CN114684855A - Method for preparing vanadium pentoxide in different shapes by combining hydrothermal method with calcination method - Google Patents
Method for preparing vanadium pentoxide in different shapes by combining hydrothermal method with calcination method Download PDFInfo
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- CN114684855A CN114684855A CN202210549799.4A CN202210549799A CN114684855A CN 114684855 A CN114684855 A CN 114684855A CN 202210549799 A CN202210549799 A CN 202210549799A CN 114684855 A CN114684855 A CN 114684855A
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 227
- 238000000034 method Methods 0.000 title claims abstract description 66
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 59
- 238000001354 calcination Methods 0.000 title claims abstract description 53
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 55
- 238000010438 heat treatment Methods 0.000 claims description 53
- 238000006243 chemical reaction Methods 0.000 claims description 41
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000000843 powder Substances 0.000 claims description 36
- 239000002904 solvent Substances 0.000 claims description 36
- 238000005406 washing Methods 0.000 claims description 36
- 238000001816 cooling Methods 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 34
- 229910021641 deionized water Inorganic materials 0.000 claims description 34
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 25
- 235000006408 oxalic acid Nutrition 0.000 claims description 20
- 238000005119 centrifugation Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 229910045601 alloy Inorganic materials 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 4
- PTXMVOUNAHFTFC-UHFFFAOYSA-N alumane;vanadium Chemical compound [AlH3].[V] PTXMVOUNAHFTFC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 34
- 235000019441 ethanol Nutrition 0.000 description 17
- 239000010935 stainless steel Substances 0.000 description 16
- 229910001220 stainless steel Inorganic materials 0.000 description 16
- 238000009210 therapy by ultrasound Methods 0.000 description 16
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 14
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 8
- 229960002303 citric acid monohydrate Drugs 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000010304 firing Methods 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 210000002268 wool Anatomy 0.000 description 4
- 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 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 238000000277 atomic layer chemical vapour deposition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
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- 238000003980 solgel method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910000314 transition metal oxide 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
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
Abstract
The invention discloses a method for preparing vanadium pentoxide with different shapes by combining a hydrothermal method with a calcining method, and the method comprises the step of preparing the vanadium pentoxide with different shapes by combining the hydrothermal method with the calcining method. The method mainly adopts a hydrothermal method and a calcining method to prepare vanadium pentoxide (V) with different shapes2O5) The method is expected to be applied to improving the charge and discharge performance of the all-vanadium redox flow battery, the vanadium-aluminum intermediate alloy, the electrode material, the photocatalytic efficiency or the solid-state ion battery and the like.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for preparing vanadium pentoxide with different shapes by combining a hydrothermal method with a calcining method.
Background
In the rapidly developing 21 st century, environmental pollution and energy scarcity are important problems facing modern mankind and urgently to be solved. Vanadium is a globally recognized resource shortage and an important strategic substance, and the creation of new energy has become a major subject of research under the strategy of the current sustainable development. Vanadium has excellent alloy performance and catalytic performance, and is widely applied to the fields of metallurgy, chemical industry, machinery, electronics, automobiles, railways, light industry and the like 85% of vanadium is consumed by the steel industry, wherein the high-purity vanadium oxide is applied to high-precision fields such as all-vanadium redox flow batteries, vanadium-aluminum intermediate alloys, electrode materials or catalysts (photocatalysis). Transition metal oxide, vanadium pentoxide (V) with low gap energy (2.3eV)2O5) Has received much attention due to its excellent physicochemical properties. The catalysis is one of the properties of vanadium pentoxide, and the photocatalysis has the advantages of environmental compatibility, high energy efficiency, safety, no pollution and the like, and is expected to become one of the most promising effective air purification technologies in the field of energy environment. It is well known that different preparation methods affect the structure, morphology, properties of the material. Common methods for preparing vanadium pentoxide in the prior art include atomic layer chemical vapor deposition, sol-gel processes, thermal deposition, hydrothermal processes, and thermal evaporation processes. Preparation of V2O5The structure is mostly nano-wire, nano-rod, nano-tube and nano-belt. Compared with the above methods, both the hydrothermal method and the calcination method are simple and easy to operate. The method mainly adopts a hydrothermal method as a main calcination method and adopts a hydrothermal method as an auxiliary calcination method to produce various shapes with different shapes.
