CN112266018A - Method for preparing nano vanadium dioxide by reverse hydrolysis precipitation - Google Patents
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Abstract
The invention belongs to the technical field of vanadium dioxide preparation, and particularly relates to a method for preparing nano vanadium dioxide by reverse hydrolysis precipitation. Aiming at the problem that the existing chemical precipitation method for preparing vanadium dioxide is difficult to obtain the nano vanadium dioxide with high crystallinity, good uniformity and small granularity, the invention provides a method for preparing the nano vanadium dioxide by reverse hydrolysis precipitation, which comprises the following steps: a. taking a sodium hydroxide solution, and dropwise adding a tetravalent vanadium solution while stirring until the pH value of the solution is 7-8.5; b. centrifuging, washing, drying and grinding to obtain precursor powder; c. adding an ethanol solution, carrying out hydrothermal reaction for 12-24 h, cooling to room temperature, centrifuging, and separating to obtain M-phase VO2And (3) powder. The method has the advantages of simple process, convenient operation and low preparation cost, and can rapidly prepare a large amount of vanadium dioxide and VO2The method has the advantages of high purity, uniform particle size distribution and good crystallinity, and can be widely applied to the fields of intelligent windows, photoelectric switches, thermistors and the like.
Description
Technical Field
The invention belongs to the technical field of vanadium dioxide preparation, and particularly relates to a method for preparing nano vanadium dioxide by reverse hydrolysis precipitation.
Background
Chemical precipitation and hydrothermal method are two most commonly used methods for preparing nano powder liquid phase, the chemical precipitation mainly adopts tetravalent vanadium source, under the action of precipitant, hydrolytic precipitation is carried out to obtain vanadyl hydroxide or basic vanadyl carbonate precursor, then the precursor is crystallized to obtain target product, the crystallization mode mainly has two, one is through high temperature heat treatment, often has the problems of high energy consumption, product sintering and poor uniformity; the other is hydrothermal crystallization, and the nano powder with uniform granularity and good crystallinity can be prepared by utilizing the advantages of hydrothermal reaction, but in the process, the dispersibility and the uniformity of the precursor determine the dispersibility and the uniformity of the final product to a great extent. Therefore, how to simply and rapidly prepare the precursor with narrow particle size distribution and good dispersibility is very important. The hydrothermal method usually uses vanadium pentoxide as a raw material, adds a reducing agent, and prepares vanadium dioxide through reduction reaction in a high-temperature and high-pressure aqueous solution, and the biggest problem of the method is that the particle size of the prepared product is large when the concentration of the vanadium solution is high, and the yield of the product is extremely low when the concentration of the vanadium solution is low. In addition, the method also has the problems of excessive reduction to generate vanadium trioxide and higher requirement on the purity of the reducing agent.
Patent CN101734720A discloses a method for preparing vanadium dioxide ultrafine powder, which proposes to adopt N2H4Reducing 2HCl and oxalic acid in a hydrochloric acid medium to prepare a vanadyl dichloride solution, adding ammonium bicarbonate into the vanadyl dichloride solution, hydrolyzing to prepare a basic vanadyl ammonium carbonate precursor, ultrasonically crushing the basic vanadyl ammonium carbonate precursor to less than 2 microns, and then placing the precursor in a nitrogen atmosphere furnace to be heated and decomposed to obtain vanadium dioxide powder. The method adopts the idea of chemical precipitation-high temperature heat treatment, and the problems of partial powder melting, serious local agglomeration and poor uniformity in the heat treatment process can not be changed although the precursor is crushed in the ultrasonic treatment; meanwhile, the method also has the problem of high energy consumption because the method relates to high-temperature heat treatment.
Patent 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): and (1) 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 the reaction product to obtain the 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. Although tetravalent vanadium is adopted as a vanadium source, the method does not relate to a hydrolysis precipitation process, but is a solvothermal method, and the general solvothermal method has the defects of high cost of an organic solvent, great harm to human bodies and the environment, small yield and unsuitability for industrial application.
Patent CN101391814A discloses a method for preparing rutile phase vanadium dioxide powder, which comprises adding 1-10% (mole percentage of dopant and vanadium ion) of dopant into vanadyl sulfate, vanadyl oxalate or vanadyl dichloride solution with vanadium ion concentration of 0.05-1.5M, transferring the solution into a hydrothermal reaction kettle, and reacting at 200-300 ℃ for 1-7 days. The method omits the preparation of a precursor, directly crystallizes the vanadium dioxide from the solution in one step, has a long reaction period although the process is simple, and simultaneously the particle size of the product can overgrow to reach micron level, so that the method is not suitable for popularization and application.
Therefore, at present, no method for preparing a precursor with good dispersibility and uniformity so as to obtain the nano vanadium dioxide with high crystallinity, good uniformity and small particle size exists, and the development is urgently needed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing chemical precipitation method for preparing vanadium dioxide has the problem that the nanometer vanadium dioxide with high crystallinity, good uniformity and small granularity is difficult to obtain because the dispersibility and the uniformity are difficult to control in the preparation of a precursor.
