CN113135599B - Preparation method of vanadium iron spinel - Google Patents
Preparation method of vanadium iron spinel Download PDFInfo
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- CN113135599B CN113135599B CN202110545209.6A CN202110545209A CN113135599B CN 113135599 B CN113135599 B CN 113135599B CN 202110545209 A CN202110545209 A CN 202110545209A CN 113135599 B CN113135599 B CN 113135599B
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 38
- 239000011029 spinel Substances 0.000 title claims abstract description 38
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 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 abstract description 22
- 229940062993 ferrous oxalate Drugs 0.000 claims abstract description 19
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 12
- 230000006698 induction Effects 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000008859 change Effects 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 abstract description 21
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 19
- 229910000628 Ferrovanadium Inorganic materials 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 13
- 239000002893 slag Substances 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000011160 research Methods 0.000 abstract description 9
- 230000007246 mechanism Effects 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 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 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/04—Ferrous oxide [FeO]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention provides a preparation method of ferrovanadium spinel, which comprises the following steps: mixing vanadium trioxide and ferrous oxalate to obtain a mixture; tabletting the mixture to obtain a thin slice; and heating the slice to obtain the vanadium iron spinel. The method adopts vanadium trioxide and ferrous oxalate as raw materials to prepare the vanadium iron spinel, and has the advantages of easy acquisition of reaction raw materials, low cost and simple storage. The preparation method of the ferrovanadium spinel provided by the invention is simple and easy to operate, and the prepared ferrovanadium spinel can be effectively used for the research on the roasting mechanism of vanadium slag.
Description
Technical Field
The invention belongs to the technical field of spinels, and particularly relates to a preparation method of vanadium iron spinel.
Background
The vanadium-containing spinel is the most main vanadium-containing phase in the vanadium slag and is also a target processing mineral for vanadium extraction by vanadium slag oxidation. The vanadium-containing spinel is a complex metal oxide solid solution which takes vanadium-iron spinel as a framework and contains a plurality of metal elements such as V, Fe, Ti, Cr, Mg, Al and the like. The phase change characteristics of the vanadium-containing spinel in the oxidizing roasting stage and the migration occurrence characteristics of vanadium elements are always the focus of vanadium slag research and are also the key links for explaining the oxidation phase change mechanism of the vanadium slag. The phase change characteristics of vanadium slag in the oxidizing roasting stage containing different additives are studied all the time, but the evolution characteristics of the vanadium slag have larger differences due to different processes, and students pay more attention to the improvement and research of technological parameters such as roasting and leaching, and the research on the evolution mechanism of the vanadium-containing phase is not deep enough. As a key component of the vanadium-containing spinel, the research on the oxidation phase transition characteristics of the vanadium iron spinel is less, and the research on the oxidation phase transition mechanism of the vanadium iron spinel under various process conditions has important significance on explaining the oxidation of vanadium slag, and can provide key theoretical and technical support for the improvement of the roasting process.
The vanadium iron spinel has a chemical formula of FeO.V 2 O 3 Theoretically, the product is synthesized by ferrous oxide and vanadium trioxide, but the ferrous oxide is difficult to prepare, the preparation cost is high, the time consumption is long, and the product is difficult to store, so that the product is fresh in the market.
Disclosure of Invention
In view of this, the present invention aims to provide a method for preparing vanadium iron spinel, which has simple process and simple raw material source.
The invention provides a preparation method of ferrovanadium spinel, which comprises the following steps:
mixing vanadium trioxide and ferrous oxalate to obtain a mixture;
tabletting the mixture to obtain a thin slice;
and heating the slice to obtain the vanadium iron spinel.
Preferably, the mass ratio of the vanadium trioxide to the ferrous oxalate is (35-45): (55-65).
Preferably, the mixing is carried out under stirring.
Preferably, the diameter of the thin slice is 1-3 cm.
Preferably, the heating is performed under vacuum.
Preferably, the heating temperature is 1330-1370 ℃.
Preferably, the heating further comprises:
and grinding the heated product and then pickling.
Preferably, the ground particle size is 150-250 meshes.
Preferably, the acid washing reagent is dilute hydrochloric acid.
Preferably, the acid washing process further comprises the following steps:
and filtering and drying the product after acid washing to obtain the vanadium iron spinel.
The ferrous oxide is difficult to obtain, the storage is difficult and the cost is high, the vanadium oxide and the ferrous oxalate are used as raw materials to prepare the vanadium iron spinel, and the reaction raw materials are easy to obtain, low in cost and simple to store. The preparation method of the ferrovanadium spinel provided by the invention is simple and easy to operate, and the prepared ferrovanadium spinel can be effectively used for the research on the roasting mechanism of vanadium slag.