Disclosure of Invention
In the prior art, a hydrothermal method is mainly used as an auxiliary calcining method, so that a plurality of shapes with different shapes are generated rarely and rarely. Aiming at the defects in the prior art, the invention aims to provide a method for preparing vanadium pentoxide by combining a hydrothermal method with a calcining method, which is expected to be used for improving the photocatalytic efficiency, the charge and discharge performance of a solid-state ion battery and the like; the preparation method is simple, high in controllability, low in cost and capable of meeting the environmental requirements.
As the conception, the technical scheme adopted by the invention is as follows:
a method for preparing vanadium pentoxide with different shapes by combining a hydrothermal method with a calcining method is characterized by comprising the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tubular furnace, and burning at high temperature to prepare vanadium pentoxide;
(2) putting vanadium pentoxide and oxalic acid into a single-neck flask, adding deionized water, heating at a constant temperature and stirring to obtain a blue solution;
(3) mixing the blue solution and isopropanol fully, stirring and placing the mixture in a reaction kettle for hydrothermal reaction;
(4) after the reaction is finished, naturally cooling, carrying out ultrasonic centrifugal washing by taking water as a solvent until separation is carried out, and then carrying out ultrasonic centrifugal washing by taking ethanol as a solvent until separation is carried out;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) placing the black powder into a tubular furnace for vacuum calcination, and naturally cooling to obtain the vanadium pentoxide shape.
In the step (2), the mass ratio of the vanadium pentoxide to the oxalic acid is 1:2-2.5, and the weight volume ratio of the oxalic acid to the deionized water is 1g/7-15 ml.
The constant temperature heating in the step (2) is carried out at the temperature of 80-90 ℃ for 2-4 h.
The volume ratio of the blue solution to the isopropanol in the step (3) is 1: 1.
The temperature of the hydrothermal reaction in the step (3) is 180-200 ℃, and the reaction time is 6-8 h.
In the step (6), the calcination is carried out by heating to 350-380 ℃ at a heating rate of 10 ℃/min and then carrying out heat preservation for 1.8-2.5 h.
The invention has the beneficial effects that:
(1) the invention mainly adopts a hydrothermal method and a calcining method to prepare vanadium pentoxide (V) with different shapes2O5) The material is expected to be applied to improving the charge and discharge performance of the all-vanadium redox flow battery, the vanadium-aluminum intermediate alloy, the electrode material, the photocatalytic efficiency or the solid-state ion battery and the like;
(2) the invention has simple and convenient manufacturing method, high controllable degree, lower cost, wide popularization and application range, safety, no pollution to the environment and accordance with the environmental requirement of the 21 st century.
Description of the drawings:
FIG. 1 shows that V with different shapes is prepared under different reaction conditions2O5SEM image of (a):
(a) v prepared in example 12O5SEM image of (a);
(b) example 2 preparation of V2O5SEM image of (a);
(c) v prepared in example 32O5SEM image of (a);
(d) example 4 preparation of V2O5SEM image of (a);
(e) v prepared in example 52O5SEM image of (a);
(f) v prepared in example 62O5SEM image of (a);
(g) v prepared in example 72O5SEM image of (a);
(h) v prepared in example 82O5SEM image of (a);
(i) v prepared in example 92O5SEM image of (a);
(j) v prepared in example 102O5SEM image of (a);
(k) example 11 preparation of V2O5SEM image of (a);
(l) V prepared in example 122O5SEM image of (a);
(m) V prepared in example 132O5SEM image of (a);
(n) V prepared in example 142O5SEM image of (a);
(o) V prepared in example 152O5SEM image of (a);
(p) V prepared in example 162O5SEM image of (a);
FIG. 2 is V prepared in example 32O5In N2And CO2LSV image measured in atmosphere;
FIG. 3 is V prepared in example 162O5XRD pattern of (a).
Detailed Description
The embodiments of the present invention will be described in detail below, and the embodiments described below by referring to the drawings are exemplary and intended to be used for explaining the present invention, and should not be construed as limiting the present invention.
The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
A method for preparing flaky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 600 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 3mL of blue solution and 3mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and preserving heat at 180 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain the flaky vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is flaky, and an SEM image is shown in figure 1 a.