The technical scheme for solving the technical problems comprises the following steps: provides a method for preparing nano vanadium dioxide by reverse hydrolysis precipitation. The method comprises the following steps:
a. taking a sodium hydroxide solution with the concentration of 300-600 g/L, and dropwise adding a tetravalent vanadium solution into the sodium hydroxide solution under rapid stirring until the pH value of the solution is 7-8.5;
b. centrifuging the solution obtained in the step a, alternately washing the solution for 6 times by using deionized water and absolute ethyl alcohol to obtain a solid product, drying the solid product in vacuum at 60 ℃ for 12 hours, and grinding the dried solid product to obtain precursor powder;
c. taking the precursor powder prepared in the step b, adding the precursor powder into an ethanol solution with the volume fraction of 50% according to the liquid-solid ratio of 60-90: 0.5-5, carrying out hydrothermal reaction at the temperature of 200-260 ℃ for 12-24 h, cooling to room temperature after the reaction is finished, centrifuging, and separating to obtain M-phase VO2And (3) powder.
In the method for preparing the nano vanadium dioxide by reverse hydrolysis precipitation, the temperature of the solution is kept at 20-30 ℃ in the dropping process in the step a.
Wherein, in the method for preparing nano vanadium dioxide by reverse hydrolysis precipitation, the tetravalent vanadium solution in the step a comprises VOSO4、VOC2O4Or VOCl2At least one of (1).
In the method for preparing the nano vanadium dioxide by reverse hydrolysis precipitation, the centrifugal rotating speed in the step b is 10000-15000 rpm.
The invention has the beneficial effects that:
the invention provides a method for preparing nano vanadium dioxide by reverse hydrolysis precipitation, which changes the adding sequence of precipitation reaction solution in the reaction process, so that the prepared precursor has smaller particle size and better dispersibility. The particle size is changed from the original micron level to about 200nm, and the original aggregate is changed into dispersible particles under an electron microscope. The method has the advantages of simple process, convenient operation, low preparation cost, rapid preparation of a large amount of vanadium dioxide, and easy industrial popularization and application. VO obtained by the invention2Has the advantages of high purity, uniform particle size distribution and good crystallinity, and can be widely applied to intelligent windows and photoelectric windowsAnd thermistors and the like.
Drawings
FIG. 1 shows an XRD pattern of VO2 powder obtained in example 1;
FIG. 2 is an SEM picture of VO2 powder obtained in example 1.
Detailed Description
At present, sodium hydroxide is generally added into a vanadium solution dropwise to dissolve at the initial stage of dropwise addition, but the solution is limited to the case that the pH is less than 3.5, the vanadyl precipitate grows and aggregates into molecular clusters along with the increase of the pH with the addition of a precipitant, when the pH is 7-8, the particle size of a precursor grows to a micron level, and when the concentration of vanadyl sulfate is as low as 0.1M, the average particle size of a precipitation product with the pH of 7 is more than 1 μ M.
The method particularly changes the process of precipitation reaction, the vanadium solution is dropwise added into sodium hydroxide, when the sodium hydroxide is used as a supporting solution, and the vanadium solution is dropwise added into the sodium hydroxide solution, the vanadyl precipitate generated locally can be rapidly dissolved, no precipitate can be generated in the initial process, and when the pH value is reduced to be below 8.5, the phenomenon of explosion nucleation can be generated when the pH value exceeds a critical point, so that a precursor with a smaller particle size is obtained, and the average particle size of the obtained precursor is about 200 nm. The method adopts a reverse dropwise adding mode to obtain the precursor with smaller particle size and better dispersibility, is simple to operate and is suitable for popularization and use.
Specifically, the technical scheme of the invention comprises the following specific implementation processes:
a. taking a sodium hydroxide solution with the concentration of 300-600 g/L, and dropwise adding a tetravalent vanadium solution into the sodium hydroxide solution under rapid stirring until the pH value of the solution is 7-8.5; the tetravalent vanadium solution comprises VOSO4、VOC2O4Or VOCl2At least one of;
b. centrifuging the solution obtained in the step a at the rotation speed of 10000-15000 rpm, alternately washing the solution for 6 times by using deionized water and absolute ethyl alcohol to obtain a solid product, drying the solid product at 60 ℃ for 12 hours in vacuum, and grinding the dried product to obtain precursor powder;
c. taking the precursor powder prepared in the step b,adding the mixture into 50% ethanol solution according to a liquid-solid ratio of 60-90: 0.5-5, carrying out hydrothermal reaction at 200-260 ℃ for 12-24 h, cooling to room temperature after the reaction is finished, centrifuging, and separating to obtain M-phase VO2And (3) powder.