Drawings
FIG. 1 is a picture of a sample prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a sample prepared in example 1 of the present invention;
FIG. 3 is a photograph of the spectral detection of a sample prepared in example 1 of the present invention;
FIG. 4 is an XRD diffraction pattern of a sample prepared in example 1 of the present invention;
FIG. 5 is an XRD diffraction pattern of a sample prepared according to comparative example 1 of the present invention;
FIG. 6 is a scanning electron microscope image of a sample prepared in comparative example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a preparation method of ferrovanadium spinel, which comprises the following steps:
mixing vanadium trioxide and ferrous oxalate to obtain a mixture;
tabletting the mixture to obtain a thin slice;
and heating the slice to obtain the vanadium iron spinel.
In the invention, the vanadium trioxide is preferably vanadium trioxide powder; the particle size of the vanadium trioxide powder is preferably 200-300 meshes, more preferably 220-280 meshes, more preferably 240-260 meshes, and most preferably 250 meshes; the ferrous oxalate is preferably ferrous oxalate powder, and the particle size of the ferrous oxalate powder is preferably 200-300 meshes, more preferably 220-280 meshes, more preferably 240-260 meshes, and most preferably 250 meshes.
In the invention, the mass ratio of the vanadium trioxide to the ferrous oxalate is preferably (35-45): (55-65), more preferably (38-42): (58-62), most preferably 40: 60.
in the present invention, the mixing is preferably carried out in an alumina crucible; the caliber of the alumina crucible is preferably 2-4 cm, more preferably 2.5-3.5 mm, and most preferably 3 cm. In the present invention, the mixing is preferably performed under stirring, more preferably, rotational mixing in an automatic stirrer; the number of the rotation is preferably 230 to 270r, more preferably 240 to 260r, and most preferably 250 r; the rotation frequency of the rotation is preferably 40-60 r/min, more preferably 45-55 r/min, and most preferably 50 r/min.
In the present invention, the method of mixing preferably comprises:
mixing the following components in a mass ratio of 40: and putting the 60 vanadium trioxide powder and the ferrous oxalate powder into an alumina crucible with the caliber of 3cm, covering a rubber soft plug, and putting the crucible covered with the rubber soft plug into a small automatic stirring instrument to rotate so as to fully and uniformly mix the sample.
In the present invention, the tableting is preferably performed using a tableting machine. In the invention, the diameter of the thin slice is preferably 1-3 cm, more preferably 1.5-2.5 cm, and most preferably 2 cm; the thickness of the sheet is preferably 0.2 to 0.5cm, and more preferably 0.3 to 0.4 cm.
In the present invention, the heating is preferably performed in a vacuum induction melting furnace; preferably, alcohol is adopted to scrub the inner wall of the vacuum induction melting furnace before heating, the aluminum oxide crucible filled with the thin sheet is placed on a heating base in the furnace after the alcohol is completely volatilized, and the furnace door is closed.
In the present invention, the heating is preferably performed under vacuum; preferably, the vacuum induction furnace is vacuumized, then argon is introduced into the furnace until the pressure in the furnace reaches the standard atmospheric pressure, then the furnace is vacuumized again, and the process is repeated for three times to ensure that no air remains in the furnace and maintain the vacuum environment.
In the present invention, it is preferable to control the temperature rise rate in the vacuum induction furnace by adjusting the heating power, and it is preferable to maintain the vacuum atmosphere in the furnace by taking close attention to the change in the furnace gas pressure and drawing out the furnace gas when the furnace gas pressure starts to increase. In the invention, the heating rate is preferably 20-30 ℃/min, more preferably 22-28 ℃/min, more preferably 24-26 ℃/min, and most preferably 25 ℃/min.
In the invention, the heating temperature is preferably 1330-1370 ℃, more preferably 1340-1360 ℃ and most preferably 1350 ℃; the heat preservation time in the heating process is preferably 0.5-1.5 hours, more preferably 0.8-1.2 hours, and most preferably 1 hour.
In the present invention, it is preferable that the heating further includes:
and taking out the crucible after the temperature of the vacuum induction furnace is slowly reduced to the room temperature.
In the present invention, it is preferable that the heating further includes:
and grinding the heated product and then carrying out acid washing.
In the present invention, the particle size of the grinding is preferably 150 to 250 mesh, more preferably 180 to 220 mesh, and most preferably 200 mesh.
In the present invention, the acid is preferably hydrochloric acid, more preferably dilute hydrochloric acid; the mass concentration of the dilute hydrochloric acid is preferably 5-15%, more preferably 8-12%, and most preferably 10%; the pickling time is preferably 20 to 30 hours, more preferably 22 to 28 hours, and most preferably 24 to 26 hours.
In the present invention, the acid washing method preferably includes:
grinding the heated product to 200 meshes, putting the ground product into a beaker, adding 10% hydrochloric acid by mass, and standing for 24 hours.
