CN113247950B

CN113247950B - Preparation of ScVO4Method for producing powder

Info

Publication number: CN113247950B
Application number: CN202110513826.8A
Authority: CN
Inventors: 唐培松; 丁杨彬; 陈海锋; 王永亚
Original assignee: Huzhou University
Current assignee: Huzhou University
Priority date: 2021-02-25
Filing date: 2021-05-08
Publication date: 2022-04-05
Anticipated expiration: 2041-05-08
Also published as: CN113247950A

Abstract

Preparation of ScVO₄A method for preparing powder, relating to a rare earth vanadate material ScVO₄And (4) preparing. In the present invention as Sc₂O₃、NH₄VO₃And citric acid as main raw materials, and a sol-gel method is adopted to prepare ScVO₄Powder, ScVO₄Approximately spherical particles, the average grain diameter of crystal grains is about 1 mu m, and the ultraviolet light catalytic activity is excellent. The invention is ScVO₄The preparation of the powder product develops new industry, achieves the purposes of simple operation, energy conservation, high efficiency and industrialized production of ScVO₄The purpose of the powder is.

Description

Preparation of ScVO4Method for producing powder

Technical Field

The invention relates to preparation of a rare earth vanadate material, in particular to preparation of ScVO₄A method for preparing powder.

Background

S_cVO₄(scandium vanadate) is a typical Rare earth vanadate material, and as reported in the literature (Xu Shuilin et al. journal of Rare Earth, 2017, 35 (1): 28-33), the Rare earth vanadate material has good optical, magnetic and mechanical properties, excellent thermal stability, and wide application prospects in the fields of luminescent materials, catalysis, drug delivery, solar cells, laser materials and the like. Xu Shuilin et al in ScCl₃·6H₂O and NH₄VO₃As the main raw material, 0.2mmol of ScCl₃·6H₂O was dissolved in 10 mL of deionized water, and 0.2mmol of NH was added₄VO₃5mL of the solution is used to obtain a reaction solution, and the reaction solution is transferred into an autoclave with a polytetrafluoroethylene lining to react for 24 hours at 180 ℃ by a hydrothermal method; after the reaction kettle is naturally cooled to room temperature, taking out the primary product precipitate, washing the primary product precipitate with deionized water for a plurality of times, and then drying the primary product precipitate for 12 hours at the temperature of 60 ℃ to prepare ScVO₄And (5) producing the product. Literature (Limb et al spectroscopy and spectroscopy, 2020, 40(10): 3077-3080) also reported as Sc₂O₃、V₂O₅And Eu₂O₃Taking absolute ethyl alcohol as an auxiliary agent as a main raw material, weighing the raw materials according to a certain proportion, grinding to obtain a precursor, and carrying out solid-phase reaction on the precursor at the high temperature of 1000 ℃ for 3 hours to prepare ScVO₄：Eu³⁺And (4) red fluorescent powder. ScVO is obtained by carrying out hydrothermal reaction on an autoclave with a polytetrafluoroethylene lining at 180 ℃ for 24h and carrying out solid-phase reaction on the ground precursor at 1000 ℃ for 3h₄And the compound thereof has the defects of long time consumption, high energy consumption and the like, and has great industrial application prospect.

The sol-gel method generally refers to a method of synthesizing a product by solidifying a compound containing a highly chemically active component through solution, sol, gel, and then calcining and heat-treating. The sol-gel method generally has the advantages of simple industry, energy conservation, high efficiency, good product uniformity and the like. The sol-gel method has wide application in the field of material preparation, but the sol-gel method is adopted to prepare ScVO₄The powder and the research on the ultraviolet light catalytic activity of the powder are not reported.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a sol-gel method for preparing ScVO₄A method for preparing powder.

The invention is realized by the following technical scheme, and the specific steps are as follows:

(1) 0.005mol of Sc is added at room temperature under stirring₂O₃Dissolving in 3.0ml of concentrated nitric acid, and adding 17.0ml of distilled water to obtain a solution A; adding 0.01mol of NH₄VO₃Dissolved in 5.0ml of concentrated ammonia water, and then 15.0ml of distilled water was added to obtain solution B.