Example 2
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 600 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 6g oxalic acid (H)2C2O4·2H2O) in a single-necked flask, 60mL of deionized water was addedHeating and stirring the sub-water in a digital display temperature-controlled magnetic stirrer at a constant temperature of 90 ℃ for 3 hours to obtain a blue solution;
(3) taking 3mL of blue solution and 3mL of isopropanol, fully mixing and stirring for 30min, placing the mixture into a 100mL stainless steel reaction kettle for hydrothermal reaction, and preserving heat for 8h at 180 ℃;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tubular furnace for vacuum calcination, heating to 380 ℃ at the heating rate of 10 ℃/min, then preserving the heat for 1.8h, and naturally cooling to obtain the blocky vanadium pentoxide.
Vanadium pentoxide prepared in this example is blocky in morphology, and the SEM image is shown in fig. 1 b.
Example 3
A method for preparing vanadium pentoxide in a shape by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 600 ℃ for 2 hours, and burning to prepare vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 5.2g oxalic acid (H)2C2O4·2H2O) adding 53mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 9mL of blue solution and 9mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2.5 hours, and naturally cooling to obtain the spherical vanadium pentoxide.
In this example, a small amount of V can be formed on the surface due to too short reaction time2O5Smooth spheres, SEM image see FIG. 1 c.
Example 4
A method for preparing vanadium pentoxide in a shape by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature of 900 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 5.5g oxalic acid (H)2C2O4·2H2O) adding 56mL of deionized water into a single-neck flask, and heating and stirring for 3h at a constant temperature of 90 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 9mL of blue solution and 9mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tubular furnace for vacuum calcination, heating to 370 ℃ at the heating rate of 10 ℃/min, then preserving heat for 2.3h, and naturally cooling to obtain petal-shaped vanadium pentoxide.
The vanadium pentoxide prepared in this example is petal-shaped, and the SEM image is shown in fig. 1 d.
Example 5
A method for preparing vanadium pentoxide in a shape by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 450 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 5.1g oxalic acid (H)2C2O4·2H2O) adding 52mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 10mL of blue solution and 10mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) placing the black powder in a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain the honeycomb vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is honeycomb-shaped, and an SEM image is shown in figure 1 e.
Example 6
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 3mL of blue solution and 3mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and preserving heat at 180 ℃ for 8 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tubular furnace for vacuum calcination, heating to 360 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain the hemispherical cluster vanadium pentoxide.
In the embodiment, vanadium pentoxide is prepared, and at 180 ℃, the reaction temperature is low, the formed spheres are agglomerated together, the structure is damaged, the morphology of the spheres is a hemispherical agglomerate, and an SEM image is shown in fig. 1 f.
Example 7
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 12mL of blue solution and 12mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain spherical vanadium pentoxide.
Vanadium pentoxide prepared in this example was smooth in morphology and embedded in blocks (not exfoliated), and the SEM image is shown in fig. 1 g.
Example 8
A method for preparing massive vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2 hours, and burning to prepare vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 10mL of blue solution and 10mL of isopropanol, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain spherical vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is spherical, and an SEM image is shown in figure 1 h.
Example 9
A method for preparing massive vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 12mL of blue solution, 12mL of isopropanol and 0.0151g of citric acid monohydrate, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain spherical vanadium pentoxide.
The vanadium pentoxide prepared in this example is spherical, and the SEM image thereof is shown in fig. 1 i.
Example 10
A method for preparing massive vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 10mL of blue solution, 10mL of isopropanol and 0.0126g of citric acid monohydrate, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain the smooth spherical vanadium pentoxide.
Vanadium pentoxide prepared in this example was in the form of smooth spheres, and a smoother SEM image of the surface of the spheres of example 8 above is shown in fig. 1 j.
Example 11
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 12mL of blue solution, 12mL of isopropanol and 0.0151g of citric acid monohydrate, stirring for 30min, placing the mixture in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain wool spherical vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is in a shape of a wool ball, and an SEM image is shown in figure 1 k.
Example 12
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) taking 14mL of blue solution, 14mL of isopropanol and 0.0173g of citric acid monohydrate, fully mixing and stirring for 30min, placing the mixture into a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain spherical vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is spherical, and an SEM image is shown in figure 1 l.
