CN101362083B - Visible-light response nano Bi3TaO7 photocatalyst preparation method and use thereof - Google Patents

Visible-light response nano Bi3TaO7 photocatalyst preparation method and use thereof Download PDF

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CN101362083B
CN101362083B CN2008101970194A CN200810197019A CN101362083B CN 101362083 B CN101362083 B CN 101362083B CN 2008101970194 A CN2008101970194 A CN 2008101970194A CN 200810197019 A CN200810197019 A CN 200810197019A CN 101362083 B CN101362083 B CN 101362083B
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bismuth
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tao
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CN101362083A (en
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张高科
李名
杨军玲
熊茜
吕凡
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Wuhan University of Technology WUT
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Abstract

The invention relates to a preparation method of Bi3TaO7, and the application of the Bi3TaO7. The preparation method comprises the following steps: Ta2O5 is taken as raw material to prepare a hydrosoluble tantalum oxalate aqueous solution; bismuth nitrate (Bi(NO3)3 question mark 5H2O) is added into a citric acid solution and then added with a mixed solution of EDTA and stronger ammonia water so as to form the aqueous solution of bismuth, wherein, the mole ratio of bismuth irons and citric acid is 1:3-1:6; then, the tantalum oxalate aqueous solution is added into the aqueous solution of bismuth according to the composition of a mixture ratio, ammonia water is utilized for regulating the pH value to be between 7 and 8, and the obtained solution is heated and stirred under 60 DEG C to 80 DEGC so as to obtain a precursor solution of Bi3TaO7 photocatalyst which is then treated with polyesterification and is burned to decarburize and then roasted under 450 DEG C to 600 DEG C to obtain the manometer Bi3TaO7 photocatalyst. The Bi3TaO7 photocatalyst prepared by the invention has good visible-light catalytic activity and the preparation method thereof is characterized by low synthesis temperature and simple and convenient operation.