(2) Slowly adding 20.0ml of the solution A to 20.0ml of the solution B under stirring, and then adding a certain amount of citric acid to ensure that the citric acid is mixed with the Sc³⁺The mass ratio of the substances is 1.1: 1 to 1.6: 1, the solution is heated to 60 ℃ and continuously stirred for 20min to obtain reaction liquid.

(3) Adjusting the pH value of the reaction solution to 8.5-9.5 by using 0.1mol of dilute nitric acid, continuously stirring for 20-30 min to obtain sol, and putting the sol into a drying oven at 100 ℃ for reacting for 6h to obtain gel; and putting the dried gel into a muffle furnace to calcine for 2 to 5 hours at the temperature of between 700 and 800 ℃.

(4) After the muffle furnace is cooled to room temperature, taking out the product to obtain ScVO₄And (3) powder.

The invention has the positive effects that: preparing ScVO by adopting a sol-gel method₄The powder product is ScVO₄The preparation of the powder product develops new industry, achieves the purposes of simple operation, energy conservation, high efficiency and industrialized production of ScVO₄The purpose of the powder is.

Drawings

FIG. 1: ScVO obtained in example 1₄XRD pattern of the product;

FIG. 2: ScVO obtained in example 1₄Scanning electron microscope photographs of the products;

FIG. 3: ScVO obtained in example 1₄The change curve of the degradation rate of the product for photocatalytic degradation of methyl orange along with time.

Detailed Description

Example 1

0.005mol of Sc is added at room temperature under stirring₂O₃Dissolving in 3.0ml of concentrated nitric acid, and adding 17.0ml of distilled water to obtain a solution A; adding 0.01mol of NH₄VO₃Dissolved in 5.0ml of concentrated ammonia water, and then 15.0ml of distilled water was added to obtain solution B. Slowly adding 20.0ml of the solution A to 20.0ml of the solution B under stirring, and then adding a certain amount of citric acid to ensure that the citric acid is mixed with the Sc³⁺The mass ratio of the substances is 1.1: 1, the solution is heated to 60 ℃ and continuously stirred for 20min to obtain reaction liquid. Adjusting the pH value of the reaction solution to 9.0 by using 0.1mol of dilute nitric acid, continuously stirring for 20min to obtain sol, and putting the sol into a drying oven at 100 ℃ for reacting for 6h to obtain gel; the dried gel is put into a muffle furnace to be calcined for 2h at 750 ℃, and after the muffle furnace is cooled to room temperature, the product is taken out to obtain ScVO₄And (3) powder. The obtained product was subjected to X-ray diffraction (XRD) analysis and Scanning Electron Microscope (SEM) test, respectively, and the results are shown in fig. 1 and 2.

FIG. 1 is an XRD pattern obtained by analyzing and measuring a product by a powder method. As can be seen from FIG. 1, the XRD diffraction peak of the obtained product is consistent with that of standard ScVO₄The diffraction peaks of (PDF #74-1945) were completely coincident, indicating that the product was ScVO₄。

FIG. 2 is a scanning electron micrograph of the product obtained by the scanning electron microscopy test of Hitachi S-3400N. As can be seen from FIG. 2, ScVO₄The product is similar to spherical particles, mainly particles with the average grain diameter of about 1 mu m exist, the grains are slightly agglomerated, but the overall uniformity is good.

To characterize ScVO₄The photocatalytic activity of the powder, the photocatalytic experiment is carried out in a self-made photocatalytic reaction device: the light source was a 150W ultraviolet high-pressure mercury lamp, and 20mg of ScVO was added₄Adding the powder into a simulated sewage methyl orange solution of 20mg/L for 5min in a dark place, and carrying out a photocatalytic degradation experiment; the resulting solution was centrifuged to remove the powder after the time required for degradation, and the absorbance of the centrifuged clear solution was measured with an ultraviolet-visible spectrophotometer (λ 464nm) to obtain ScVO₄The degradation rate of methyl orange is shown in FIG. 3. As can be seen from FIG. 3, ScVO was observed for the first 30min of the photocatalytic reaction₄The photocatalytic degradation rate of methyl orange is high; in the range of 30min to 60min, the photocatalytic degradation rate is slowed, but after 60min of photocatalytic reaction, the degradation rate of methyl orange reaches 99.2%, which shows that ScVO₄Has excellent ultraviolet light catalytic degradation activity on methyl orange.

