CN112125338A - Method for preparing M-phase vanadium dioxide by solvothermal method - Google Patents
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- CN112125338A CN112125338A CN202011112463.9A CN202011112463A CN112125338A CN 112125338 A CN112125338 A CN 112125338A CN 202011112463 A CN202011112463 A CN 202011112463A CN 112125338 A CN112125338 A CN 112125338A
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Abstract
The invention discloses a method for preparing M-phase vanadium dioxide by a solvothermal method, belonging to nanometer VO2The technical field of preparation. The invention provides a method for synthesizing nano vanadium dioxide by a solvothermal method for preparing M-phase nano vanadium dioxide powder with high purity, high crystallinity and high uniformity, which comprises the following steps: uniformly mixing an organic solvent, vanadyl acetate and a morphology regulating agent to form a uniform solution, then reacting at 130-260 ℃ for 4-24 h, and after the reaction is finished, centrifuging, washing and drying to obtain the catalyst. The method takes vanadyl acetate as a precursor, and realizes the preparation of vanadium dioxide powder with high granularity crystallinity, good uniformity and smaller granularity by changing a vanadium source, an organic solvent and adding a regulator.
Description
Technical Field
The invention belongs to a nanometer VO2The technical field of preparation, in particular to a method for preparing M-phase vanadium dioxide by adopting a solvothermal method.
Background
VO2The preparation method of the powder mainly comprises a liquid phase method, a solid phase method, a sol-gel method, a thermal decomposition method and the like, wherein the solid phase method generally needs a high-temperature process, and the prepared powder has the defects of large particle size, poor uniformity, serious agglomeration, incapability of effectively controlling the morphology of a product and the like; although the sol-gel method can prepare powder with ideal particle size and uniformity, the powder needs to be subjected to heat treatment, and the problems of high energy consumption and high process cost exist; the thermal decomposition method also has the problems of high energy consumption, low yield and the like.
Different from other methods, the liquid phase method can lead water or other solvents to be in a critical or supercritical state under the environment of high temperature and high pressure, improves the reaction activity, and greatly changes the physical and chemical properties of the required substances in the solvents, so that the liquid phase method not only can prepare powder with uniform granularity, high crystallinity and complete crystal morphology, but also can regulate and control the morphology, crystal form and granularity of the product through process parameters to obtain nano powder with different properties, and is a preferred method for preparing the nano powder. The liquid phase method mainly comprises a hydrothermal method and a solvothermal method, as the name suggests, the hydrothermal method mainly uses an aqueous solution as a solvent, and the solvothermal method mainly uses different organic solvents as solvents, and the principle methods and the advantages of the two methods are approximately the same, but the difference exists.
CN1986125A discloses a preparation method of vanadium dioxide powder, which comprises the steps of dispersing vanadium pentoxide powder into enough organic solvent, adding the solution into a reactor, heating to 140-190 ℃, keeping the solution for 2-24 hours under the pressure of 0.05-10 MPa, naturally cooling and discharging, washing with deionized water and absolute ethyl alcohol, drying in vacuum to obtain vanadium dioxide powder, and finally calcining the powder at the temperature of 300-800 ℃ under the protection of inert gas for 1-12 hours to obtain crystallized vanadium dioxide; wherein the organic solvent is one or a mixed solvent of two or more of methanol, ethanol, n-propanol, isopropanol, n-butanol and n-hexanol. However, the method relates to high-temperature heat treatment, and has the problems of complex process, high energy consumption and low efficiency.
CN101734720A discloses a preparation method of vanadium dioxide ultrafine powder, which comprises the steps of adding oxalic acid into tetravalent or pentavalent alkoxide of vanadium to form a viscous substance, and roasting at 250-800 ℃ for 1-10 hours in vacuum or protective atmosphere to obtain rutile phase vanadium dioxide. The method is different from a solvothermal method, the transformation can be completed only by roasting a crystal phase, and the method also has the defects of complex process and high energy consumption.