Description

Visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst and application thereof
Technical field
The present invention relates to Bi 3TaO 7Preparation method and Bi 3TaO 7Application.
Background technology
In recent years, the photocatalyst treatment Dyeing Wastewater has become a domestic research focus.But most researchs mainly concentrate on TiO 2And on the titanate, yet because it has higher energy gap, general only have absorption for ultraviolet light, limited extensive use for it, therefore, develop one the hot issue that a kind of novel photochemical catalyst that can have the high light catalytic activity under visible light has become photocatalysis field.And recently for over ten years, a series of niobiums (tantalum) hydrochlorate photochemical catalyst is widely studied owing to it has higher photocatalytic activity.For example, a series of niobate photocatalyst Pb 3Nb 4O 13, BiNbO 4And Bi 2MNbO 7(M=Al, Ga, In, Y, rare earth metal, Fe) grade and niobium potassium compound oxide photocatalyst such as KNbO 3, KNb 3O 8, K 4Nb 6O 17And K 6Nb 10.8O 30Or the like photocatalytic activity is widely studied because of having preferably.Kudo and Kato have studied a series of tantalates, alkali-metal tantalates ATaO 3The tantalates photochemical catalyst BTa of (A=Li, Na and K), alkaline-earth metal 2O 6(B=Ca, Sr and Ba), these photochemical catalysts have the TiO of ratio 2Higher photocatalysis effect.The InTaO of huebnerite type 4And InNbO 4The oxide semiconductor photochemical catalyst has higher photocatalytic activity under visible light.Yet; the preparation of niobium (tantalum) hydrochlorate photochemical catalyst at present mainly is to adopt traditional solid phase method to send out and should obtain by long sintering under higher temperature; but because of raw material difficulty mix; the reaction temperature height; reaction is difficult for carrying out fully, so the powder granule of preparing is bigger, and skewness; the crystal that usually is mixed with dephasign and often preparation has defective, and these two aspects make the photocatalytic activity of the photochemical catalyst that solid phase method is synthetic reduce.
Summary of the invention
The object of the present invention is to provide the high visible-light response nano Bi of a kind of photocatalytic activity 3TaO 7The preparation method of photochemical catalyst and application thereof, this method have synthesis temperature characteristics lower, easy and simple to handle.
To achieve these goals, technical scheme of the present invention is: visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst is characterized in that it comprises the steps:
1) presses Ta 2O 5Choose Ta with the mol ratio 1: 2～20 of potassium hydroxide 2O 5And potassium hydroxide, standby;
With Ta 2O 5Even with the potassium hydroxide mixed grinding, put into corundum crucible, at 400～500 ℃ of following calcination 2～4h, obtain the melt of potassium tantalate; Press Ta 2O 5With the mass ratio of deionized water be 1: 20～100, choose deionized water, the melt of potassium tantalate is dissolved in deionized water, filter, with the clear liquid after filtering, add nitric acid and make solution be highly acid (pH＜2), make tantalum in the solution fully with tantalic acid (Ta 2O 5NH 2O) form is precipitated out, and gets sediment; With deionized water rinsing to remove the potassium ion of the remnants that adsorb on the sediment; Obtain the tantalic acid sediment;
2) the tantalic acid sediment that obtains is added oxalic acid, and constantly stir, promptly obtain the water miscible tantalum oxalate aqueous solution; Wherein the quality proportioning of tantalic acid sediment and oxalic acid is 1: 1～10;
3) by tantalum ion and five water bismuth nitrate (Bi (NO in the tantalum oxalate aqueous solution 3) 35H 2O) mol ratio is 1: 3, chooses the tantalum oxalate aqueous solution and five water bismuth nitrates, and is standby;
Mol ratio by Bi in the five water bismuth nitrates and citric acid is 1: 3～1: 6, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent EDTA (ethylenediamine tetra-acetic acid) is 1:1.8～1:6, chooses chelating agent EDTA (ethylenediamine tetra-acetic acid), and is standby;
Bismuth nitrate is joined in the citric acid solution of 0.3～0.7mol/L, stir down in 60～80 ℃, the mixed solution that adds chelating agent EDTA (ethylenediamine tetra-acetic acid) and ammoniacal liquor, chelating agent EDTA (ethylenediamine tetra-acetic acid) is 12～16g:20ml with the proportioning of ammoniacal liquor in the mixed solution; Dissolve the solution that forms water white bismuth fully until five water bismuth nitrates;
The tantalum oxalate acid solution is joined in the solution of bismuth, mix, and adding ammoniacal liquor, to regulate pH value be 7～8,, be heated to 100～200 ℃ of gels 2～4 hours, obtain colloidal polymer 60～80 ℃ of stirrings 2～8 hours down;
4) with above-mentioned colloidal polymer 300～450 ℃ of calcination 2～4h in Muffle furnace, promptly obtain Bi 3TaO 7The presoma of photochemical catalyst; With Bi 3TaO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450～600 ℃ of calcination 4～6h 3TaO 7Photochemical catalyst.
Gained visible-light response nano Bi 3TaO 7Photochemical catalyst has cubic structure, and its crystallite dimension is in 5～80 nanometers.
