CN102583535A

CN102583535A - Method for synthesizing bismuth vanadate by phonochemistry

Info

Publication number: CN102583535A
Application number: CN2012100599447A
Authority: CN
Inventors: 黄剑锋; 孟岩; 曹丽云; 张振伟; 吴建鹏; 费杰; 辛宇
Original assignee: Shaanxi University of Science and Technology
Current assignee: Shaanxi University of Science and Technology
Priority date: 2012-03-07
Filing date: 2012-03-07
Publication date: 2012-07-18

Abstract

A method for synthesizing bismuth vanadate by phonochemistry comprises the steps as follows: Bi(NO3)3.5H2O and NH4VO3 are respectively resolved into HNO3 solution and hot water; the two solutions are mixed and then are stirred uniformly on a magnetic stirrer, and the pH value of the mixed solution is adjusted to range from 3 to 9 by NaOH solution so as to obtain yellow turbid liquid; and the prepared yellow turbid liquid is placed in an ultrasonic generator, and after reaction, products are subjected to centrifugal separation, are respectively washed by deionized water and absolute ethyl alcohol and finally are vacuumized, so that the bright-yellow powdered bismuth vanadate is obtained. As the method adopts the simple phonochemistry preparation process, a reaction period is short, energy consumption is low, the operation is convenient, the prepared bismuth vanadate has the advantages of being small in particle size and uniform in size and morphology, according to the Scherrer formula, the particle size of the prepared bismuth vanadate is 18.6 nm and is less than the particle size (namely 41nm) of bismuth vanadate prepared by zhou, and along with the reduction of the particle size, a contact area between the bismuth vanadate and a reactant is enlarged, so that a photochemical catalysis rate is enhanced greatly.

Description

The method of the synthetic pucherite of a kind of sonochemistry

Technical field

The invention belongs to the preparation method of pucherite, be specifically related to the method for the synthetic pucherite of a kind of sonochemistry.

Background technology

In the last few years, environmental pollution and energy dilemma had been brought serious threat to human existence, and photocatalysis technology has obtained to pay close attention to widely as a kind of new technique.Use photocatalyst such as titanium oxide (TiO the most widely at present ₂) etc., be the wide band gap semiconducter catalyzer, only have corresponding in ultraviolet light range.Sunshine medium ultraviolet light is less than 5%, and that visible light accounts for is nearly 43%, therefore develops the corresponding high-activity photocatalyst of visible light and be that to improve solar energy utilization ratio be the photocatalysis technology Development Trend.

Pucherite also has photocatalytic simultaneously, pastes characteristics such as elasticity, acousto-optic transformant, particle conductive property as a kind of lead-free inorganic yellow dyestuff, has been applied to the research of degradation of contaminant, photodissociation aquatic products oxygen and photoelectrochemistry water of decomposition at present.

The method that prepare at present pucherite mainly contain chemical precipitation method [Gao Shanmin, Qiao Qingan, Zhao Peipei, Tao Furong, Zhangjiang is worn beautiful jade, golden cypress is marked. the precipitator method prepare the nanometer BiVO4 [J] of different-shape and structure. Chinese Journal of Inorganic Chemistry, 2007; 23 (7): 1153-1158], low-temperature solid-phase method [Shenmue loud, high-pitched sound; Hou Xiaohu; Na Ren figure is refined, Li Jinmei, Zhao Zhihong. and combustion method prepares nanometer bismuth vanadate powder and performance [J]. non-ferrous metal (smelting part); 2011 (6): 45-49.], hydrothermal method [Yang T; Xia D, Chen G, Chen Y. Influence of the surfactant and temperature on the morphology and physico-chemical properties of hydrothermally synthesized composite oxide BiVO ₄[J] .Materials Chemistry and Physics.2009; 114 (1): 69-72.], microemulsion method [Chung C-Y, Lu C-H.Reverse-microemulsion preparation of visible-light-driven nano-sized BiVO4 [J] .Journal of Alloys and Compounds.2010; 502 (1): L1-L5.].Yet the pucherite size heterogeneity of these method preparations perhaps needs the long reaction times and bigger for environmental pollution.Therefore seek a kind of ease of Use, environmental friendliness and reaction times, short method seemed rather important.

Though ultrasonic method [Zhou L; Wang W, Liu S, Zhang L; Xu H, Zhu W. A sonochemical route to visible-light-driven high-activity BiVO4 photocatalyst.Journal of Molecular Catalysis A:Chemical.2006; 252 (1-2): 120-4.] existing research, but the crystal grain of this method preparation is bigger, and its product contact area in degraded is little, and the photochemical catalysis rate is lower.

Summary of the invention

The purpose of this invention is to provide the method that a kind of sonochemistry legal system is equipped with pucherite.This preparation method reaction time is short, temperature of reaction is low, environmental friendliness, with low cost, and simple to operate, does not need later stage thermal treatment, good reproducibility, and prepared pucherite particle size is little, size pattern homogeneous.

For achieving the above object, the technical scheme that the present invention adopts is:

1) with the Bi (NO of 0.002-0.02mol ₃) ₃5H ₂The NH of O and 0.002-0.02mol ₄VO ₃According to Bi: V=1: 1 mole proportioning is dissolved in the HNO of 10ml respectively ₃In 80 ℃ of hot water of solution and 20ml;

2) after two kinds of solution mixing with the step 1) preparation, on magnetic stirring apparatus, stir, use NaOH solution to regulate pH then and be 3-9, make yellow suspension liquid;

3) the yellow suspension liquid with above-mentioned preparation places ultrasonic generator, and setting ultrasonic power is 400-700W, and temperature of reaction is 30-90 ℃, reaction 30-120min;

4) after question response is accomplished,, and, use absolute ethanol washing 1-2 time again,, obtain the Powdered vanadic acid bismuth of glassy yellow at last 50-80 ℃ of following vacuum-drying with behind deionized water wash 3-5 time with the product spinning.

