature after heating is finished, crushing to obtain the nitrided vanadium-iron alloy, and detecting that the vanadium content in the prepared nitrided vanadium-iron alloy is 45.2%, the nitrogen content is 22.1%, and the impurity contents in the nitrided vanadium-iron alloy are respectively: si:1.8%; s:0.049%; p:0.05%; al:1.7%.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (5)
1. The preparation method of the nitrided ferrovanadium alloy is characterized by comprising the following steps:
washing the ferric vanadate mud with hot water at 60-80 ℃ and drying to obtain dry-base ferric vanadate;
adding vanadium oxide with the granularity of 0.05-0.15 mm and graphite carbon powder into the dry-base ferric vanadate, uniformly mixing, adding water, uniformly mixing, performing and pressing, and drying to obtain a preformed material;
step three, the preformed material is subjected to low temperature heat treatment at 300-400 ℃, medium temperature heat treatment at 450-950 ℃ and high temperature heat treatment at 1050-1650 ℃ in sequence, and cooled after the heat treatment is finished, so that the nitrided ferrovanadium alloy is obtained;
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;
in the first step, the mass ratio of the ferric vanadate mud to the hot water is 1: 1-2, repeatedly performing hot water washing for 3-5 times, wherein the drying temperature is 80-90 ℃, and the drying time is 3-5 hours;
in the second step, the mass ratio of the dry-base ferric vanadate to the vanadium oxide to the graphite carbon powder is 1-3:6:1-2;
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 ℃.
2. A method of producing 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-base ferric vanadate, the vanadium oxide and the graphite carbon powder.
3. A method of producing a nitrided ferrovanadium alloy according to claim 2, wherein: in the second step, the mass of the water is 13-16% of the total mass of the dry-base ferric vanadate, vanadium oxide and graphite carbon powder.
4. A method of producing a nitrided ferrovanadium alloy according to claim 1, wherein: in the second step, the pressure of the preformed pressing is 20-30 Mpa.
5. A method of producing 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.
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