Gained visible-light response nano Bi 3TaO 7The application of photochemical catalyst is characterized in that it is as photocatalyst applications.This photochemical catalyst (under the λ 〉=400nm), has good photocatalytic activity at visible light.
The invention has the beneficial effects as follows: use Ta 2O 5Be raw material, obtained the water miscible tantalum oxalate aqueous solution, again by citric acid method under lower synthesis temperature (450～600 ℃), obtained the much higher nanometer Bi of specific activity conventional solid-state method 3TaO 7Photochemical catalyst, the nanometer Bi of acquisition 3TaO 7Photochemical catalyst has catalytic degradation effect preferably under visible light; And it is easy and simple to handle.
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
Visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst, it comprises the steps:
1) takes by weighing 2.0000 Ta that restrain 2O 5Join (Ta among 2.5300 KOH that restrain 2O 5With the mol ratio of KOH be 1:10), mixed grinding is even, puts into corundum crucible, at 500 ℃ of calcination 4h, obtains the melt of potassium tantalate; The melt of above-mentioned potassium tantalate is dissolved in the 150ml deionized water, and filtrate filtered is regulated pH value with nitric acid, and what make solution is highly acid (PH＜2), and the tantalum in the solution is fully with tantalic acid (Ta 2O 5NH 2O) form is precipitated out, and gets white depositions after the filtration; With white depositions deionized water rinsing 3 times, remove precipitation and go up remaining potassium ion; Obtain the tantalic acid sediment;
2) the tantalic acid sediment that obtains is added the oxalic acid (this moment, the quality proportioning of tantalic acid sediment and oxalic acid was about 1:6.5) of 16g, and constantly stir, promptly obtain the water miscible tantalum oxalate aqueous solution (being the oxalates aqueous solution of tantalum);
3) getting 0.072mol[is 15.1301g] citric acid, add in the 180ml water, be 7.2761g with 0.015mol[again] Bi (NO 3) 35H 2O adds, and places 80 ℃ of stirring in water bath, gets solution A; Getting 0.048mol[is 14.0280g] chelating agent EDTA adds in the 20ml ammonia, and stirring and dissolving adds in the above-mentioned solution A then; In 80 ℃ of stirring in water bath, obtain the solution of bismuth; The 0.005mol tantalum oxalate aqueous solution is added in the solution of bismuth, adding ammoniacal liquor again, to regulate pH value be 7.5 again, stirred 5 hours down in 80 ℃, when moisture will evaporate to dryness in solution, heated 2 hours in 200 ℃, obtains colloidal polymer;
4) with above-mentioned colloidal polymer 350 ℃ of calcination 4h in Muffle furnace, promptly obtain Bi 3TaO 7The presoma of photochemical catalyst; With Bi 3TaO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450 ℃ of calcination 4h 3TaO 7Photochemical catalyst.Its crystallite dimension is at 5～40nm.
Gained visible-light response nano Bi 3TaO 7Photochemical catalyst is as photocatalyst applications, and in the experiment of degraded direct scarlet 4BS, dosage is 1g/L, and the concentration of direct scarlet 4BS is 30mg/L, and λ 〉=400nm has good degradation effect.
Embodiment 2:
Visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst, it comprises the steps:
1) takes by weighing 2.0000 Ta that restrain 2O 5Join (Ta among the KOH of 2.5300g 2O 5With the KOH mol ratio be 1:10), grind evenly, put into corundum crucible, at 500 ℃ of calcination 4h, obtain the melt of potassium tantalate; The melt of above-mentioned potassium tantalate is dissolved in the deionized water of 150ml, and filtrate filtered is regulated pH value with nitric acid, and what make solution is highly acid (PH＜2), and the tantalum in the solution is fully with tantalic acid (Ta 2O 5NH 2O) form is precipitated out, and after the filtration, gets white depositions; White depositions is washed 2 times repeatedly with deionized water, remove potassium ion remaining on the sediment, to the tantalic acid sediment;
2) the tantalic acid sediment that obtains is added the oxalic acid (this moment, the quality proportioning of tantalic acid sediment and oxalic acid was about 1:8) of 20g, and constantly stir, promptly obtain the water miscible tantalum oxalate aqueous solution;
3) getting 0.06mol[is 12.6084g] citric acid, add in the 150ml water, be 7.2761g with 0.015mol[again] Bi (NO 3) 35H 2O adds, and places 80 ℃ of stirring in water bath, gets solution A; Getting 0.048mol[is 14.0280g] chelating agent EDTA adds in the 20ml ammonia, and stirring and dissolving adds in the above-mentioned solution A then, in 80 ℃ of stirring in water bath, obtains the solution of bismuth; The 0.005mol tantalum oxalate aqueous solution is added in the solution of bismuth, adding ammoniacal liquor again, to regulate pH value be 7.5 again, stirred 6 hours down in 80 ℃, when moisture will evaporate to dryness in solution, heated 3 hours in 200 ℃, obtains colloidal polymer;
4) with above-mentioned colloidal polymer 350 ℃ of calcination 4h in Muffle furnace, promptly obtain Bi 3TaO 7The presoma of photochemical catalyst; With Bi 3TaO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 500 ℃ of calcination 4h 3TaO 7Photochemical catalyst.Its crystallite dimension is at 10～50nm.