Described HNO ₃The concentration of solution is 2-5mol/L.

The concentration of described NaOH solution is 2-10mol/L.

The present invention adopts simple sonochemistry method preparation technology, and reaction time is short, and energy consumption is low; Easy to operate, the pucherite that makes has that particle size is little, the characteristics of size pattern homogeneous, is 18.6nm according to Scherrer formula calculation result; Than [Zhou L; Wang W, Liu S, Zhang L; Xu H, Zhu W. A sonochemical route to visible-light-driven high-activity BiVO4 photocatalyst.Journal of Molecular Catalysis A:Chemical.2006; 252 (1-2): 120-4.] little grain-size reduces more than one times for the pucherite grain-size (41nm) of preparation, then increases with the reactant contact area, has greatly promoted the photochemical catalysis rate.

Description of drawings

Fig. 1 prepares (XRD) collection of illustrative plates of pucherite particle for the present invention, and wherein X-coordinate is diffraction angle 2 θ, and unit is °; Ordinate zou is a diffraction peak intensity, and unit is a.u.

Embodiment

Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.

Embodiment 1:

1) with the Bi (NO of 0.002mol ₃) ₃.5H ₂The concentration that O is dissolved in 10ml is the HNO of 2mol/L ₃In the solution, with the NH of 0.002mol ₄VO ₃Be dissolved in 80 ℃ of hot water of 20ml;

2) two kinds of solution of step 1) preparation are mixed after, on magnetic stirring apparatus, stir 30min, be that the NaOH solution adjusting pH of 2mol/L is 3 with concentration then, make yellow suspension;

3) the yellow suspension liquid with above-mentioned preparation places ultrasonic generator, and setting ultrasonic power is 400W, and temperature of reaction is 30 ℃, reaction 30min;

4) after question response is accomplished,, and, use absolute ethanol washing again 1 time,, obtain the Powdered vanadic acid bismuth of glassy yellow at last 50 ℃ of following vacuum-dryings with behind the deionized water wash 3 times with the product spinning.

Embodiment 2:

1) with the Bi (NO of 0.008mol ₃) ₃5H ₂The concentration that O is dissolved in 10ml is the HNO of 3mol/L ₃In the solution, with the NH of 0.008mol ₄VO ₃Be dissolved in 80 ℃ of hot water of 20ml;

2) two kinds of solution of step 1) preparation are mixed after, on magnetic stirring apparatus, stir 40min, be that the NaOH solution adjusting pH of 5mol/L is 5 with concentration then, make yellow suspension;

3) the yellow suspension liquid with above-mentioned preparation places ultrasonic generator, and setting ultrasonic power is 500W, and temperature of reaction is 50 ℃, reaction 60min;

4) after question response is accomplished,, and, use absolute ethanol washing again 1 time,, obtain the Powdered vanadic acid bismuth of glassy yellow at last 60 ℃ of following vacuum-dryings with behind the deionized water wash 4 times with the product spinning.

Embodiment 3:

1) with the Bi (NO of 0.014mol ₃) ₃5H ₂The concentration that O is dissolved in 10ml is the HNO of 4mol/L ₃In the solution, with the NH of 0.014mol ₄VO ₃Be dissolved in 80 ℃ of hot water of 20ml;

2) two kinds of solution of step 1) preparation are mixed after, on magnetic stirring apparatus, stir 50min, be that the NaOH solution adjusting pH of 8mol/L is 7 with concentration then, make yellow suspension;

3) the yellow suspension liquid with above-mentioned preparation places ultrasonic generator, and setting ultrasonic power is 600W, and temperature of reaction is 70 ℃, reaction 90min;

4) after question response is accomplished,, and, use absolute ethanol washing again 2 times,, obtain the Powdered vanadic acid bismuth of glassy yellow at last 70 ℃ of following vacuum-dryings with behind the deionized water wash 4 times with the product spinning.

Embodiment 4:

1) with the Bi (NO of 0.02mol ₃) ₃5H ₂The concentration that O is dissolved in 10ml is the HNO of 5mol/L ₃In the solution, with the NH of 0.02mol ₄VO ₃Be dissolved in 80 ℃ of hot water of 20ml;

2) two kinds of solution of step 1) preparation are mixed after, on magnetic stirring apparatus, stir 60min, be that the NaOH solution adjusting pH of 10mol/L is 9 with concentration then, make yellow suspension;

3) the yellow suspension liquid with above-mentioned preparation places ultrasonic generator, and setting ultrasonic power is 700W, and temperature of reaction is 90 ℃, reaction 120min;

4) after question response is accomplished,, and, use absolute ethanol washing again 2 times,, obtain the Powdered vanadic acid bismuth of glassy yellow at last 80 ℃ of following vacuum-dryings with behind the deionized water wash 5 times with the product spinning.

With gained obtain glassy yellow powdery product pucherite with Japanese D/max2000PCX-x ray diffraction analysis x sample of science, find that product gained collection of illustrative plates is the diffraction peak of pucherite, see Fig. 1.

Claims

1. the method for the synthetic pucherite of a sonochemistry is characterized in that:

2. the method for the synthetic pucherite of sonochemistry according to claim 1 is characterized in that: described HNO ₃The concentration of solution is 2-5mol/L.

3. the method for the synthetic pucherite of sonochemistry according to claim 1, it is characterized in that: the concentration of described NaOH solution is 2-10mol/L.