CN104724757A discloses a method for directly synthesizing rutile phase vanadium dioxide nano powder based on solvothermal low temperature, which comprises the following steps: (1-10): (1-5) carrying out solvothermal reaction on the uniform solution of the solvent, the cosolvent and the vanadium source at 150-240 ℃ for 2-24 hours, and then centrifuging, washing and drying a reaction product to obtain rutile phase vanadium dioxide nano powder; wherein the solvent is at least one of ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, isopropanol and n-butanol; the vanadium source is at least one of vanadyl acetylacetonate, vanadyl oxalate, vanadyl sulfate, vanadium tetrachloride and vanadium dichloride; the cosolvent is any one of hydrogen peroxide, dilute hydrochloric acid, sodium hydroxide, ammonia water, dilute sulfuric acid, sodium bicarbonate and ammonium bicarbonate. The method mainly uses alcohols as solvents, and practice shows that the alcohol solvents can not effectively control the growth of crystals, so that the prepared vanadium dioxide powder grows excessively, the particle size is mostly in the range of 300-500 nm, and the use requirement of the intelligent window film is difficult to meet.
Disclosure of Invention
Aiming at the defects of the prior solvothermal method, the invention aims to realize the preparation of the M-phase nano vanadium dioxide powder with high purity, high crystallinity and high uniformity.
In order to achieve the aim, the invention provides a novel method for synthesizing nano vanadium dioxide by a solvothermal method, which comprises the following steps: uniformly mixing an organic solvent, vanadyl acetate and a morphology regulator to form a uniform solution, then reacting at 130-260 ℃ for 4-24 h, and after the reaction is finished, centrifuging, washing and drying to obtain the M-phase vanadium dioxide.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the mass ratio of the organic solvent to the vanadyl acetate to the morphology regulator is 70: 0.5-5: 0.1 to 1.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the vanadyl acetate is prepared by the following method: mixing sodium acetate trihydrate and a vanadyl sulfate solution, then reacting at 25-80 ℃, filtering and drying after the reaction is finished, thus obtaining the sodium acetate trihydrate.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the molar ratio of the sodium acetate trihydrate to the vanadyl sulfate in the vanadyl sulfate solution is 2: 1.
in the method for preparing the M-phase vanadium dioxide by the solvothermal method, the molar concentration of the vanadyl sulfate solution is 0.3 mol/L.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the reaction time is 1-5 hours when the vanadyl acetate is prepared; the drying temperature is 60 ℃ and the drying time is 12 h.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the organic solvent is one of toluene, tetrahydrofuran, dioxane, N-dimethylformamide and dimethyl sulfoxide.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the morphology regulator is oleic acid.
In the method for preparing the M-phase vanadium dioxide by the solvothermal method, the reaction is carried out in a reaction kettle with a polytetrafluoroethylene lining.
By adopting the method, the vanadium dioxide powder with high granularity crystallinity, good uniformity and smaller granularity can be prepared, and the granularity range is 50-100 nm.
The invention has the beneficial effects that:
according to the invention, a reaction product of sodium acetate and vanadyl sulfate is used as a new precursor, toluene, tetrahydrofuran, dioxane, N-dimethylformamide, dimethyl sulfoxide and the like are used as organic solvents, oleic acid is used as a protective agent and a morphology regulating agent, and the defects of vanadium dioxide prepared by the existing solvothermal method are overcome by changing a vanadium source, the organic solvents and a method for adding a regulator, so that the preparation of vanadium dioxide powder with high granularity crystallinity, good uniformity and smaller granularity is realized, and the vanadium dioxide powder is a raw material for preparing a window film with excellent performance; the reaction can be realized at a lower temperature, the test condition is mild, the process is controllable, the reaction is synthesized in one step, the process method is simple, the cost is low, and the method is easy to popularize and apply.
Drawings
FIG. 1 shows VO obtained in example 12XRD pattern of powder.
FIG. 2 shows VO obtained in example 12SEM image of powder.
Detailed Description
Specifically, the method for synthesizing the nano vanadium dioxide by the solvothermal method comprises the following steps: uniformly mixing an organic solvent, vanadyl acetate and a morphology regulator to form a uniform solution, then reacting at 130-260 ℃ for 4-24 h, and after the reaction is finished, centrifuging, washing and drying to obtain the M-phase vanadium dioxide.