Gained visible-light response nano Bi 3TaO 7Photochemical catalyst is as photocatalyst applications, and in the experiment of degraded direct scarlet 4BS, dosage is 1g/L, and the concentration of direct scarlet 4BS is 30mg/L, and λ 〉=400nm has good degradation effect.
Embodiment 3:
Visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst, it comprises the steps:
1) presses Ta 2O 5Choose Ta with the mol ratio 1:2 of potassium hydroxide 2O 5And potassium hydroxide, standby;
With Ta 2O 5Even with the potassium hydroxide mixed grinding, put into corundum crucible, at 400 ℃ of following calcination 2h, obtain the melt of potassium tantalate; Press Ta 2O 5With the mass ratio of deionized water be 1:20, choose ionized water, the melt of potassium tantalate is dissolved in deionized water, filter, with the clear liquid after filtering, add nitric acid and make solution be highly acid (pH＜2), make tantalum in the solution fully with tantalic acid (Ta 2O 5NH 2O) form is precipitated out, and gets sediment; With deionized water rinsing to remove the potassium ion of the remnants that adsorb on the sediment; Obtain the tantalic acid sediment;
2) the tantalic acid sediment that obtains is added oxalic acid, and constantly stir, promptly obtain the water miscible tantalum oxalate aqueous solution; Wherein the quality proportioning of tantalic acid sediment and oxalic acid is 1:1;
3) by tantalum ion and five water bismuth nitrate (Bi (NO in the tantalum oxalate aqueous solution 3) 35H 2O) mol ratio is 1:3, chooses the tantalum oxalate aqueous solution and five water bismuth nitrates, and is standby;
Mol ratio by Bi in the five water bismuth nitrates and citric acid is 1:3, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent EDTA is 1:1.8, chooses chelating agent EDTA, and is standby;
Bismuth nitrate is joined in the citric acid solution of 0.3mol/L, stir down in 60 ℃, add the mixed solution of chelating agent EDTA and ammoniacal liquor, the proportioning of chelating agent EDTA and ammoniacal liquor is 12g: 20ml in the mixed solution; Dissolve the solution that forms water white bismuth fully until five water bismuth nitrates;
The tantalum oxalate acid solution joined in the solution of bismuth, mix, and adding ammoniacal liquor, to regulate pH value be 7 that 60 ℃ of stirrings 2 hours down, moisture content will be heated to 100 ℃ of gels 2 hours during evaporate to dryness in the solution, obtain colloidal polymer;
4) with above-mentioned colloidal polymer 300 ℃ of calcination 2h in Muffle furnace, promptly obtain Bi 3TaO 7The presoma of photochemical catalyst; With Bi 3TaO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450 ℃ of calcination 4h 3TaO 7Photochemical catalyst.Its crystallite dimension is in 5～80 nanometers.
Embodiment 4:
Visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst, it comprises the steps:
1) presses Ta 2O 5Choose Ta at 1: 20 with the mol ratio of potassium hydroxide 2O 5And potassium hydroxide, standby;
With Ta 2O 5Even with the potassium hydroxide mixed grinding, put into corundum crucible, at 500 ℃ of following calcination 4h, obtain the melt of potassium tantalate; Press Ta 2O 5With the mass ratio of deionized water be 1: 100, choose deionized water, the melt of potassium tantalate is dissolved in deionized water, filter, with the clear liquid after filtering, add nitric acid and make solution be highly acid (pH＜2), make tantalum in the solution fully with tantalic acid (Ta 2O 5NH 2O) form is precipitated out, and gets sediment; With deionized water rinsing to remove the potassium ion of the remnants that adsorb on the sediment; Obtain the tantalic acid sediment;
2) the tantalic acid sediment that obtains is added oxalic acid, and constantly stir, promptly obtain the water miscible tantalum oxalate aqueous solution; Wherein the quality proportioning of tantalic acid sediment and oxalic acid is 1: 10;
3) by tantalum ion and five water bismuth nitrate (Bi (NO in the tantalum oxalate aqueous solution 3) 35H 2O) mol ratio is 1: 3, chooses the tantalum oxalate aqueous solution and five water bismuth nitrates, and is standby;
Mol ratio by Bi in the five water bismuth nitrates and citric acid is 1: 6, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent EDTA is 1: 6, chooses chelating agent EDTA, and is standby;
Bismuth nitrate is joined in the citric acid solution of 0.7mol/L, stir down in 80 ℃, add the mixed solution of chelating agent EDTA and ammoniacal liquor, the proportioning of chelating agent EDTA and ammoniacal liquor is 16g: 20ml in the mixed solution; Dissolve the solution that forms water white bismuth fully until five water bismuth nitrates;
The tantalum oxalate acid solution joined in the solution of bismuth, mix, and adding ammoniacal liquor, to regulate pH value be 8 that 80 ℃ of stirrings 8 hours down, moisture content will be heated to 200 ℃ of gels 4 hours during evaporate to dryness in the solution, obtain colloidal polymer;
4) with above-mentioned colloidal polymer 450 ℃ of calcination 4h in Muffle furnace, promptly obtain Bi 3TaO 7The presoma of photochemical catalyst; With Bi 3TaO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 600 ℃ of calcination 6h 3TaO 7Photochemical catalyst.