In the present invention, it is preferable that the pickling further includes:
and filtering and drying the product after acid washing.
In the present invention, the method of filtering preferably comprises:
and repeatedly cleaning the filter residue obtained after acid washing by using filter paper and distilled water until the pH value of the filter residue water washing liquid is neutral, and then performing suction filtration on the cleaned filter residue by using a suction filter to realize solid-liquid separation.
In the present invention, the drying is preferably performed in an electric hot air drying oven; the drying time is preferably 10-15 hours, more preferably 11-14 hours, and most preferably 12-13 hours.
In the present invention, it is preferable to further include, after obtaining the ferrovanadium spinel:
the morphology, the components and the phase composition of the ferrovanadium spinel are tested by adopting a scanning electron microscope, an energy spectrometer and an X-ray diffractometer.
The method adopts vanadium trioxide and ferrous oxalate as raw materials to prepare the vanadium iron spinel, and has the advantages of easy acquisition of reaction raw materials, low cost and simple storage. The preparation method of the ferrovanadium spinel provided by the invention is simple and easy to operate, and the prepared ferrovanadium spinel can be effectively used for the research on the roasting mechanism of vanadium slag.
Example 1
Accurately weighing 4g of vanadium trioxide powder and 6g of ferrous oxalate powder according to the weight ratio of 40:60, then placing the vanadium trioxide powder and the ferrous oxalate powder into an alumina crucible with the caliber of 3cm, and covering a rubber soft plug; and (3) putting the crucible covered with the rubber soft plug into a small automatic stirring instrument for rotating to fully and uniformly mix the sample, wherein the number of rotation turns is 250r, and the rotation frequency is 50r/min, so as to obtain a mixture.
And preparing the uniformly mixed mixture in the crucible into a circular sheet with the diameter of about 2cm by using a tabletting device.
Scrubbing the inner wall of the vacuum induction melting furnace by using alcohol, putting the alumina crucible containing the slice sample on a heating base in the furnace after the alcohol is completely volatilized, and closing the furnace door; vacuumizing the furnace, introducing argon until the pressure in the furnace reaches the standard atmospheric pressure, and vacuumizing the furnace again; repeating the above steps for three times to ensure that no air remains in the furnace and maintain a vacuum environment.
Starting the induction furnace, controlling the temperature rise rate in the furnace by adjusting the heating power, simultaneously closely paying attention to the change of the pressure in the furnace, immediately pumping out the gas in the furnace when the pressure in the furnace begins to increase, and maintaining the vacuum environment in the furnace; heating to about 1350 ℃, adjusting the heating power to a proper value, keeping the temperature in the furnace to be about 1350 ℃ as much as possible, and keeping the temperature for about 1 h; and (5) stopping heating after the heat preservation is finished, and taking out the crucible after the furnace temperature is slowly reduced to the room temperature.
Taking out a sample in the crucible, grinding the sample to about 200 meshes, then putting the sample into a 200ml beaker, adding 100ml of dilute hydrochloric acid with the mass fraction of 10%, and standing for 24 hours.
Repeatedly cleaning the filter residue after acid washing by using filter paper and a large amount of distilled water until the Ph of the filter residue water washing liquid is neutral; and (3) carrying out suction filtration on the cleaned filter residue by using a suction filter to realize solid-liquid separation, and then placing the obtained solid in an electrothermal blowing drying oven to dry for 12 hours to obtain a sample.
The picture of the sample prepared in example 1 of the present invention is shown in fig. 1, and is clear from fig. 1.
The shape, components and phase composition of the sample prepared in example 1 of the present invention are detected by a scanning electron microscope, an energy spectrometer and an X-ray diffractometer, and the detection results are shown in fig. 2 to 4, as can be seen from fig. 2, the shape of the phase of the sample prepared in example 1 of the present invention is an octahedral crystal form, and is consistent with the feature that ferrovanadium spinel has an octahedral crystal form, as can be seen from fig. 3, the phase of the sample prepared in example 1 of the present invention mainly comprises three elements of V, Fe and O, and is consistent with the element composition of ferrovanadium spinel, as can be seen from fig. 4, the X-ray diffractometer phase analysis results prove that the sample prepared in example 1 of the present invention is ferrovanadium spinel FeO · V 2 O 3 。
Comparative example 1
Accurately weighing 4.55g of vanadium trioxide powder and 5.45g of ferrous oxalate powder according to the weight ratio of 45.5:54.5, then placing the vanadium trioxide powder and the ferrous oxalate powder into an alumina crucible with the caliber of 3cm, and covering a rubber soft plug; and (3) putting the crucible covered with the rubber soft plug into a small automatic stirring instrument to rotate so as to fully and uniformly mix the sample, wherein the number of rotation turns is 250r, and the rotation frequency is 50r/min, so that a mixture is obtained.