In the invention, vanadyl acetate can be decomposed in an organic solvent to form vanadium dioxide, and in order to obtain vanadium dioxide powder with high granularity crystallinity, good uniformity and smaller granularity, the invention controls the mass ratio of the organic solvent, the vanadyl acetate and the morphology regulator to be 70: 0.5-5: 0.1 to 1.
In the invention, the vanadyl acetate can be prepared by the following method: mixing sodium acetate trihydrate and a vanadyl sulfate solution, then reacting for 1-5 h at 25-80 ℃, filtering after the reaction is finished, and drying for 12h at 60 ℃ to obtain the sodium acetate trihydrate; wherein the molar ratio of the sodium acetate trihydrate to the vanadyl sulfate in the vanadyl sulfate solution is 2: 1, the molar concentration of the vanadyl sulfate solution is 0.3 mol/L; other methods conventional in the art may also be used.
In the invention, the organic solvent is one of toluene, tetrahydrofuran, dioxane, N-dimethylformamide and dimethyl sulfoxide; the organic solvents have strong solubility and high boiling point, and the hydrophobic solvents can be recycled, thereby being beneficial to obtaining vanadium dioxide powder with high granularity crystallinity, good uniformity and smaller granularity and reducing the production cost.
Through a large amount of screening, the invention takes the oleic acid as the protective agent and the morphology regulating agent, and the oleic acid can form a layer of protective film outside the oleic acid in the formation process of the seed crystal, thereby avoiding the overgrowth of the seed crystal and obtaining the nano powder.
The process of the invention can generally be carried out in a reaction vessel with a polytetrafluoroethylene liner.
By adopting the method, the vanadium dioxide powder with high granularity crystallinity, good uniformity and smaller granularity can be prepared, and the granularity range is 50-100 nm.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
7.5g of sodium acetate trihydrate (CH) are weighed3COONa·3H2O) is added into 92mL vanadyl sulfate solution with the concentration of 0.3mol/L, stirred for 1h under the condition of heat preservation at 25 ℃, filtered and dried for 12h at 60 ℃ to obtain green solid of vanadyl acetate.
Uniformly mixing 70g of toluene, 0.5g of vanadyl acetate and 0.1g of oleic acid, placing the mixture into a 100mL reaction kettle with a polytetrafluoroethylene lining, reacting at 130 ℃ for 24 hours, and after the reaction is finished, centrifuging, washing and drying the product to obtain blue-black powder.
FIG. 1 is an XRD pattern of the blue-black powder, which is illustrated as an M phase, and FIG. 2 is an SEM pattern of the blue-black powder, which has a particle size of about 50 to 100 nm.
Example 2
7.5g of sodium acetate trihydrate (CH) are weighed3COONa·3H2O) is added into 92mL vanadyl sulfate solution with the concentration of 0.3mol/L, stirred for 2h under the condition of heat preservation at 40 ℃, filtered and dried for 12h at 60 ℃ to obtain green solid of vanadyl acetate.
Uniformly mixing 70g of tetrahydrofuran, 2.0g of vanadyl acetate and 0.25g of oleic acid, placing the mixture in a 100mL reaction kettle with a polytetrafluoroethylene lining, reacting at 180 ℃ for 18h, and after the reaction is finished, centrifuging, washing and drying the product to obtain blue-black powder which is M-phase vanadium dioxide powder and has the particle size range of 50-100 nm.
Example 3
7.5g of sodium acetate trihydrate (CH) are weighed3COONa·3H2O) is added into 92mL vanadyl sulfate solution with the concentration of 0.3mol/L, stirred for 3h under the condition of heat preservation at 50 ℃, filtered and dried for 12h at 60 ℃ to obtain green solid of vanadyl acetate.
Uniformly mixing 70g of dioxane, 3.0g of vanadyl acetate and 0.5g of oleic acid, placing the mixture into a 100mL reaction kettle with a polytetrafluoroethylene lining, reacting at 200 ℃ for 12 hours, and after the reaction is finished, centrifuging, washing and drying the product to obtain blue-black powder which is M-phase vanadium dioxide powder and has the granularity of 50-100 nm.