Example 13
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 2.4g of vanadium pentoxide (V) are taken2O5) And 4.98g oxalic acid (H)2C2O4·2H2O) in a single-neck flask, adding 20mL of deionized water, heating and stirring for 3h in a digital display temperature-controlled magnetic stirrer at constant temperature of 80 ℃ to obtain a blue solution；
(3) Taking 20mL of blue solution, 20mL of isopropanol and 0.0225g of citric acid monohydrate, fully mixing and stirring for 30min, placing in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain the smooth spherical vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is smooth and spherical, and an SEM image is shown in figure 1 m.
Example 14
A method for preparing blocky vanadium pentoxide by combining a hydrothermal method with a calcining method comprises the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tube furnace, keeping the temperature at 300 ℃ for 2h, and burning to obtain vanadium pentoxide (V)2O5)；
(2) 0.9960g of vanadium pentoxide (V) are taken2O5) And 2.0082g oxalic acid (H)2C2O4·2H2O) adding 40mL of deionized water into a single-neck flask, and heating and stirring for 3h at constant temperature of 80 ℃ in a digital display temperature-controlled magnetic stirrer to obtain a blue solution;
(3) fully mixing 18mL of blue solution, 18mL of isopropanol and 0.0200g of citric acid monohydrate, stirring for 30min, placing in a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 200 ℃ for 6 h;
(4) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 2 hours, and naturally cooling to obtain spherical vanadium pentoxide.
The vanadium pentoxide prepared by the embodiment is spherical, and an SEM image is shown in figure 1 n.
Example 15
A method for preparing dandelion-shaped vanadium pentoxide by a hydrothermal method comprises the following steps:
(1) 1mmol ammonium metavanadate, 40mL absolute ethyl alcohol and 3mL polyethylene glycol (PEG-400) are mixed and stirred for 30 min;
(2) adding 1mL of concentrated nitric acid into the solution, stirring for 30min, placing the solution into a 100mL stainless steel reaction kettle for hydrothermal reaction, and preserving the temperature at 180 ℃ for 20 h;
(3) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(4) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven at 60 ℃ for drying for 6 hours to obtain black powder;
(5) and (3) putting the black powder into a tube furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 3 hours, and naturally cooling to obtain dandelion-shaped vanadium pentoxide.
The vanadium pentoxide prepared in the embodiment is dandelion-shaped, and the SEM image is shown in fig. 1 o.
Example 16
A method for preparing rice-shaped vanadium pentoxide by a hydrothermal method comprises the following steps:
(1) mixing and stirring 2mmol of ammonium metavanadate, 30mL of absolute ethyl alcohol and 3mL of polyethylene glycol (PEG-400) for 30 min;
(2) adding 1mL of concentrated nitric acid and 0.0189g of 3mmol citric acid monohydrate into the solution, stirring for 30min, placing the solution into a 100mL stainless steel reaction kettle for hydrothermal reaction, and keeping the temperature at 180 ℃ for 24 h;
(3) after the reaction is finished, naturally cooling, washing and separating for 5 times at the rotating speed of 5000r/m by taking deionized water as a solvent, carrying out ultrasonic treatment for 2 times for 10min, and then washing and separating for 3 times at the rotating speed of 5000r/m by taking ethanol as a solvent;
(4) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven at 60 ℃ for drying for 6 hours to obtain black powder;
(5) and (3) putting the black powder into a tubular furnace for vacuum calcination, heating to 350 ℃ at a heating rate of 10 ℃/min, then preserving heat for 3 hours, and naturally cooling to obtain the rice-shaped vanadium pentoxide.
Vanadium pentoxide prepared in the embodiment is in a rice-ball shape, and an SEM image is shown in figure 1 p.