Example 2

0.005mol of Sc is added at room temperature under stirring₂O₃Dissolving in 3.0ml of concentrated nitric acid, and adding 17.0ml of distilled water to obtain a solution A; adding 0.01mol of NH₄VO₃Dissolved in 5.0ml of concentrated ammonia water, and then 15.0ml of distilled water was added to obtain solution B. Slowly adding 20.0ml of the solution A to 20.0ml of the solution B under stirring, and then adding a certain amount of citric acid to ensure that the citric acid is mixed with the Sc³⁺The mass ratio of the substances is 1.6: 1, the solution is heated to 60 ℃ and continuously stirred for 20min to obtain reaction liquid. Adjusting the pH value of the reaction solution to 9.5 by using 0.1mol of dilute nitric acid, continuously stirring for 30min to obtain sol, and putting the sol into a drying oven at 100 ℃ for reacting for 6h to obtain gel; the dried gel is put into a muffle furnace to be calcined for 5 hours at 700 ℃, and after the muffle furnace is cooled to room temperature, the product is taken outScVO₄And (3) powder. ScVO was prepared according to the same photocatalytic experiment as in example 1₄When 20mg/L methyl orange solution is degraded in a photocatalytic manner for 60min, the degradation rate of methyl orange reaches 99.5 percent, and ScVO₄Has excellent ultraviolet light catalytic degradation activity on methyl orange.

Example 3

0.005mol of Sc is added at room temperature under stirring₂O₃Dissolving in 3.0ml of concentrated nitric acid, and adding 17.0ml of distilled water to obtain a solution A; adding 0.01mol of NH₄VO₃Dissolved in 5.0ml of concentrated ammonia water, and then 15.0ml of distilled water was added to obtain solution B. Slowly adding 20.0ml of the solution A to 20.0ml of the solution B under stirring, and then adding a certain amount of citric acid to ensure that the citric acid is mixed with the Sc³⁺The mass ratio of the substances is 1.4: 1, the solution is heated to 60 ℃ and continuously stirred for 20min to obtain reaction liquid. Adjusting the pH value of the reaction solution to 8.5 by using 0.1mol of dilute nitric acid, continuously stirring for 20min to obtain sol, and putting the sol into a drying oven at 100 ℃ for reacting for 6h to obtain gel; the dried gel is put into a muffle furnace to be calcined for 2h at 800 ℃, and after the muffle furnace is cooled to room temperature, the product is taken out to obtain ScVO₄And (3) powder. ScVO was prepared according to the same photocatalytic experiment as in example 1₄When 20mg/L methyl orange solution is degraded in a photocatalytic manner for 60min, the degradation rate of methyl orange reaches 99.3%, and ScVO₄Has excellent ultraviolet light catalytic degradation activity on methyl orange.

Claims

1. Preparation of ScVO₄A method for producing a powder, characterized by comprising the step of (1) mixing 0.005mol of Sc at room temperature with stirring₂O₃Dissolving in 3.0ml of concentrated nitric acid, and adding 17.0ml of distilled water to obtain a solution A; adding 0.01mol of NH₄VO₃Dissolving in 5.0ml of concentrated ammonia water, and adding 15.0ml of distilled water to obtain a solution B; (2) slowly adding 20.0ml of the solution A into the 20.0mlB solution under the condition of stirring, then adding a certain amount of citric acid, heating the solution to 60 ℃, and continuously stirring for 20min to obtain a reaction solution; (3) adjusting the pH of the reaction solution by using 0.1mol of dilute nitric acid, continuously stirring for 20-30 min to obtain sol, and putting the sol into a drying oven at 100 ℃ for reacting for 6h to obtain gel; mixing the xerogelCalcining the mixture for 2 to 5 hours at the temperature of between 700 and 800 ℃ in a muffle furnace; (4) after the muffle furnace is cooled to room temperature, taking out the product to obtain ScVO₄And (3) powder.

2. ScVO according to claim 1₄The sol-gel preparation method of the powder is characterized in that when citric acid is added into the solution, the citric acid and Sc are controlled to be³⁺The ratio of the amounts of the substances is in the range from 1.1: 1 to 1.6: 1.

3. ScVO according to claim 1₄The sol-gel preparation method of the powder is characterized in that the pH of a reaction solution is controlled to be 8.5-9.5.