Claims (2)

1. visible-light response nano Bi 3TaO 7The preparation method of photochemical catalyst is characterized in that it comprises the steps:
1) presses Ta 2O 5Choose Ta with the mol ratio 1: 2～20 of potassium hydroxide 2O 5And potassium hydroxide, standby;
With Ta 2O 5Even with the potassium hydroxide mixed grinding, put into corundum crucible, at 400～500 ℃ of following calcination 2～4h, obtain the melt of potassium tantalate; Press Ta 2O 5With the mass ratio of deionized water be 1: 20～100, choose deionized water, the melt of potassium tantalate is dissolved in deionized water, filter, with the clear liquid after filtering, add nitric acid and make solution be highly acid, sediment; With deionized water rinsing to remove the potassium ion of the remnants that adsorb on the sediment; Obtain the tantalic acid sediment;
2) the tantalic acid sediment that obtains is added oxalic acid, and constantly stir, promptly obtain the water miscible tantalum oxalate aqueous solution; Wherein the quality proportioning of tantalic acid sediment and oxalic acid is 1: 1～10;
3) mol ratio by tantalum ion in the tantalum oxalate aqueous solution and five water bismuth nitrates is 1: 3, chooses the tantalum oxalate aqueous solution and five water bismuth nitrates, and is standby;
Mol ratio by Bi in the five water bismuth nitrates and citric acid is 1: 3～1: 6, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent ethylenediamine tetra-acetic acid is 1: 1.8～1: 6, chooses the chelating agent ethylenediamine tetra-acetic acid, and is standby;
Bismuth nitrate is joined in the citric acid solution of 0.3～0.7mol/L, stir down in 60～80 ℃, add the mixed solution of chelating agent ethylenediamine tetra-acetic acid and ammoniacal liquor, the proportioning of chelating agent ethylenediamine tetra-acetic acid and ammoniacal liquor is 12～16g: 20ml in the mixed solution; Dissolve the solution that forms water white bismuth fully until five water bismuth nitrates;
The tantalum oxalate acid solution is joined in the solution of bismuth, mix, and adding ammoniacal liquor, to regulate pH value be 7～8,, be heated to 100～200 ℃ of gels 2～4 hours, obtain colloidal polymer 60～80 ℃ of stirrings 2～8 hours down;
4) with above-mentioned colloidal polymer 300～450 ℃ of calcination 2～4h in Muffle furnace, promptly obtain Bi 3TaO 7The presoma of photochemical catalyst; With Bi 3TaO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450～600 ℃ of calcination 4～6h 3TaO 7Photochemical catalyst.
2. as claim 1 gained visible-light response nano Bi 3TaO 7The application of photochemical catalyst is characterized in that it is as photocatalyst applications.
CN2008101970194A 2008-09-18 2008-09-18 Visible-light response nano Bi3TaO7 photocatalyst preparation method and use thereof Expired - Fee Related CN101362083B (en)

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CN104275176B (en) * 2014-10-13 2016-06-29 桂林理工大学 Visible light-responded photocatalyst Ca3Nb3V5O23And preparation method thereof
CN104275188B (en) * 2014-10-16 2016-06-29 桂林理工大学 Visible light-responded photocatalyst CuTi2V4O15And preparation method thereof
CN104607176A (en) * 2015-01-05 2015-05-13 江苏科技大学 Preparation method of nano bismuth tantalite photocatalyst and application of nano bismuth tantalite photocatalyst to photocatalytic degradation of organic pollutants
CN108057434A (en) * 2017-12-01 2018-05-22 常州大学 A kind of preparation method of silica supported photochemical catalyst

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