Example 4
7.5g of sodium acetate trihydrate (CH) are weighed3COONa·3H2O) is added into 92mL vanadyl sulfate solution with the concentration of 0.3mol/L, stirred for 4h under the condition of heat preservation at 65 ℃, filtered and dried for 12h at 60 ℃ to obtain green solid of vanadyl acetate.
Uniformly mixing 70g N, N-dimethylformamide, 4.0g of vanadyl acetate and 0.8g of oleic acid, placing the mixture in a 100mL reaction kettle with a polytetrafluoroethylene lining, reacting at 220 ℃ for 8 hours, and after the reaction is finished, centrifuging, washing and drying the product to obtain blue-black powder which is M-phase vanadium dioxide powder and has the granularity range of 50-100 nm.
Example 5
7.5g of sodium acetate trihydrate (CH) are weighed3COONa·3H2O) is added into 92mL vanadyl sulfate solution with the concentration of 0.3mol/L, stirred for 5h under the condition of heat preservation at 80 ℃, filtered and dried for 12h at 60 ℃ to obtain green solid of vanadyl acetate.
Uniformly mixing 70g of dimethyl sulfoxide, 5.0g of vanadyl acetate and 1.0g of oleic acid, placing the mixture into a 100mL reaction kettle with a polytetrafluoroethylene lining, reacting at 260 ℃ for 4h, and after the reaction is finished, centrifuging, washing and drying the product to obtain blue-black powder which is M-phase vanadium dioxide powder and has the particle size range of 50-100 nm.
Claims (10)
1. The method for preparing the M-phase vanadium dioxide by the solvothermal method is characterized by comprising the following steps: the method comprises the following steps: uniformly mixing an organic solvent, vanadyl acetate and a morphology regulator to form a uniform solution, then reacting at 130-260 ℃ for 4-24 h, and after the reaction is finished, centrifuging, washing and drying to obtain the M-phase vanadium dioxide.
2. The solvothermal method for preparing M-phase vanadium dioxide according to claim 1, wherein: the mass ratio of the organic solvent to the vanadyl acetate to the morphology regulating agent is 70: 0.5-5: 0.1 to 1.
3. The solvothermal method for preparing M-phase vanadium dioxide according to claim 1, wherein: the vanadyl acetate is prepared by the following method: mixing sodium acetate trihydrate and a vanadyl sulfate solution, then reacting at 25-80 ℃, filtering and drying after the reaction is finished, thus obtaining the sodium acetate trihydrate.
4. The solvothermal method for preparing M-phase vanadium dioxide according to claim 3, wherein: the molar ratio of the sodium acetate trihydrate to the vanadyl sulfate in the vanadyl sulfate solution is 2: 1.
5. the solvothermal method for preparing M-phase vanadium dioxide according to claim 3, wherein: the molar concentration of the vanadyl sulfate solution is 0.3 mol/L.
6. The solvothermal method for preparing M-phase vanadium dioxide according to any one of claims 3 to 5, wherein: when vanadyl acetate is prepared, the reaction time is 1-5 h; the drying temperature is 60 ℃ and the drying time is 12 h.
7. The solvothermal method for preparing M-phase vanadium dioxide according to claim 1, wherein: the organic solvent is one of toluene, tetrahydrofuran, dioxane, N-dimethylformamide or dimethyl sulfoxide.
8. The solvothermal method for preparing M-phase vanadium dioxide according to claim 1, wherein: the morphology regulator is oleic acid.
9. The solvothermal method for preparing M-phase vanadium dioxide according to claim 1, wherein: the reaction is carried out in a reaction kettle with a polytetrafluoroethylene lining.
10. The solvothermal method for preparing M-phase vanadium dioxide according to any one of claims 1 to 9, wherein: the granularity of the M-phase vanadium dioxide is 50-100 nm.
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| CN116102063A (en) * | 2022-12-06 | 2023-05-12 | 成都先进金属材料产业技术研究院股份有限公司 | M-phase vanadium dioxide and preparation method thereof |
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| CN116102063B (en) * | 2022-12-06 | 2024-08-02 | 成都先进金属材料产业技术研究院股份有限公司 | M-phase vanadium dioxide and preparation method thereof |
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