In the method, the temperature of the solution needs to be kept at 20-30 ℃ in the dropping process in the step a, and the solution is aggregated and grown at an excessively high temperature, so that the dispersibility is influenced.
The following examples are intended to illustrate specific embodiments of the present invention without limiting the scope of the invention to the examples.
Example 1
Measuring 500ml of sodium hydroxide solution with the concentration range of 300g/L, and dropwise adding VOSO into the solution during rapid stirring4Centrifuging the solution until the pH value is 7, alternately washing the solution for 6 times by using deionized water and absolute ethyl alcohol, drying the washed solid product at 60 ℃ for 12 hours, grinding the dried solid product to obtain gray black powder, adding 0.5g of the powder into 60ml of ethanol solution with the volume fraction of 50%, placing the powder into a high-temperature high-pressure reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 24 hours, cooling the solution to room temperature after the reaction is finished, and carrying out centrifugal separation to obtain VO2And (3) powder.
FIG. 1 shows the VO2XRD pattern of the powder, which shows that the product is M phase, and FIG. 2 shows the VO2SEM image of powder.
Example 2
500ml of sodium hydroxide solution with the concentration range of 450g/L is measured, VOSO is dropwise added into the solution in the process of rapid stirring4Centrifuging the solution until the pH value is 8, alternately washing the solution for 6 times by using deionized water and absolute ethyl alcohol, drying the washed solid product at 60 ℃ for 12 hours, grinding the dried solid product to obtain gray black powder, adding 3.0g of the powder into 75ml of ethanol solution with the volume fraction of 50%, placing the powder into a high-temperature high-pressure reaction kettle, performing hydrothermal reaction at 230 ℃ for 18 hours, cooling the solution to room temperature after the reaction is finished, and performing centrifugal separation to obtain VO2And (4) obtaining a target product.
Example 3
Measuring 500ml of sodium hydroxide solution with the concentration range of 600g/L, and dropwise adding VOSO into the solution during rapid stirring4The solution is brought to pH 8.5Centrifuging, alternately washing with deionized water and anhydrous ethanol for 6 times, drying the washed solid product at 60 deg.C for 12h, grinding to obtain gray black powder, adding 5.0g of the powder into 90ml of 50% ethanol solution, placing in a high-temperature high-pressure reaction kettle, performing hydrothermal reaction at 260 deg.C for 12h, cooling to room temperature after the reaction is completed, and centrifuging to obtain VO2And (4) obtaining a target product.
From the results of the examples, it can be seen that the present invention prepares VO by reverse precipitation method only by changing the dropping mode of chemical precipitation2Determining the dropping end point to be the pH value of the solution to 7-8.5 through repeated experiments, and finally obtaining the VO2The particle size is smaller, the particle size is reduced from micron to nanometer, the dispersibility is better, the invention achieves the expected technical effect through simple experimental adjustment, and is suitable for popularization and use.
Claims (4)
1. The method for preparing the nano vanadium dioxide by reverse hydrolysis precipitation is characterized by comprising the following steps of:
a. taking a sodium hydroxide solution with the concentration of 300-600 g/L, and dropwise adding a tetravalent vanadium solution into the sodium hydroxide solution under rapid stirring until the pH value of the solution is 7-8.5;
b. centrifuging the solution obtained in the step a, alternately washing the solution for 6 times by using deionized water and absolute ethyl alcohol to obtain a solid product, drying the solid product in vacuum at 60 ℃ for 12 hours, and grinding the dried solid product to obtain precursor powder;
c. taking the precursor powder prepared in the step b, adding the precursor powder into an ethanol solution with the volume fraction of 50% according to the liquid-solid ratio of 60-90: 0.5-5, carrying out hydrothermal reaction at the temperature of 200-260 ℃ for 12-24 h, cooling to room temperature after the reaction is finished, centrifuging, and separating to obtain M-phase VO2And (3) powder.
2. The method for preparing nano vanadium dioxide by reverse hydrolysis precipitation according to claim 1, wherein: and c, keeping the temperature of the solution at 20-30 ℃ in the dropping process of the step a.
3. The reverse hydrolytic sink of claim 1The method for preparing the nano vanadium dioxide by precipitation is characterized by comprising the following steps: the tetravalent vanadium solution in the step a comprises VOSO4、VOC2O4Or VOCl2At least one of (1).
4. The method for preparing nano vanadium dioxide by reverse hydrolysis precipitation according to claim 1, wherein: and c, the rotating speed of the centrifugation in the step b is 10000-15000 rpm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113912115A (en) * | 2021-10-29 | 2022-01-11 | 广州钰芯传感科技有限公司 | Preparation method of vanadium oxide nano material and application of vanadium oxide nano material in gas sensor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113912115A (en) * | 2021-10-29 | 2022-01-11 | 广州钰芯传感科技有限公司 | Preparation method of vanadium oxide nano material and application of vanadium oxide nano material in gas sensor |
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