FIG. 1 is an SEM image of the products of examples 1-16, and the results show that V with different sizes and shapes can be obtained by controlling different reaction conditions (reaction temperature, reaction time and feeding ratio)2O5Solid microspheres;
examples 1 to 7
The ammonium metavanadate firing vanadium pentoxide temperature in the above examples 1, 2, 3 was 600 ℃, but examples 1 and 2 did not form spheres, and the temperature in example 3 was increased, and the sample amount was increased, so that the vanadium pentoxide formed spheres but was not completely formed. In example 4, the temperature for firing the vanadium pentoxide by the ammonium metavanadate is 900 ℃, and the temperature is too high, so that the vanadium pentoxide forms petal shapes. In example 5, the temperature for firing the vanadium pentoxide by the ammonium metavanadate is 450 ℃, and the temperature is high, so that the vanadium pentoxide forms a honeycomb shape. In examples 6 and 7, the temperature for firing the vanadium pentoxide by the ammonium metavanadate is 300 ℃, and the prepared vanadium pentoxide gradually forms a smooth sphere. Therefore, the vanadium pentoxide fired by the ammonium metavanadate at 300 ℃ has a shape closer to the shape.
Examples 8 to 14
In the above embodiment, the temperature for firing the vanadium pentoxide by using the ammonium metavanadate is 300 ℃, the temperature for hydrothermal reaction is 200 ℃ and the time is 6 hours, and the input amount of the blue solution and the isopropanol in the hydrothermal method is increased, so that the vanadium pentoxide is smooth in shape and has a dispersed and clearly visible surface. In example 11, the appearance of the pellets was the ideal appearance of smooth-surfaced wool pellets, the surface was smooth, there were similar wools wound on the pellets with distinct villous roots, and citric acid monohydrate was added in different proportions to disperse the sample without aggregation, making it smoother.
Examples 15 to 16
In the above examples, unlike the above examples, the hydrothermal reaction was directly performed by combining ammonium metavanadate and an organic solvent, and the obtained spheres were not solid spheres.
The positions and relative intensities of the diffraction peaks in FIG. 3 are both V2O5The XRD patterns are matched, which shows that the product synthesized by the method is vanadium pentoxide (V)2O5) A material;
it is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention.
The foregoing embodiments are merely illustrative of the principles and features of this invention, which is not limited to the above-described embodiments, but rather is susceptible to various changes and modifications without departing from the spirit and scope of the invention, which changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for preparing vanadium pentoxide with different shapes by combining a hydrothermal method with a calcining method is characterized by comprising the following steps:
(1) taking a certain amount of ammonium metavanadate, introducing oxygen into a tubular furnace, and burning at high temperature to prepare vanadium pentoxide;
(2) putting vanadium pentoxide and oxalic acid into a single-neck flask, adding deionized water, heating at a constant temperature and stirring to obtain a blue solution;
(3) mixing the blue solution and isopropanol fully, stirring and placing the mixture in a reaction kettle for hydrothermal reaction;
(4) after the reaction is finished and the reaction product is naturally cooled, firstly, water is taken as a solvent for ultrasonic centrifugal washing until separation is finished, and then, ethanol is taken as a solvent for ultrasonic centrifugal washing until separation is finished;
(5) after the centrifugation is finished, putting the obtained bottom layer precipitate into a vacuum drying oven for drying to obtain black powder;
(6) and (3) placing the black powder into a tubular furnace for vacuum calcination, and naturally cooling to obtain the vanadium pentoxide shape.
2. The hydrothermal method combined with the calcination method for preparing vanadium pentoxide with different shapes according to claim 1, wherein the mass ratio of the vanadium pentoxide to the oxalic acid in the step (2) is 1:2-2.5, and the weight-volume ratio of the oxalic acid to the deionized water is 1g/7-15 ml.
3. The hydrothermal method combined with the calcination method for preparing vanadium pentoxide with different shapes according to claim 1, wherein the constant temperature heating in the step (2) is 80-90 ℃ for 2-4 h.
4. The hydrothermal method combined with the calcination method for preparing vanadium pentoxide in different shapes according to claim 1, wherein the volume ratio of the blue solution to the isopropanol in the step (3) is 1: 1.
5. The method for preparing vanadium pentoxide with different shapes according to the combination of a hydrothermal method and a calcination method in the claim 1, wherein the temperature of the hydrothermal reaction in the step (3) is 180-200 ℃, and the reaction time is 6-8 h.
6. The method for preparing vanadium pentoxide with different shapes by combining the hydrothermal method and the calcination method as claimed in claim 1, wherein the calcination in the step (6) is performed by heating to 350-380 ℃ at a heating rate of 10 ℃/min and then maintaining the temperature for 1.8-2.5 h.
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