The mixture mixed in the crucible is made into a round slice with the diameter of about 2cm by a tabletting device.
Scrubbing the inner wall of the vacuum induction melting furnace by using alcohol, putting the alumina crucible containing the slice sample on a heating base in the furnace after the alcohol is completely volatilized, and closing the furnace door; vacuumizing the furnace, introducing argon until the pressure in the furnace reaches the standard atmospheric pressure, and vacuumizing the furnace again; repeating the above steps for three times to ensure that no air remains in the furnace and maintain a vacuum environment.
Starting the induction furnace, controlling the temperature rise rate in the furnace by adjusting the heating power, simultaneously closely paying attention to the change of the pressure in the furnace, immediately pumping out the gas in the furnace when the pressure in the furnace begins to increase, and maintaining the vacuum environment in the furnace; heating to about 1350 ℃, adjusting the heating power to a proper value, keeping the temperature in the furnace to be about 1350 ℃ as much as possible, and keeping the temperature for about 1 h; and (5) stopping heating after the heat preservation is finished, and taking out the crucible after the furnace temperature is slowly reduced to the room temperature.
Taking out a sample in the crucible, grinding the sample to about 200 meshes, then putting the sample into a 200ml beaker, adding 100ml of dilute hydrochloric acid with the mass fraction of 10%, and standing for 24 hours.
Repeatedly cleaning the filter residue after acid washing by using filter paper and a large amount of distilled water until the Ph of the filter residue water washing liquid is neutral; and (3) carrying out suction filtration on the cleaned filter residue by using a suction filter to realize solid-liquid separation, and then placing the obtained solid in an electrothermal blowing drying oven to dry for 12 hours to obtain a sample.
The sample prepared in comparative example 1 was subjected to X-ray diffraction phase analysis and scanning electron microscope morphology analysis, and the detection results are shown in fig. 5 and 6; as can be seen from FIGS. 5 and 6, the product prepared in comparative example 1 of the present invention contains a phase of vanadium trioxide, which indicates that the vanadium trioxide as the starting material is not completely reacted, i.e., the vanadium trioxide is excessive and cannot be removed by the subsequent acid washing.
The method adopts vanadium trioxide and ferrous oxalate as raw materials to prepare the vanadium iron spinel, and has the advantages of easy acquisition of reaction raw materials, low cost and simple storage. The preparation method of the ferrovanadium spinel provided by the invention is simple and easy to operate, and the prepared ferrovanadium spinel can be effectively used for the research on the roasting mechanism of vanadium slag.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (1)
1. A preparation method of vanadium iron spinel comprises the following steps:
accurately weighing 4g of vanadium trioxide powder and 6g of ferrous oxalate powder according to the weight ratio of 40:60, then placing the vanadium trioxide powder and the ferrous oxalate powder into an alumina crucible with the caliber of 3cm, and covering a rubber soft plug; putting the crucible covered with the rubber soft plug into a small automatic stirring instrument for rotating to fully and uniformly mix the sample, wherein the number of rotating circles is 250r, and the rotating frequency is 50r/min to obtain a mixture;
preparing the uniformly mixed mixture in the crucible into a circular sheet with the diameter of 2cm by using a tabletting device;
scrubbing the inner wall of the vacuum induction melting furnace by using alcohol, putting the alumina crucible containing the slice sample on a heating base in the furnace after the alcohol is completely volatilized, and closing the furnace door; vacuumizing the furnace, introducing argon until the pressure in the furnace reaches the standard atmospheric pressure, and vacuumizing the furnace again; repeating the above steps for three times to ensure that no air remains in the furnace and maintain a vacuum environment;
starting the induction furnace, controlling the temperature rise rate in the furnace by adjusting the heating power, simultaneously closely paying attention to the change of the pressure in the furnace, immediately pumping out the gas in the furnace when the pressure in the furnace begins to increase, and maintaining the vacuum environment in the furnace; heating to 1350 ℃, adjusting the heating power to a proper value, keeping the temperature in the furnace at 1350 ℃, and preserving the heat for 1 h; stopping heating after the heat preservation is finished, and taking out the crucible after the furnace temperature is slowly reduced to the room temperature;
Taking out a sample in the crucible, grinding the sample to 200 meshes, then putting the sample into a 200ml beaker, adding 100ml of dilute hydrochloric acid with the mass fraction of 10%, and standing for 24 hours;
repeatedly cleaning the filter residue after acid washing by using filter paper and a large amount of distilled water until the pH value of the filter residue water washing liquid is neutral; and carrying out suction filtration on the cleaned filter residue by using a suction filter to realize solid-liquid separation, and then placing the obtained solid in an electrothermal blowing drying oven to dry for 12h to obtain the vanadium iron spinel.
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