CN101774637A

CN101774637A - Method for preparing self-assembly Bi12TiO20 micro-spheres by solution method

Info

Publication number: CN101774637A
Application number: CN200910228694A
Authority: CN
Inventors: 侯军刚; 曲远方
Original assignee: Tianjin University
Current assignee: Tianjin University
Priority date: 2009-11-25
Filing date: 2009-11-25
Publication date: 2010-07-14

Abstract

The invention relates to a method for preparing self-assembly Bi12TiO20 micro-spheres by a solution method, and belongs to preparation technology of a photocatalytic material. The method comprises the following steps: mixing bismuth nitrate and tetraethyl titanate in a molar ratio of 0.6-0.8 to 0.4-0.2, adding deionized water into the mixture, and adjusting the pH of solution by using potassium hydroxide; dripping solution of polyvinyl alcohol into the prepared solution, and stirring and performing ultrasonic dispersion to obtain solution of precursor; transferring the solution of precursor to a reaction kettle, adding the deionized water into the reaction kettle, and performing reaction for 36 to 60 hours at the temperature of between 140 and 200 DEG C; separating out a product from reactants by adopting a centrifugal separator, washing the product with the deionized water and drying the washed product to obtain the self-assembly Bi12TiO20 micro-spheres. The method has the advantages that: the preparation process is simple; and the prepared Bi12TiO20 micro-spheres have excellent photocatalytic performance under the condition of visible light.

Description

Solution method self-assembly Bi 12TiO 20The preparation method of micron ball

Technical field

The present invention relates to a kind of solution method self-assembly Bi ₁₂TiO ₂₀The preparation method of micron ball belongs to the technology of preparing of photocatalyst material.

Background technology

TiO ₂As semiconductor light-catalyst, very extensive studies and application have been obtained at aspects such as environmental pollution treatment technology and illumination hydrolytic hydrogen productions.Bi ₁₂TiO ₂₀Also has the feature of semiconductor light-catalyst Deng the bismuth titanates based compound, wherein Bi ₁₂TiO ₂₀Photocatalytic activity the strongest, reached the activity [W.F.Yao, H.Wang, X.H.Xu, X.F.Cheng, J.Huang, S.X.Shang, X.N.Yang, M.Wang, Appl.Catal.A.2003,243,185] identical with P-25.Human chemical solution deposition reported first such as Yao Bi ₁₂TiO ₂₀Crystal in ultraviolet light range to the photocatalysis performance of methyl orange solution and made the research [W.F.Yao of doping vario-property, H.Wang, X.H.Xu, Y.Zhang, X.N.Yang, S.X.Shang, Y.H.Liu, J.T.Zhou, M.Wang, Journal of Molecular Catalysis A:Chemical 202 (2003) 305-311], but Bi ₁₂TiO ₂₀The photocatalysis performance of nano-powder still is confined in the ultraviolet light range.The synthetic Bi of humans such as Zhou tradition solid sintering technology ₁₂TiO ₂₀And photocatalysis performance [J.K.Zhou, Z.G.Zou, A.K.Ray, X.S.Zhao have been showed in visible-range to methyl alcohol, Ind.Eng.Chem.Res.2007,46,745], although the application to visible-range has had expansion, on traditional solid sintering technology, Bi ₁₂TiO ₂₀The particle size that the powder micron order is bigger has influenced its photocatalysis performance greatly.

Summary of the invention

The purpose of this invention is to provide a kind of solution method self-assembly Bi ₁₂TiO ₂₀The preparation method of micron ball, this procedure is simple, prepared Bi ₁₂TiO ₂₀The micron ball has good photocatalysis performance under the visible light condition.

The present invention is realized by the following technical programs, a kind of solution method self-assembly Bi ₁₂TiO ₂₀The preparation method of micron ball is characterized in that comprising following process:

1. press Bismuth trinitrate (Bi (NO ₃) ₃5H ₂O) with tetraethyl titanate (Ti (OC ₃H ₇) ₄) mol ratio be (0.6-0.8): (0.4-0.2), take by weighing Bismuth trinitrate (Bi (NO ₃) ₃5H ₂O) and tetraethyl titanate (Ti (OC ₃H ₇) ₄) prepare burden, add the deionized water of 5-30ml by every mole of batching, batching is dissolved in the deionized water, stirred 10-50 minute, reach 10-14 with the pH value of potassium hydroxide (KOH) regulator solution;

2. in the solution that step 1 makes, the mass concentration that drips 0.075-0.15mmol by every mole of batching is the polyvinyl alcohol solution of 10-30%, gets precursor solution through stirring 10-50 minute, and precursor solution is again through ultra-sonic dispersion 10-50 minute;

3. the precursor solution that step 2 is made is transferred in the teflon-lined reactor, adding deionized water again, to make the compactedness of reaction vessel be 60-80%, the temperature of reaction of precursor solution is 140-200 ℃, reaction times is 36-60 hour, and question response finishes, and adopts the separating centrifuge of the rotating speed of 1500-3000rpm, from reactant, isolate product, separated products is used deionized water rinsing again, dries under 60-100 ℃ of condition then, obtains the Bi of self-assembly ₁₂TiO ₂₀The micron ball.

The invention has the advantages that preparation process is simple, prepared Bi ₁₂TiO ₂₀The micron ball has good photocatalysis performance under the visible light condition.

Embodiment

Take by weighing 0.80mol Bismuth trinitrate (Bi (NO ₃) ₃5H ₂O) and 0.20mol tetraethyl titanate (Ti (OC ₃H ₇) ₄), it is dissolved in the 10ml deionized water, stirred 30 minutes, regulate the pH value 14 with potassium hydroxide (KOH), drip 0.125mmol polyvinyl alcohol solution (mass concentration is 17.5%) afterwards, precursor solution was stirred 30 minutes, again with its solution ultra-sonic dispersion 30 minutes.Solution is transferred in the teflon-lined reactor afterwards, adding deionized water again, to make the compactedness of reaction vessel be 80%.The temperature of reaction of control presoma is 150 ℃, reaction times is 48 hours, and question response finishes, and product separates (velocity of separation 3000rpm), deionized water rinsing separated product 3 times with separating centrifuge from reactant, through 80 ℃ of oven dry, can obtain the Bi of high catalytic performance again ₁₂TiO ₂₀The micron ball.

Claims

1. solution method self-assembly Bi ₁₂TiO ₂₀The preparation method of micron ball is characterized in that comprising following process:

1) mol ratio of pressing Bismuth trinitrate and tetraethyl titanate is (0.6-0.8): (0.4-0.2), take by weighing Bismuth trinitrate and tetraethyl titanate is prepared burden, the deionized water that adds 5-30ml by every mole of batching, batching is dissolved in the deionized water, stirred 10-50 minute, and reached 10-14 with the pH value of potassium hydroxide regulator solution;

2) in the solution that step 1) makes, the mass concentration that drips 0.075-0.15mmol by every mole of batching is the polyvinyl alcohol solution of 10-30%, gets precursor solution through stirring 10-50 minute, and precursor solution is again through ultra-sonic dispersion 10-50 minute;

3) with step 2) precursor solution that makes transfers in the teflon-lined reactor, adding deionized water again, to make the compactedness of reaction vessel be 60-80%, the temperature of reaction of precursor solution is 140-200 ℃, reaction times is 36-60 hour, and question response finishes, and adopts the separating centrifuge of the rotating speed of 1500-3000rpm, from reactant, isolate product, separated products is used deionized water rinsing again, dries under 60-100 ℃ of condition then, obtains the Bi of self-assembly ₁₂TiO ₂₀The micron ball.